# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
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data_Ir1dpyxL4_16srv479
_database_code_depnum_ccdc_archive 'CCDC 2006844'
loop_
_audit_author_name
_audit_author_address
'Dmitry Yufit'
;Durham University
United Kingdom
;
_audit_update_record
;
2020-06-01 deposited with the CCDC. 2020-07-10 downloaded from the CCDC.
;
_audit_creation_date 2016-12-14
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C32 H29 Ir N5 O2, F6 P, C2 H3 N'
_chemical_formula_sum 'C34 H32 F6 Ir N6 O2 P'
_chemical_formula_weight 893.83
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'
_cell_length_a 11.4532(5)
_cell_length_b 15.8034(7)
_cell_length_c 18.1543(8)
_cell_angle_alpha 90.00
_cell_angle_beta 95.0909(16)
_cell_angle_gamma 90.00
_cell_volume 3273.0(2)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9850
_cell_measurement_temperature 120.0
_cell_measurement_theta_max 31.57
_cell_measurement_theta_min 2.40
_exptl_absorpt_coefficient_mu 4.206
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.6619
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0871 before and 0.0418 after correction.
The Ratio of minimum to maximum transmission is 0.6619.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour 'clear dark orange'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier dark
_exptl_crystal_colour_primary orange
_exptl_crystal_density_diffrn 1.814
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 1760
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.21
_exptl_crystal_size_min 0.08
_exptl_special_details ?
_diffrn_reflns_av_R_equivalents 0.0310
_diffrn_reflns_av_unetI/netI 0.0174
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_number 71211
_diffrn_reflns_theta_full 30.00
_diffrn_reflns_theta_max 30.00
_diffrn_reflns_theta_min 2.40
_diffrn_ambient_temperature 120.0
_diffrn_detector 'Bruker PHOTON 100 CMOS'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type 'CMOS sensor'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device '3-circle diffractometer'
_diffrn_measurement_device_type 'Bruker D8 Venture'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator 'focusing mirrors'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_type 'Incoatec I\mS microsource'
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number 0
_reflns_number_gt 8563
_reflns_number_total 9548
_reflns_threshold_expression >2sigma(I)
_computing.bruker_data_scaling 'SADABS V2012/1 (Bruker AXS Inc.)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection 'APEX2 v.2013.4_1 (Bruker, 2013)'
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'XS (Sheldrick, 2008)'
_refine_diff_density_max 0.809
_refine_diff_density_min -1.012
_refine_diff_density_rms 0.081
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.054
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 456
_refine_ls_number_reflns 9548
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0214
_refine_ls_R_factor_gt 0.0161
_refine_ls_restrained_S_all 1.054
_refine_ls_shift/su_max 0.007
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0120P)^2^+3.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0348
_refine_ls_wR_factor_ref 0.0367
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C10(H10), C11(H11), C13(H13),
C15(H15), C16(H16), C17(H17), C18(H18), C24(H24), C29(H29), C30(H30), C31(H31),
C32(H32)
2.b Idealised Me refined as rotating group:
C6(H6A,H6B,H6C), C14(H14A,H14B,H14C), C26(H26A,H26B,H26C), C27(H27A,H27B,
H27C), C2S(H2SA,H2SB,H2SC)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Ir1 Ir 0.370623(5) 0.324619(4) 0.673333(3) 0.00869(2) Uani 1 d . . .
O1 O 0.45082(10) 0.33310(7) 0.77758(6) 0.0126(2) Uani 1 d . . .
O2 O 0.25885(13) 0.43371(10) 1.03269(7) 0.0281(3) Uani 1 d . . .
N1 N 0.26920(12) 0.31464(8) 0.57693(8) 0.0113(3) Uani 1 d . . .
N2 N 0.11660(12) 0.31803(9) 0.65376(8) 0.0142(3) Uani 1 d . . .
N3 N 0.20397(12) 0.33416(9) 0.70949(8) 0.0112(3) Uani 1 d . . .
N4 N 0.39145(12) 0.19696(9) 0.68130(7) 0.0113(3) Uani 1 d . . .
N5 N 0.40181(12) 0.44988(9) 0.65249(8) 0.0117(3) Uani 1 d . . .
C1 C 0.30759(15) 0.31075(10) 0.50832(9) 0.0138(3) Uani 1 d . . .
H1 H 0.3897 0.3107 0.5040 0.017 Uiso 1 calc . . R
C2 C 0.23318(16) 0.30687(11) 0.44518(10) 0.0177(3) Uani 1 d . . .
H2 H 0.2628 0.3055 0.3980 0.021 Uiso 1 calc . . R
C3 C 0.11302(17) 0.30504(12) 0.45166(10) 0.0208(4) Uani 1 d . . .
H3 H 0.0596 0.3015 0.4086 0.025 Uiso 1 calc . . R
C4 C 0.07191(16) 0.30834(12) 0.52048(10) 0.0203(4) Uani 1 d . . .
H4 H -0.0100 0.3071 0.5254 0.024 Uiso 1 calc . . R
C5 C 0.15215(14) 0.31356(10) 0.58344(9) 0.0135(3) Uani 1 d . . .
C6 C -0.00530(14) 0.31183(12) 0.66918(10) 0.0179(3) Uani 1 d . . .
H6A H -0.0100 0.2864 0.7181 0.027 Uiso 1 calc . . GR
H6B H -0.0480 0.2764 0.6316 0.027 Uiso 1 calc . . GR
H6C H -0.0402 0.3685 0.6683 0.027 Uiso 1 calc . . GR
C7 C 0.18024(14) 0.35424(11) 0.77551(9) 0.0127(3) Uani 1 d . . .
H7 H 0.1003 0.3602 0.7848 0.015 Uiso 1 calc . . R
C8 C 0.26915(14) 0.36811(10) 0.83594(9) 0.0125(3) Uani 1 d . . .
C9 C 0.39148(14) 0.35414(10) 0.83513(9) 0.0122(3) Uani 1 d . . .
C10 C 0.46076(15) 0.36529(11) 0.90286(9) 0.0161(3) Uani 1 d . . .
H10 H 0.5424 0.3540 0.9046 0.019 Uiso 1 calc . . R
C11 C 0.41480(16) 0.39171(12) 0.96616(10) 0.0186(3) Uani 1 d . . .
H11 H 0.4649 0.3991 1.0103 0.022 Uiso 1 calc . . R
C12 C 0.29507(16) 0.40782(12) 0.96632(10) 0.0187(3) Uani 1 d . . .
C13 C 0.22385(15) 0.39575(11) 0.90226(9) 0.0154(3) Uani 1 d . . .
H13 H 0.1422 0.4061 0.9023 0.018 Uiso 1 calc . . R
C14 C 0.13751(18) 0.45230(15) 1.03425(11) 0.0289(5) Uani 1 d . . .
H14A H 0.1149 0.4965 0.9979 0.043 Uiso 1 calc . . GR
H14B H 0.1227 0.4721 1.0837 0.043 Uiso 1 calc . . GR
H14C H 0.0914 0.4011 1.0223 0.043 Uiso 1 calc . . GR
C15 C 0.31624(15) 0.14404(11) 0.71030(9) 0.0141(3) Uani 1 d . . .
H15 H 0.2456 0.1664 0.7260 0.017 Uiso 1 calc . . R
C16 C 0.33735(16) 0.05859(11) 0.71817(10) 0.0170(3) Uani 1 d . . .
H16 H 0.2819 0.0224 0.7381 0.020 Uiso 1 calc . . R
C17 C 0.44154(15) 0.02675(11) 0.69625(9) 0.0165(3) Uani 1 d . . .
H17 H 0.4597 -0.0316 0.7025 0.020 Uiso 1 calc . . R
C18 C 0.51906(15) 0.08060(11) 0.66524(9) 0.0151(3) Uani 1 d . . .
H18 H 0.5900 0.0587 0.6496 0.018 Uiso 1 calc . . R
C19 C 0.49420(14) 0.16645(10) 0.65679(9) 0.0116(3) Uani 1 d . . .
C20 C 0.56631(13) 0.23232(10) 0.62423(9) 0.0111(3) Uani 1 d . . .
C21 C 0.52107(13) 0.31401(10) 0.63180(9) 0.0109(3) Uani 1 d . . .
C22 C 0.57269(14) 0.38805(11) 0.60657(9) 0.0126(3) Uani 1 d . . .
C23 C 0.67538(14) 0.37931(11) 0.56932(9) 0.0145(3) Uani 1 d . . .
C24 C 0.71620(14) 0.29720(12) 0.55951(9) 0.0153(3) Uani 1 d . . .
H24 H 0.7833 0.2911 0.5328 0.018 Uiso 1 calc . . R
C25 C 0.66686(14) 0.22284(11) 0.58570(9) 0.0140(3) Uani 1 d . . .
C26 C 0.72470(16) 0.13997(12) 0.56998(11) 0.0204(4) Uani 1 d . . .
H26A H 0.7581 0.1149 0.6165 0.031 Uiso 1 calc . . GR
H26B H 0.7872 0.1498 0.5375 0.031 Uiso 1 calc . . GR
H26C H 0.6664 0.1013 0.5457 0.031 Uiso 1 calc . . GR
C27 C 0.74283(16) 0.45191(12) 0.53951(11) 0.0216(4) Uani 1 d . . .
H27A H 0.6915 0.4836 0.5032 0.032 Uiso 1 calc . . GR
H27B H 0.8100 0.4298 0.5157 0.032 Uiso 1 calc . . GR
H27C H 0.7707 0.4895 0.5802 0.032 Uiso 1 calc . . GR
C28 C 0.50462(14) 0.46495(11) 0.62040(9) 0.0131(3) Uani 1 d . . .
C29 C 0.53363(16) 0.54830(11) 0.60483(10) 0.0188(3) Uani 1 d . . .
H29 H 0.6048 0.5598 0.5836 0.023 Uiso 1 calc . . R
C30 C 0.46022(18) 0.61467(12) 0.61987(11) 0.0228(4) Uani 1 d . . .
H30 H 0.4810 0.6713 0.6093 0.027 Uiso 1 calc . . R
C31 C 0.35631(17) 0.59761(12) 0.65045(11) 0.0213(4) Uani 1 d . . .
H31 H 0.3038 0.6420 0.6602 0.026 Uiso 1 calc . . R
C32 C 0.33061(15) 0.51445(11) 0.66655(10) 0.0157(3) Uani 1 d . . .
H32 H 0.2600 0.5025 0.6884 0.019 Uiso 1 calc . . R
P1 P 0.99313(4) 0.43138(3) 0.26201(3) 0.01740(9) Uani 1 d . . .
F1 F 1.02847(11) 0.38028(8) 0.19147(7) 0.0291(3) Uani 1 d . . .
F2 F 0.93276(11) 0.34861(8) 0.29223(7) 0.0315(3) Uani 1 d . . .
F3 F 1.11514(10) 0.40577(9) 0.30631(7) 0.0323(3) Uani 1 d . . .
F4 F 1.05445(11) 0.51473(8) 0.23202(7) 0.0294(3) Uani 1 d . . .
F5 F 0.87191(10) 0.45841(8) 0.21830(7) 0.0305(3) Uani 1 d . . .
F6 F 0.95841(10) 0.48326(8) 0.33275(7) 0.0295(3) Uani 1 d . . .
N1S N 0.8681(2) 0.18289(18) 0.40373(13) 0.0590(8) Uani 1 d . . .
C1S C 0.81506(19) 0.18218(14) 0.34781(12) 0.0297(5) Uani 1 d . . .
C2S C 0.74658(17) 0.18213(14) 0.27663(11) 0.0253(4) Uani 1 d . . .
H2SA H 0.7668 0.1322 0.2483 0.038 Uiso 1 calc . . GR
H2SB H 0.7638 0.2335 0.2493 0.038 Uiso 1 calc . . GR
H2SC H 0.6629 0.1806 0.2842 0.038 Uiso 1 calc . . GR
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ir1 0.00703(3) 0.00839(3) 0.01066(3) 0.00024(2) 0.00090(2) -0.00006(2)
O1 0.0095(5) 0.0159(6) 0.0123(5) -0.0009(4) 0.0005(4) 0.0002(4)
O2 0.0266(7) 0.0444(9) 0.0140(6) -0.0040(6) 0.0053(5) 0.0087(7)
N1 0.0104(6) 0.0100(6) 0.0131(6) 0.0002(5) -0.0004(5) 0.0003(5)
N2 0.0075(6) 0.0198(7) 0.0150(7) -0.0009(6) -0.0001(5) -0.0012(5)
N3 0.0080(6) 0.0117(6) 0.0136(6) 0.0006(5) -0.0008(5) -0.0005(5)
N4 0.0111(6) 0.0108(6) 0.0118(6) 0.0002(5) 0.0001(5) 0.0001(5)
N5 0.0117(6) 0.0101(6) 0.0132(6) -0.0003(5) 0.0009(5) -0.0008(5)
C1 0.0158(8) 0.0119(8) 0.0138(7) -0.0001(6) 0.0016(6) -0.0012(6)
C2 0.0235(9) 0.0164(8) 0.0132(8) -0.0012(6) 0.0009(6) -0.0021(7)
C3 0.0214(9) 0.0239(9) 0.0161(8) 0.0010(7) -0.0046(7) -0.0049(7)
C4 0.0131(8) 0.0277(10) 0.0191(9) 0.0024(7) -0.0032(6) -0.0028(7)
C5 0.0116(7) 0.0132(8) 0.0154(8) 0.0010(6) -0.0007(6) -0.0005(6)
C6 0.0087(7) 0.0223(9) 0.0225(9) -0.0004(7) 0.0012(6) -0.0013(6)
C7 0.0101(7) 0.0126(7) 0.0158(8) 0.0013(6) 0.0027(6) 0.0005(6)
C8 0.0137(7) 0.0110(7) 0.0129(7) 0.0021(6) 0.0015(6) 0.0002(6)
C9 0.0130(7) 0.0102(7) 0.0137(7) 0.0020(6) 0.0023(6) -0.0002(6)
C10 0.0137(8) 0.0190(9) 0.0152(8) 0.0015(6) -0.0003(6) -0.0002(6)
C11 0.0202(9) 0.0226(9) 0.0125(8) 0.0009(7) -0.0013(6) 0.0010(7)
C12 0.0225(9) 0.0202(9) 0.0139(8) 0.0008(7) 0.0049(7) 0.0022(7)
C13 0.0151(8) 0.0165(8) 0.0149(8) 0.0016(6) 0.0038(6) 0.0013(6)
C14 0.0276(10) 0.0396(12) 0.0209(10) -0.0036(8) 0.0107(8) 0.0049(9)
C15 0.0128(7) 0.0133(7) 0.0163(8) 0.0012(6) 0.0028(6) -0.0007(6)
C16 0.0183(8) 0.0140(8) 0.0192(8) 0.0028(6) 0.0041(6) -0.0010(6)
C17 0.0196(8) 0.0124(7) 0.0172(8) 0.0025(6) -0.0009(6) 0.0027(6)
C18 0.0156(8) 0.0145(8) 0.0154(8) 0.0005(6) 0.0018(6) 0.0034(6)
C19 0.0107(7) 0.0140(8) 0.0097(7) -0.0005(6) -0.0010(5) 0.0009(6)
C20 0.0090(7) 0.0136(7) 0.0104(7) 0.0002(6) -0.0015(5) 0.0006(6)
C21 0.0085(7) 0.0145(8) 0.0095(7) -0.0003(6) 0.0000(5) -0.0003(6)
C22 0.0106(7) 0.0138(8) 0.0132(7) 0.0002(6) -0.0004(6) -0.0014(6)
C23 0.0104(7) 0.0188(8) 0.0143(8) 0.0014(6) 0.0012(6) -0.0021(6)
C24 0.0088(7) 0.0212(8) 0.0162(8) 0.0004(6) 0.0030(6) 0.0008(6)
C25 0.0106(7) 0.0170(8) 0.0142(7) -0.0006(6) -0.0005(6) 0.0028(6)
C26 0.0155(8) 0.0200(9) 0.0271(9) 0.0005(7) 0.0086(7) 0.0052(7)
C27 0.0169(8) 0.0211(9) 0.0282(10) 0.0027(7) 0.0092(7) -0.0039(7)
C28 0.0133(7) 0.0131(8) 0.0129(7) -0.0004(6) 0.0013(6) -0.0016(6)
C29 0.0194(8) 0.0154(8) 0.0224(9) 0.0022(7) 0.0063(7) -0.0039(7)
C30 0.0285(10) 0.0119(8) 0.0287(10) 0.0032(7) 0.0067(8) -0.0018(7)
C31 0.0252(9) 0.0120(8) 0.0271(9) -0.0004(7) 0.0047(7) 0.0032(7)
C32 0.0157(8) 0.0133(8) 0.0185(8) -0.0008(6) 0.0033(6) 0.0012(6)
P1 0.0155(2) 0.0176(2) 0.0196(2) 0.00141(17) 0.00391(17) 0.00237(17)
F1 0.0362(7) 0.0249(6) 0.0280(6) -0.0054(5) 0.0131(5) 0.0030(5)
F2 0.0335(7) 0.0232(6) 0.0395(7) 0.0052(5) 0.0136(6) -0.0057(5)
F3 0.0195(6) 0.0468(8) 0.0306(6) 0.0115(6) 0.0031(5) 0.0082(5)
F4 0.0315(6) 0.0216(6) 0.0367(7) 0.0028(5) 0.0116(5) -0.0034(5)
F5 0.0214(6) 0.0390(7) 0.0302(6) 0.0010(5) -0.0031(5) 0.0081(5)
F6 0.0247(6) 0.0373(7) 0.0276(6) -0.0108(5) 0.0089(5) -0.0028(5)
N1S 0.0574(16) 0.0772(19) 0.0390(13) 0.0192(12) -0.0139(11) -0.0332(14)
C1S 0.0272(10) 0.0317(11) 0.0302(11) 0.0053(9) 0.0030(8) -0.0100(9)
C2S 0.0189(9) 0.0318(11) 0.0251(10) -0.0011(8) 0.0020(7) -0.0029(8)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 O1 2.0334(12) . ?
Ir1 N1 2.0190(14) . ?
Ir1 N3 2.0782(13) . ?
Ir1 N4 2.0352(14) . ?
Ir1 N5 2.0527(14) . ?
Ir1 C21 1.9483(16) . ?
O1 C9 1.3379(19) . ?
O2 C12 1.371(2) . ?
O2 C14 1.423(2) . ?
N1 C1 1.359(2) . ?
N1 C5 1.356(2) . ?
N2 N3 1.3822(19) . ?
N2 C5 1.376(2) . ?
N2 C6 1.451(2) . ?
N3 C7 1.292(2) . ?
N4 C15 1.341(2) . ?
N4 C19 1.381(2) . ?
N5 C28 1.380(2) . ?
N5 C32 1.345(2) . ?
C1 H1 0.9500 . ?
C1 C2 1.368(2) . ?
C2 H2 0.9500 . ?
C2 C3 1.392(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.375(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.404(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7 0.9500 . ?
C7 C8 1.446(2) . ?
C8 C9 1.420(2) . ?
C8 C13 1.421(2) . ?
C9 C10 1.414(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.371(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.395(3) . ?
C12 C13 1.373(2) . ?
C13 H13 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15 0.9500 . ?
C15 C16 1.377(2) . ?
C16 H16 0.9500 . ?
C16 C17 1.385(2) . ?
C17 H17 0.9500 . ?
C17 C18 1.385(2) . ?
C18 H18 0.9500 . ?
C18 C19 1.392(2) . ?
C19 C20 1.484(2) . ?
C20 C21 1.402(2) . ?
C20 C25 1.408(2) . ?
C21 C22 1.406(2) . ?
C22 C23 1.415(2) . ?
C22 C28 1.477(2) . ?
C23 C24 1.396(2) . ?
C23 C27 1.510(2) . ?
C24 H24 0.9500 . ?
C24 C25 1.405(2) . ?
C25 C26 1.506(2) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.394(2) . ?
C29 H29 0.9500 . ?
C29 C30 1.386(3) . ?
C30 H30 0.9500 . ?
C30 C31 1.384(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.384(2) . ?
C32 H32 0.9500 . ?
P1 F1 1.5962(12) . ?
P1 F2 1.5991(13) . ?
P1 F3 1.6012(13) . ?
P1 F4 1.6101(12) . ?
P1 F5 1.5951(12) . ?
P1 F6 1.6032(12) . ?
N1S C1S 1.136(3) . ?
C1S C2S 1.451(3) . ?
C2S H2SA 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ir1 N3 93.03(5) . . ?
O1 Ir1 N4 87.63(5) . . ?
O1 Ir1 N5 92.09(5) . . ?
N1 Ir1 O1 171.70(5) . . ?
N1 Ir1 N3 78.79(5) . . ?
N1 Ir1 N4 92.23(5) . . ?
N1 Ir1 N5 90.67(5) . . ?
N4 Ir1 N3 98.89(5) . . ?
N4 Ir1 N5 161.42(6) . . ?
N5 Ir1 N3 99.67(5) . . ?
C21 Ir1 O1 91.37(6) . . ?
C21 Ir1 N1 96.80(6) . . ?
C21 Ir1 N3 175.57(6) . . ?
C21 Ir1 N4 80.80(6) . . ?
C21 Ir1 N5 80.63(6) . . ?
C9 O1 Ir1 121.63(10) . . ?
C12 O2 C14 116.83(15) . . ?
C1 N1 Ir1 126.16(11) . . ?
C5 N1 Ir1 115.00(11) . . ?
C5 N1 C1 118.83(14) . . ?
N3 N2 C6 121.17(14) . . ?
C5 N2 N3 115.72(13) . . ?
C5 N2 C6 123.00(14) . . ?
N2 N3 Ir1 112.40(10) . . ?
C7 N3 Ir1 125.85(11) . . ?
C7 N3 N2 121.74(14) . . ?
C15 N4 Ir1 124.80(11) . . ?
C15 N4 C19 120.26(14) . . ?
C19 N4 Ir1 114.89(11) . . ?
C28 N5 Ir1 114.41(11) . . ?
C32 N5 Ir1 125.34(12) . . ?
C32 N5 C28 120.25(15) . . ?
N1 C1 H1 118.6 . . ?
N1 C1 C2 122.82(16) . . ?
C2 C1 H1 118.6 . . ?
C1 C2 H2 120.7 . . ?
C1 C2 C3 118.52(17) . . ?
C3 C2 H2 120.7 . . ?
C2 C3 H3 120.1 . . ?
C4 C3 C2 119.79(17) . . ?
C4 C3 H3 120.1 . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.33(17) . . ?
C5 C4 H4 120.3 . . ?
N1 C5 N2 117.16(14) . . ?
N1 C5 C4 120.69(16) . . ?
N2 C5 C4 122.15(16) . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 C7 H7 118.3 . . ?
N3 C7 C8 123.31(15) . . ?
C8 C7 H7 118.3 . . ?
C9 C8 C7 126.71(15) . . ?
C9 C8 C13 119.43(15) . . ?
C13 C8 C7 113.82(15) . . ?
O1 C9 C8 128.09(15) . . ?
O1 C9 C10 115.17(14) . . ?
C10 C9 C8 116.72(15) . . ?
C9 C10 H10 118.7 . . ?
C11 C10 C9 122.64(16) . . ?
C11 C10 H10 118.7 . . ?
C10 C11 H11 119.7 . . ?
C10 C11 C12 120.53(16) . . ?
C12 C11 H11 119.7 . . ?
O2 C12 C11 115.50(16) . . ?
O2 C12 C13 125.62(17) . . ?
C13 C12 C11 118.88(16) . . ?
C8 C13 H13 119.1 . . ?
C12 C13 C8 121.73(16) . . ?
C12 C13 H13 119.1 . . ?
O2 C14 H14A 109.5 . . ?
O2 C14 H14B 109.5 . . ?
O2 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N4 C15 H15 118.7 . . ?
N4 C15 C16 122.63(16) . . ?
C16 C15 H15 118.7 . . ?
C15 C16 H16 120.8 . . ?
C15 C16 C17 118.31(16) . . ?
C17 C16 H16 120.8 . . ?
C16 C17 H17 120.2 . . ?
C18 C17 C16 119.54(16) . . ?
C18 C17 H17 120.2 . . ?
C17 C18 H18 119.6 . . ?
C17 C18 C19 120.76(16) . . ?
C19 C18 H18 119.6 . . ?
N4 C19 C18 118.45(15) . . ?
N4 C19 C20 113.80(14) . . ?
C18 C19 C20 127.74(15) . . ?
C21 C20 C19 112.54(14) . . ?
C21 C20 C25 118.20(15) . . ?
C25 C20 C19 129.21(15) . . ?
C20 C21 Ir1 117.66(12) . . ?
C20 C21 C22 124.37(15) . . ?
C22 C21 Ir1 117.80(12) . . ?
C21 C22 C23 117.78(15) . . ?
C21 C22 C28 112.69(14) . . ?
C23 C22 C28 129.44(15) . . ?
C22 C23 C27 124.80(16) . . ?
C24 C23 C22 116.99(15) . . ?
C24 C23 C27 118.21(15) . . ?
C23 C24 H24 117.1 . . ?
C23 C24 C25 125.80(15) . . ?
C25 C24 H24 117.1 . . ?
C20 C25 C26 125.43(16) . . ?
C24 C25 C20 116.78(15) . . ?
C24 C25 C26 117.80(15) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 H27A 109.5 . . ?
C23 C27 H27B 109.5 . . ?
C23 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N5 C28 C22 114.38(14) . . ?
N5 C28 C29 118.45(15) . . ?
C29 C28 C22 127.17(15) . . ?
C28 C29 H29 119.5 . . ?
C30 C29 C28 121.03(17) . . ?
C30 C29 H29 119.5 . . ?
C29 C30 H30 120.3 . . ?
C31 C30 C29 119.33(17) . . ?
C31 C30 H30 120.3 . . ?
C30 C31 H31 120.8 . . ?
C32 C31 C30 118.45(17) . . ?
C32 C31 H31 120.8 . . ?
N5 C32 C31 122.46(16) . . ?
N5 C32 H32 118.8 . . ?
C31 C32 H32 118.8 . . ?
F1 P1 F2 90.54(7) . . ?
F1 P1 F3 90.17(7) . . ?
F1 P1 F4 89.62(7) . . ?
F1 P1 F6 179.55(8) . . ?
F2 P1 F3 90.32(7) . . ?
F2 P1 F4 179.66(8) . . ?
F2 P1 F6 89.89(7) . . ?
F3 P1 F4 89.38(7) . . ?
F3 P1 F6 89.68(7) . . ?
F5 P1 F1 90.45(7) . . ?
F5 P1 F2 90.34(7) . . ?
F5 P1 F3 179.09(8) . . ?
F5 P1 F4 89.95(7) . . ?
F5 P1 F6 89.70(7) . . ?
F6 P1 F4 89.95(7) . . ?
N1S C1S C2S 179.3(3) . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C5 N2 N3 8.1(2) . . . . ?
C4 C5 N2 N3 -171.74(16) . . . . ?
C4 C5 N2 C6 4.4(3) . . . . ?
C5 N2 N3 Ir1 -10.90(17) . . . . ?
C5 N2 N3 C7 167.90(15) . . . . ?
C6 N2 N3 Ir1 172.86(12) . . . . ?
C6 N2 N3 C7 -8.3(2) . . . . ?
C6 N2 C5 N1 -175.78(15) . . . . ?
C8 C7 N3 Ir1 -4.0(2) . . . . ?
C8 C7 N3 N2 177.34(15) . . . . ?
C9 C8 C7 N3 -6.8(3) . . . . ?
C11 C12 O2 C14 178.77(18) . . . . ?
C13 C8 C7 N3 175.55(16) . . . . ?
C13 C12 O2 C14 -2.3(3) . . . . ?
C18 C19 C20 C21 -173.43(16) . . . . ?
C18 C19 C20 C25 9.5(3) . . . . ?
C21 C20 C19 N4 6.09(19) . . . . ?
C21 C22 C28 N5 -2.4(2) . . . . ?
C21 C22 C28 C29 177.41(17) . . . . ?
C23 C22 C28 N5 174.02(16) . . . . ?
C23 C22 C28 C29 -6.2(3) . . . . ?
C25 C20 C19 N4 -170.95(16) . . . . ?
_iucr_refine_instructions_details
;
TITL 16srv479 in P21/c #14
REM reset to P21/c #14
CELL 0.71073 11.4532 15.8034 18.1543 90 95.0909 90
ZERR 4 0.0005 0.0007 0.0008 0 0.0016 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H F Ir N O P
UNIT 136 128 24 4 24 8 4
L.S. 9
PLAN 5
SIZE 0.08 0.21 0.25
TEMP -153.15
CONF N1 C5 N2 N3
CONF C4 C5 N2 N3
CONF C6 N2 C5 N1
CONF C4 C5 N2 C6
CONF C5 N2 N3 Ir1
CONF C6 N2 N3 Ir1
CONF C5 N2 N3 C7
CONF C6 N2 N3 C7
CONF C8 C7 N3 Ir1
CONF C8 C7 N3 N2
CONF C9 C8 C7 N3
CONF C13 C8 C7 N3
CONF C11 C12 O2 C14
CONF C13 C12 O2 C14
CONF C21 C20 C19 N4
CONF C18 C19 C20 C21
CONF C25 C20 C19 N4
CONF C18 C19 C20 C25
CONF C21 C22 C28 N5
CONF C23 C22 C28 N5
CONF C21 C22 C28 C29
CONF C23 C22 C28 C29
BOND $h
fmap 2
acta
OMIT -2 60
WGHT 0.012 3.3
FVAR 0.08035
REM
REM
REM
Ir1 4 0.37062 0.32462 0.67333 11.00000 0.00703 0.00839 0.01066 =
0.00024 0.00090 -0.00006
O1 6 0.45082 0.33310 0.77758 11.00000 0.00948 0.01593 0.01228 =
-0.00095 0.00046 0.00016
O2 6 0.25885 0.43371 1.03269 11.00000 0.02658 0.04441 0.01396 =
-0.00397 0.00534 0.00869
N1 5 0.26920 0.31464 0.57693 11.00000 0.01044 0.01000 0.01311 =
0.00020 -0.00043 0.00027
N2 5 0.11660 0.31803 0.65376 11.00000 0.00752 0.01981 0.01500 =
-0.00091 -0.00012 -0.00119
N3 5 0.20397 0.33416 0.70949 11.00000 0.00802 0.01165 0.01363 =
0.00062 -0.00079 -0.00049
N4 5 0.39145 0.19696 0.68131 11.00000 0.01108 0.01080 0.01179 =
0.00018 0.00005 0.00011
N5 5 0.40181 0.44988 0.65249 11.00000 0.01172 0.01012 0.01320 =
-0.00035 0.00094 -0.00082
C1 1 0.30759 0.31075 0.50832 11.00000 0.01577 0.01188 0.01377 =
-0.00008 0.00157 -0.00125
AFIX 43
H1 2 0.38965 0.31072 0.50401 11.00000 -1.20000
AFIX 0
C2 1 0.23318 0.30688 0.44519 11.00000 0.02351 0.01641 0.01316 =
-0.00118 0.00087 -0.00209
AFIX 43
H2 2 0.26284 0.30546 0.39796 11.00000 -1.20000
AFIX 0
C3 1 0.11302 0.30504 0.45166 11.00000 0.02138 0.02389 0.01611 =
0.00100 -0.00456 -0.00493
AFIX 43
H3 2 0.05959 0.30153 0.40865 11.00000 -1.20000
AFIX 0
C4 1 0.07191 0.30834 0.52048 11.00000 0.01313 0.02773 0.01910 =
0.00239 -0.00316 -0.00281
AFIX 43
H4 2 -0.00996 0.30711 0.52539 11.00000 -1.20000
AFIX 0
C5 1 0.15215 0.31356 0.58344 11.00000 0.01158 0.01316 0.01542 =
0.00101 -0.00068 -0.00054
C6 1 -0.00530 0.31183 0.66918 11.00000 0.00868 0.02234 0.02252 =
-0.00040 0.00121 -0.00134
AFIX 137
H6a 2 -0.00998 0.28645 0.71808 11.00000 -1.50000
H6b 2 -0.04801 0.27638 0.63156 11.00000 -1.50000
H6c 2 -0.04021 0.36848 0.66832 11.00000 -1.50000
AFIX 0
C7 1 0.18024 0.35424 0.77551 11.00000 0.01009 0.01264 0.01578 =
0.00132 0.00268 0.00054
AFIX 43
H7 2 0.10033 0.36020 0.78481 11.00000 -1.20000
AFIX 0
C8 1 0.26915 0.36811 0.83594 11.00000 0.01373 0.01101 0.01293 =
0.00208 0.00152 0.00017
C9 1 0.39148 0.35414 0.83513 11.00000 0.01300 0.01022 0.01368 =
0.00200 0.00230 -0.00015
C10 1 0.46076 0.36529 0.90286 11.00000 0.01367 0.01899 0.01525 =
0.00154 -0.00030 -0.00017
AFIX 43
H10 2 0.54243 0.35401 0.90457 11.00000 -1.20000
AFIX 0
C11 1 0.41480 0.39171 0.96616 11.00000 0.02023 0.02264 0.01249 =
0.00086 -0.00132 0.00101
AFIX 43
H11 2 0.46490 0.39910 1.01027 11.00000 -1.20000
AFIX 0
C12 1 0.29507 0.40782 0.96632 11.00000 0.02247 0.02021 0.01387 =
0.00078 0.00493 0.00222
C13 1 0.22385 0.39575 0.90226 11.00000 0.01514 0.01654 0.01492 =
0.00164 0.00379 0.00125
AFIX 43
H13 2 0.14215 0.40614 0.90227 11.00000 -1.20000
AFIX 0
C14 1 0.13751 0.45230 1.03425 11.00000 0.02764 0.03962 0.02086 =
-0.00358 0.01067 0.00491
AFIX 137
H14a 2 0.11492 0.49646 0.99786 11.00000 -1.50000
H14b 2 0.12267 0.47212 1.08372 11.00000 -1.50000
H14c 2 0.09138 0.40111 1.02227 11.00000 -1.50000
AFIX 0
C15 1 0.31624 0.14404 0.71030 11.00000 0.01282 0.01334 0.01635 =
0.00124 0.00282 -0.00074
AFIX 43
H15 2 0.24559 0.16640 0.72605 11.00000 -1.20000
AFIX 0
C16 1 0.33735 0.05859 0.71817 11.00000 0.01826 0.01396 0.01924 =
0.00277 0.00406 -0.00095
AFIX 43
H16 2 0.28189 0.02240 0.73811 11.00000 -1.20000
AFIX 0
C17 1 0.44154 0.02675 0.69625 11.00000 0.01956 0.01238 0.01722 =
0.00247 -0.00093 0.00271
AFIX 43
H17 2 0.45968 -0.03162 0.70246 11.00000 -1.20000
AFIX 0
C18 1 0.51906 0.08060 0.66524 11.00000 0.01559 0.01452 0.01539 =
0.00046 0.00177 0.00336
AFIX 43
H18 2 0.59002 0.05869 0.64956 11.00000 -1.20000
AFIX 0
C19 1 0.49420 0.16645 0.65679 11.00000 0.01069 0.01401 0.00966 =
-0.00050 -0.00102 0.00093
C20 1 0.56631 0.23232 0.62423 11.00000 0.00904 0.01357 0.01038 =
0.00017 -0.00149 0.00065
C21 1 0.52107 0.31401 0.63180 11.00000 0.00848 0.01450 0.00952 =
-0.00031 0.00002 -0.00026
C22 1 0.57269 0.38805 0.60657 11.00000 0.01057 0.01384 0.01324 =
0.00020 -0.00045 -0.00144
C23 1 0.67538 0.37931 0.56932 11.00000 0.01044 0.01882 0.01434 =
0.00141 0.00122 -0.00214
C24 1 0.71620 0.29720 0.55951 11.00000 0.00876 0.02123 0.01620 =
0.00043 0.00296 0.00082
AFIX 43
H24 2 0.78331 0.29106 0.53275 11.00000 -1.20000
AFIX 0
C25 1 0.66686 0.22284 0.58570 11.00000 0.01062 0.01696 0.01417 =
-0.00059 -0.00048 0.00279
C26 1 0.72470 0.13997 0.56998 11.00000 0.01546 0.01999 0.02707 =
0.00050 0.00864 0.00523
AFIX 137
H26a 2 0.75808 0.11485 0.61653 11.00000 -1.50000
H26b 2 0.78723 0.14980 0.53748 11.00000 -1.50000
H26c 2 0.66640 0.10133 0.54572 11.00000 -1.50000
AFIX 0
C27 1 0.74283 0.45191 0.53951 11.00000 0.01689 0.02106 0.02819 =
0.00266 0.00920 -0.00393
AFIX 137
H27a 2 0.69153 0.48356 0.50323 11.00000 -1.50000
H27b 2 0.81001 0.42976 0.51571 11.00000 -1.50000
H27c 2 0.77072 0.48953 0.58025 11.00000 -1.50000
AFIX 0
C28 1 0.50462 0.46495 0.62040 11.00000 0.01327 0.01311 0.01289 =
-0.00037 0.00131 -0.00157
C29 1 0.53363 0.54830 0.60483 11.00000 0.01940 0.01536 0.02242 =
0.00217 0.00634 -0.00386
AFIX 43
H29 2 0.60481 0.55983 0.58358 11.00000 -1.20000
AFIX 0
C30 1 0.46022 0.61467 0.61987 11.00000 0.02847 0.01189 0.02875 =
0.00316 0.00674 -0.00185
AFIX 43
H30 2 0.48105 0.67128 0.60928 11.00000 -1.20000
AFIX 0
C31 1 0.35631 0.59761 0.65045 11.00000 0.02524 0.01198 0.02715 =
-0.00038 0.00474 0.00323
AFIX 43
H31 2 0.30384 0.64197 0.66017 11.00000 -1.20000
AFIX 0
C32 1 0.33061 0.51445 0.66655 11.00000 0.01569 0.01333 0.01853 =
-0.00080 0.00329 0.00121
AFIX 43
H32 2 0.26003 0.50252 0.68836 11.00000 -1.20000
AFIX 0
P1 7 0.99313 0.43138 0.26201 11.00000 0.01551 0.01756 0.01955 =
0.00141 0.00391 0.00237
F1 3 1.02847 0.38028 0.19147 11.00000 0.03625 0.02494 0.02795 =
-0.00539 0.01313 0.00297
F2 3 0.93276 0.34861 0.29223 11.00000 0.03352 0.02324 0.03948 =
0.00519 0.01355 -0.00567
F3 3 1.11514 0.40577 0.30631 11.00000 0.01951 0.04680 0.03065 =
0.01154 0.00311 0.00825
F4 3 1.05445 0.51473 0.23202 11.00000 0.03150 0.02163 0.03674 =
0.00281 0.01156 -0.00340
F5 3 0.87191 0.45841 0.21830 11.00000 0.02143 0.03903 0.03017 =
0.00103 -0.00314 0.00813
F6 3 0.95841 0.48327 0.33275 11.00000 0.02471 0.03733 0.02757 =
-0.01079 0.00889 -0.00282
N1S 5 0.86805 0.18289 0.40373 11.00000 0.05738 0.07724 0.03903 =
0.01920 -0.01388 -0.03324
C1S 1 0.81506 0.18218 0.34781 11.00000 0.02720 0.03167 0.03018 =
0.00528 0.00303 -0.01002
C2S 1 0.74658 0.18213 0.27663 11.00000 0.01886 0.03183 0.02509 =
-0.00108 0.00204 -0.00295
AFIX 137
H2Sa 2 0.76679 0.13224 0.24832 11.00000 -1.50000
H2Sb 2 0.76377 0.23348 0.24931 11.00000 -1.50000
H2Sc 2 0.66294 0.18065 0.28418 11.00000 -1.50000
AFIX 0
HKLF 4
END
;
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_Ir2dpyx2L5_16srv305
_database_code_depnum_ccdc_archive 'CCDC 2006847'
loop_
_audit_author_name
_audit_author_address
'Dmitry Yufit'
;Durham University
United Kingdom
;
_audit_update_record
;
2020-07-07 deposited with the CCDC. 2020-07-10 downloaded from the CCDC.
;
_audit_creation_date 2016-08-17
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.07.26 svn.r3321 for OlexSys, GUI svn.r5206)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C56 H48 Ir2 N10 O2, 2(F6 P), 4(C2 H3 N)'
_chemical_formula_sum 'C64 H60 F12 Ir2 N14 O2 P2'
_chemical_formula_weight 1731.60
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 12.7200(11)
_cell_length_b 14.3155(12)
_cell_length_c 19.9170(17)
_cell_angle_alpha 86.983(3)
_cell_angle_beta 79.538(3)
_cell_angle_gamma 78.218(2)
_cell_volume 3490.9(5)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 9972
_cell_measurement_temperature 120.0
_cell_measurement_theta_max 23.15
_cell_measurement_theta_min 2.41
_shelx_estimated_absorpt_T_max 0.925
_shelx_estimated_absorpt_T_min 0.649
_exptl_absorpt_coefficient_mu 3.939
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.8363
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0709 before and 0.0577 after correction.
The Ratio of minimum to maximum transmission is 0.8363.
The \l/2 correction factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'dull brownish yellow'
_exptl_crystal_colour_lustre dull
_exptl_crystal_colour_modifier brownish
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.647
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 1700
_exptl_crystal_size_max 0.12
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.02
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.1680
_diffrn_reflns_av_unetI/netI 0.2280
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 74344
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.500
_diffrn_reflns_theta_min 2.108
_diffrn_ambient_temperature 120.0
_diffrn_detector 'Bruker PHOTON 100 CMOS'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type 'CMOS sensor'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device '3-circle diffractometer'
_diffrn_measurement_device_type 'Bruker D8 Venture'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator 'focusing mirrors'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_type 'Incoatec I\mS microsource'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 8465
_reflns_number_total 16016
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing.bruker_data_scaling 'SADABS V2012/1 (Bruker AXS Inc.)'
_computing_cell_refinement 'APEX2 v.2013.4_1 (Bruker, 2013)'
_computing_data_collection 'APEX2 v.2013.4_1 (Bruker, 2013)'
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'XS (Sheldrick, 2008)'
_refine_diff_density_max 3.375
_refine_diff_density_min -1.402
_refine_diff_density_rms 0.204
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.958
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 872
_refine_ls_number_reflns 16016
_refine_ls_number_restraints 914
_refine_ls_R_factor_all 0.1517
_refine_ls_R_factor_gt 0.0735
_refine_ls_restrained_S_all 0.949
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0840P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1514
_refine_ls_wR_factor_ref 0.1700
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
N1S-C1S \\sim N4S-C7S \\sim N3S-C5S \\sim N5S-C9S
with sigma of 0.005
C2S-C1S \\sim C8S-C7S \\sim C6S-C5S
with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uiso(C12S) = Uiso(C11S)
4. Rigid body (RIGU) restrains
All non-hydrogen atoms
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{N5S, C9S, C10S} sigma for 1-2: 0.02, 1-3: 0.02
{N4S, C7S, C8S} sigma for 1-2: 0.02, 1-3: 0.02
{N3S, C5S, C6S} sigma for 1-2: 0.02, 1-3: 0.02
{N6S, C11S, C12S} sigma for 1-2: 0.005, 1-3: 0.01
as
{N1S, C1S, C2S}
6. Others
Fixed Sof: N5S(0.7) C9S(0.7) C10S(0.7) H10A(0.7) H10B(0.7) H10C(0.7) N6S(0.3)
C11S(0.3) C12S(0.3) H12D(0.3) H12E(0.3) H12F(0.3)
7.a Aromatic/amide H refined with riding coordinates:
C1(H1), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C11(H11), C13(H13), C14(H14),
C15(H15), C16(H16), C22(H22), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41),
C42(H42), C48(H48), C53(H53), C54(H54), C55(H55), C56(H56)
7.b Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C38(H38A,H38B,
H38C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C2S(H2SA,H2SB,H2SC), C6S(H6SA,
H6SB,H6SC), C8S(H8SA,H8SB,H8SC), C10S(H10A,H10B,H10C), C12S(H12D,H12E,H12F)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.46313(3) 0.17458(3) 0.19088(2) 0.03277(14) Uani 1 1 d . U . . .
Ir2 Ir 0.01350(3) 0.38193(3) 0.30610(2) 0.02817(13) Uani 1 1 d . U . . .
O1 O 0.6043(6) 0.0781(5) 0.1785(4) 0.0453(18) Uani 1 1 d . U . . .
O2 O -0.1356(5) 0.4192(5) 0.3662(3) 0.0369(16) Uani 1 1 d . U . . .
N1 N 0.5059(7) 0.2489(6) 0.1017(4) 0.0340(18) Uani 1 1 d . U . . .
N2 N 0.4269(7) 0.3278(6) 0.0902(4) 0.042(2) Uani 1 1 d . U . . .
N3 N 0.3300(6) 0.2789(5) 0.1908(4) 0.0259(16) Uani 1 1 d . U . . .
N4 N 0.3910(7) 0.0756(6) 0.1560(5) 0.042(2) Uani 1 1 d . U . . .
N5 N 0.5250(6) 0.2473(6) 0.2536(4) 0.0357(18) Uani 1 1 d . U . . .
N6 N 0.1512(6) 0.3588(5) 0.2365(4) 0.0261(16) Uani 1 1 d . U . . .
N7 N 0.0565(7) 0.4826(6) 0.1752(4) 0.0329(19) Uani 1 1 d . U . . .
N8 N -0.0243(6) 0.4865(5) 0.2334(4) 0.0294(17) Uani 1 1 d . U . . .
N9 N -0.0360(6) 0.2701(5) 0.2691(4) 0.0333(18) Uani 1 1 d . U . . .
N10 N 0.0722(6) 0.4626(6) 0.3689(4) 0.0343(18) Uani 1 1 d . U . . .
C1 C 0.6004(8) 0.2327(7) 0.0605(5) 0.036(2) Uani 1 1 d . U . . .
H1 H 0.6130 0.2739 0.0222 0.043 Uiso 1 1 calc R . . . .
C2 C 0.6865(9) 0.1521(8) 0.0724(6) 0.043(2) Uani 1 1 d . U . . .
C3 C 0.6801(9) 0.0801(8) 0.1260(6) 0.045(3) Uani 1 1 d . U . . .
C4 C 0.7728(10) 0.0064(8) 0.1246(7) 0.061(3) Uani 1 1 d . U . . .
H4 H 0.7725 -0.0421 0.1590 0.073 Uiso 1 1 calc R . . . .
C5 C 0.8605(13) 0.0029(12) 0.0765(8) 0.088(4) Uani 1 1 d . U . . .
H5 H 0.9189 -0.0505 0.0759 0.106 Uiso 1 1 calc R . . . .
C6 C 0.8709(12) 0.0762(10) 0.0257(8) 0.079(4) Uani 1 1 d . U . . .
H6 H 0.9367 0.0764 -0.0056 0.095 Uiso 1 1 calc R . . . .
C7 C 0.7800(10) 0.1461(9) 0.0251(7) 0.062(3) Uani 1 1 d . U . . .
H7 H 0.7820 0.1933 -0.0103 0.074 Uiso 1 1 calc R . . . .
C8 C 0.3311(8) 0.3413(7) 0.1355(5) 0.029(2) Uani 1 1 d . U . . .
C9 C 0.2436(8) 0.4105(7) 0.1297(5) 0.037(2) Uani 1 1 d . U . . .
H9 H 0.2457 0.4539 0.0920 0.044 Uiso 1 1 calc R . . . .
C10 C 0.1505(8) 0.4181(7) 0.1791(5) 0.028(2) Uani 1 1 d . U . . .
C11 C 0.2399(7) 0.2917(6) 0.2368(5) 0.0239(19) Uani 1 1 d . U . . .
H11 H 0.2384 0.2479 0.2744 0.029 Uiso 1 1 calc R . . . .
C12 C 0.4476(9) 0.3922(8) 0.0325(5) 0.050(3) Uani 1 1 d . U . . .
H12A H 0.5141 0.4158 0.0344 0.075 Uiso 1 1 calc GR . . . .
H12B H 0.3859 0.4462 0.0344 0.075 Uiso 1 1 calc GR . . . .
H12C H 0.4569 0.3579 -0.0102 0.075 Uiso 1 1 calc GR . . . .
C13 C 0.3770(10) 0.0696(8) 0.0912(7) 0.056(3) Uani 1 1 d . U . . .
H13 H 0.4060 0.1116 0.0577 0.067 Uiso 1 1 calc R . . . .
C14 C 0.3209(12) 0.0031(9) 0.0711(8) 0.074(4) Uani 1 1 d . U . . .
H14 H 0.3113 0.0001 0.0251 0.088 Uiso 1 1 calc R . . . .
C15 C 0.2807(12) -0.0572(10) 0.1208(8) 0.077(4) Uani 1 1 d . U . . .
H15 H 0.2410 -0.1020 0.1097 0.092 Uiso 1 1 calc R . . . .
C16 C 0.2976(10) -0.0529(8) 0.1851(7) 0.063(3) Uani 1 1 d . U . . .
H16 H 0.2703 -0.0964 0.2181 0.075 Uiso 1 1 calc R . . . .
C17 C 0.3542(9) 0.0133(7) 0.2066(6) 0.045(2) Uani 1 1 d . U . . .
C18 C 0.3761(8) 0.0278(7) 0.2732(6) 0.042(2) Uani 1 1 d . U . . .
C19 C 0.4218(8) 0.1083(7) 0.2780(5) 0.036(2) Uani 1 1 d . U . . .
C20 C 0.4500(9) 0.1401(8) 0.3350(6) 0.044(2) Uani 1 1 d . U . . .
C21 C 0.4212(9) 0.0876(9) 0.3967(6) 0.054(3) Uani 1 1 d . U . . .
C22 C 0.3796(9) 0.0069(8) 0.3928(7) 0.055(3) Uani 1 1 d . U . . .
H22 H 0.3630 -0.0277 0.4341 0.066 Uiso 1 1 calc R . . . .
C23 C 0.3598(9) -0.0285(9) 0.3327(7) 0.056(3) Uani 1 1 d . U . . .
C24 C 0.3295(10) -0.1226(8) 0.3380(7) 0.073(4) Uani 1 1 d . U . . .
H24A H 0.2611 -0.1182 0.3209 0.109 Uiso 1 1 calc GR . . . .
H24B H 0.3199 -0.1440 0.3859 0.109 Uiso 1 1 calc GR . . . .
H24C H 0.3873 -0.1684 0.3108 0.109 Uiso 1 1 calc GR . . . .
C25 C 0.4405(11) 0.1157(10) 0.4661(6) 0.071(4) Uani 1 1 d . U . . .
H25A H 0.5186 0.0997 0.4678 0.106 Uiso 1 1 calc GR . . . .
H25B H 0.4010 0.0810 0.5027 0.106 Uiso 1 1 calc GR . . . .
H25C H 0.4141 0.1845 0.4723 0.106 Uiso 1 1 calc GR . . . .
C26 C 0.5076(10) 0.2179(8) 0.3228(6) 0.050(3) Uani 1 1 d . U . . .
C27 C 0.5547(13) 0.2584(10) 0.3659(7) 0.082(5) Uani 1 1 d . U . . .
H27 H 0.5486 0.2368 0.4121 0.098 Uiso 1 1 calc R . . . .
C28 C 0.6118(14) 0.3304(11) 0.3451(7) 0.091(5) Uani 1 1 d . U . . .
H28 H 0.6430 0.3576 0.3773 0.109 Uiso 1 1 calc R . . . .
C29 C 0.6242(12) 0.3638(9) 0.2775(7) 0.068(4) Uani 1 1 d . U . . .
H29 H 0.6605 0.4151 0.2628 0.082 Uiso 1 1 calc R . . . .
C30 C 0.5814(9) 0.3186(8) 0.2344(6) 0.044(3) Uani 1 1 d . U . . .
H30 H 0.5913 0.3377 0.1877 0.053 Uiso 1 1 calc R . . . .
C31 C -0.1077(8) 0.5541(7) 0.2408(5) 0.035(2) Uani 1 1 d . U . . .
H31 H -0.1135 0.6008 0.2052 0.042 Uiso 1 1 calc R . . . .
C32 C -0.1943(8) 0.5645(7) 0.2996(5) 0.037(2) Uani 1 1 d . U . . .
C33 C -0.2026(9) 0.4988(7) 0.3556(5) 0.037(2) Uani 1 1 d . U . . .
C34 C -0.2979(8) 0.5198(8) 0.4075(6) 0.042(3) Uani 1 1 d . U . . .
H34 H -0.3093 0.4756 0.4441 0.050 Uiso 1 1 calc R . . . .
C35 C -0.3731(9) 0.6036(8) 0.4047(7) 0.053(3) Uani 1 1 d . U . . .
H35 H -0.4314 0.6197 0.4420 0.064 Uiso 1 1 calc R . . . .
C36 C -0.3654(9) 0.6640(8) 0.3495(6) 0.048(3) Uani 1 1 d . U . . .
H36 H -0.4217 0.7183 0.3466 0.058 Uiso 1 1 calc R . . . .
C37 C -0.2777(8) 0.6467(8) 0.2987(6) 0.044(3) Uani 1 1 d . U . . .
H37 H -0.2720 0.6908 0.2615 0.053 Uiso 1 1 calc R . . . .
C38 C 0.0390(9) 0.5434(7) 0.1159(5) 0.040(3) Uani 1 1 d . U . . .
H38A H -0.0357 0.5477 0.1082 0.061 Uiso 1 1 calc GR . . . .
H38B H 0.0906 0.5162 0.0757 0.061 Uiso 1 1 calc GR . . . .
H38C H 0.0505 0.6073 0.1239 0.061 Uiso 1 1 calc GR . . . .
C39 C -0.0877(8) 0.2745(8) 0.2153(5) 0.041(3) Uani 1 1 d . U . . .
H39 H -0.1036 0.3336 0.1915 0.049 Uiso 1 1 calc R . . . .
C40 C -0.1172(10) 0.1979(8) 0.1945(7) 0.057(3) Uani 1 1 d . U . . .
H40 H -0.1559 0.2034 0.1574 0.069 Uiso 1 1 calc R . . . .
C41 C -0.0915(11) 0.1119(9) 0.2264(7) 0.064(4) Uani 1 1 d . U . . .
H41 H -0.1118 0.0573 0.2115 0.077 Uiso 1 1 calc R . . . .
C42 C -0.0352(10) 0.1042(8) 0.2815(7) 0.059(3) Uani 1 1 d . U . . .
H42 H -0.0157 0.0440 0.3031 0.071 Uiso 1 1 calc R . . . .
C43 C -0.0083(8) 0.1833(7) 0.3040(5) 0.039(2) Uani 1 1 d . U . . .
C44 C 0.0445(8) 0.1905(7) 0.3633(5) 0.039(2) Uani 1 1 d . U . . .
C45 C 0.0596(8) 0.2830(7) 0.3728(5) 0.034(2) Uani 1 1 d . U . . .
C46 C 0.1011(8) 0.3116(8) 0.4267(5) 0.039(2) Uani 1 1 d . U . . .
C47 C 0.1328(9) 0.2387(9) 0.4740(5) 0.050(3) Uani 1 1 d . U . . .
C48 C 0.1204(9) 0.1488(9) 0.4645(6) 0.051(3) Uani 1 1 d . U . . .
H48 H 0.1427 0.1007 0.4966 0.061 Uiso 1 1 calc R . . . .
C49 C 0.0772(9) 0.1223(8) 0.4106(6) 0.046(3) Uani 1 1 d . U . . .
C50 C 0.0646(11) 0.0189(8) 0.4087(6) 0.067(4) Uani 1 1 d . U . . .
H50A H -0.0124 0.0168 0.4108 0.100 Uiso 1 1 calc GR . . . .
H50B H 0.0910 -0.0165 0.4478 0.100 Uiso 1 1 calc GR . . . .
H50C H 0.1073 -0.0102 0.3662 0.100 Uiso 1 1 calc GR . . . .
C51 C 0.1771(10) 0.2580(10) 0.5386(6) 0.068(4) Uani 1 1 d . U . . .
H51A H 0.2430 0.2847 0.5249 0.101 Uiso 1 1 calc GR . . . .
H51B H 0.1947 0.1981 0.5641 0.101 Uiso 1 1 calc GR . . . .
H51C H 0.1216 0.3035 0.5677 0.101 Uiso 1 1 calc GR . . . .
C52 C 0.1061(9) 0.4119(8) 0.4240(5) 0.043(2) Uani 1 1 d . U . . .
C53 C 0.1355(9) 0.4642(9) 0.4715(6) 0.051(3) Uani 1 1 d . U . . .
H53 H 0.1584 0.4329 0.5112 0.061 Uiso 1 1 calc R . . . .
C54 C 0.1322(10) 0.5593(9) 0.4625(7) 0.060(3) Uani 1 1 d . U . . .
H54 H 0.1529 0.5930 0.4962 0.072 Uiso 1 1 calc R . . . .
C55 C 0.1005(9) 0.6074(8) 0.4075(6) 0.050(3) Uani 1 1 d . U . . .
H55 H 0.1000 0.6736 0.4007 0.060 Uiso 1 1 calc R . . . .
C56 C 0.0690(8) 0.5552(7) 0.3620(6) 0.041(3) Uani 1 1 d . U . . .
H56 H 0.0435 0.5873 0.3233 0.049 Uiso 1 1 calc R . . . .
P1 P 0.2416(3) 0.5441(2) -0.07527(17) 0.0518(9) Uani 1 1 d . U . . .
F1 F 0.3709(5) 0.5122(5) -0.0970(3) 0.0648(19) Uani 1 1 d . U . . .
F2 F 0.2330(6) 0.4439(5) -0.0440(4) 0.076(2) Uani 1 1 d . U . . .
F3 F 0.2250(6) 0.5125(5) -0.1468(4) 0.077(2) Uani 1 1 d . U . . .
F4 F 0.2468(6) 0.6479(5) -0.1048(3) 0.068(2) Uani 1 1 d . U . . .
F5 F 0.2587(5) 0.5770(5) -0.0023(3) 0.0580(17) Uani 1 1 d . U . . .
F6 F 0.1121(6) 0.5764(6) -0.0543(4) 0.084(2) Uani 1 1 d . U . . .
P2 P 0.0145(3) 0.7953(2) 0.2292(2) 0.0706(11) Uani 1 1 d . U . . .
F7 F 0.0738(7) 0.6873(6) 0.2184(4) 0.092(2) Uani 1 1 d . U . . .
F8 F -0.0786(7) 0.7785(6) 0.1906(5) 0.100(3) Uani 1 1 d . U . . .
F9 F -0.0498(8) 0.7594(7) 0.2987(5) 0.111(3) Uani 1 1 d . U . . .
F10 F 0.1043(9) 0.8129(7) 0.2635(6) 0.139(4) Uani 1 1 d . U . . .
F11 F 0.0741(9) 0.8248(9) 0.1594(6) 0.150(4) Uani 1 1 d . U . . .
F12 F -0.0512(9) 0.8962(6) 0.2441(6) 0.134(3) Uani 1 1 d . U . . .
N1S N 0.7403(10) 0.0286(8) 0.4092(6) 0.075(3) Uani 1 1 d D U . . .
C1S C 0.7183(10) -0.0101(9) 0.3672(6) 0.059(3) Uani 1 1 d D U . . .
C2S C 0.6844(10) -0.0578(9) 0.3158(6) 0.072(4) Uani 1 1 d D U . . .
H2SA H 0.6635 -0.0118 0.2800 0.107 Uiso 1 1 calc GR . . . .
H2SB H 0.6219 -0.0862 0.3364 0.107 Uiso 1 1 calc GR . . . .
H2SC H 0.7448 -0.1082 0.2957 0.107 Uiso 1 1 calc GR . . . .
N3S N -0.3770(9) 0.2937(11) 0.5250(7) 0.106(5) Uani 1 1 d D U . . .
C5S C -0.2919(10) 0.2582(10) 0.5003(7) 0.075(4) Uani 1 1 d D U . . .
C6S C -0.1850(9) 0.2164(9) 0.4660(8) 0.088(5) Uani 1 1 d D U . . .
H6SA H -0.1667 0.2526 0.4239 0.131 Uiso 1 1 calc GR . . . .
H6SB H -0.1833 0.1502 0.4548 0.131 Uiso 1 1 calc GR . . . .
H6SC H -0.1319 0.2177 0.4958 0.131 Uiso 1 1 calc GR . . . .
N4S N 0.1481(13) 0.2263(13) 0.1074(8) 0.126(6) Uani 1 1 d D U . . .
C7S C 0.1216(14) 0.2382(12) 0.0557(8) 0.092(5) Uani 1 1 d D U . . .
C8S C 0.0910(19) 0.2561(14) -0.0102(9) 0.152(9) Uani 1 1 d D U . . .
H8SA H 0.1567 0.2529 -0.0451 0.228 Uiso 1 1 calc GR . . . .
H8SB H 0.0446 0.3197 -0.0113 0.228 Uiso 1 1 calc GR . . . .
H8SC H 0.0508 0.2079 -0.0192 0.228 Uiso 1 1 calc GR . . . .
N5S N 0.3239(14) 0.4609(13) 0.2727(9) 0.081(5) Uiso 0.7 1 d D U P A 2
C9S C 0.3569(19) 0.5087(16) 0.3038(12) 0.094(8) Uiso 0.7 1 d D U P A 2
C10S C 0.394(2) 0.560(2) 0.3529(14) 0.159(13) Uiso 0.7 1 d D U P A 2
H10A H 0.4598 0.5819 0.3312 0.239 Uiso 0.7 1 calc GR . P A 2
H10B H 0.4092 0.5171 0.3915 0.239 Uiso 0.7 1 calc GR . P A 2
H10C H 0.3364 0.6147 0.3692 0.239 Uiso 0.7 1 calc GR . P A 2
N6S N 0.341(3) 0.441(3) 0.314(2) 0.080(13) Uiso 0.3 1 d D U P B 1
C11S C 0.376(5) 0.446(7) 0.362(3) 0.19(3) Uiso 0.3 1 d D U P B 1
C12S C 0.436(6) 0.449(6) 0.416(3) 0.19(3) Uiso 0.3 1 d D U P B 1
H12D H 0.5141 0.4347 0.3980 0.284 Uiso 0.3 1 calc GR . P B 1
H12E H 0.4179 0.4018 0.4514 0.284 Uiso 0.3 1 calc GR . P B 1
H12F H 0.4155 0.5129 0.4357 0.284 Uiso 0.3 1 calc GR . P B 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ir1 0.0312(3) 0.0264(2) 0.0406(3) 0.0099(2) -0.0064(2) -0.00808(19)
Ir2 0.0333(3) 0.0250(2) 0.0248(2) 0.00921(17) -0.00502(18) -0.00494(18)
O1 0.039(4) 0.031(4) 0.063(4) 0.016(3) -0.007(3) -0.007(3)
O2 0.035(3) 0.035(3) 0.038(4) 0.003(3) -0.003(3) -0.004(3)
N1 0.033(4) 0.029(4) 0.043(4) 0.007(3) -0.010(3) -0.012(3)
N2 0.041(4) 0.044(4) 0.039(4) 0.016(4) -0.006(3) -0.010(3)
N3 0.038(4) 0.014(3) 0.026(4) 0.004(3) -0.008(3) -0.004(3)
N4 0.036(5) 0.021(4) 0.067(4) 0.004(3) -0.007(4) -0.005(3)
N5 0.024(4) 0.041(4) 0.041(4) 0.009(3) -0.006(3) -0.005(3)
N6 0.031(3) 0.022(3) 0.026(4) 0.006(3) -0.007(3) -0.008(3)
N7 0.035(4) 0.032(4) 0.030(4) 0.012(3) -0.004(3) -0.008(3)
N8 0.031(4) 0.025(4) 0.033(4) 0.008(3) -0.005(3) -0.009(3)
N9 0.030(4) 0.026(3) 0.042(4) 0.009(3) -0.007(3) -0.005(3)
N10 0.034(4) 0.035(4) 0.030(4) -0.002(3) -0.005(3) 0.001(3)
C1 0.035(4) 0.036(5) 0.045(5) -0.005(4) -0.012(4) -0.020(3)
C2 0.040(5) 0.041(5) 0.052(5) -0.001(4) -0.010(4) -0.014(4)
C3 0.042(5) 0.036(5) 0.062(5) 0.000(4) -0.011(4) -0.016(4)
C4 0.052(5) 0.040(6) 0.084(7) 0.005(5) -0.006(5) -0.003(4)
C5 0.077(5) 0.088(5) 0.092(5) 0.009(4) -0.004(4) -0.007(4)
C6 0.069(5) 0.076(5) 0.084(5) 0.006(4) -0.001(4) -0.008(4)
C7 0.049(5) 0.059(6) 0.073(7) 0.010(5) 0.003(5) -0.016(4)
C8 0.038(4) 0.025(4) 0.025(4) 0.010(3) -0.006(3) -0.012(3)
C9 0.041(4) 0.031(5) 0.037(5) 0.017(4) -0.004(3) -0.009(3)
C10 0.034(4) 0.024(4) 0.030(4) 0.008(3) -0.008(3) -0.015(3)
C11 0.031(4) 0.018(4) 0.027(5) 0.003(3) -0.010(3) -0.010(3)
C12 0.054(7) 0.046(6) 0.039(6) 0.024(5) 0.009(5) -0.005(5)
C13 0.072(8) 0.034(6) 0.063(6) 0.003(5) -0.010(5) -0.015(6)
C14 0.094(10) 0.055(7) 0.081(7) -0.006(6) -0.017(6) -0.032(7)
C15 0.089(10) 0.057(8) 0.095(7) 0.004(6) -0.019(7) -0.034(7)
C16 0.069(8) 0.036(6) 0.089(7) 0.003(5) -0.009(6) -0.027(6)
C17 0.038(6) 0.023(5) 0.071(5) 0.007(4) 0.002(4) -0.008(4)
C18 0.029(5) 0.026(4) 0.066(5) 0.014(4) -0.001(4) -0.007(4)
C19 0.029(5) 0.026(4) 0.047(4) 0.017(3) -0.004(3) 0.000(3)
C20 0.041(6) 0.044(5) 0.046(4) 0.017(4) -0.008(4) -0.007(4)
C21 0.047(7) 0.055(6) 0.051(5) 0.025(4) -0.005(4) 0.002(5)
C22 0.039(6) 0.051(6) 0.064(6) 0.029(4) 0.003(5) -0.001(5)
C23 0.040(7) 0.048(5) 0.072(5) 0.028(4) 0.003(5) -0.009(5)
C24 0.062(9) 0.050(6) 0.101(10) 0.037(6) -0.009(7) -0.015(6)
C25 0.071(9) 0.077(9) 0.052(6) 0.022(5) -0.004(6) 0.001(7)
C26 0.061(7) 0.050(6) 0.040(5) 0.012(4) -0.014(4) -0.013(5)
C27 0.137(12) 0.083(9) 0.048(6) 0.027(6) -0.046(7) -0.054(9)
C28 0.146(13) 0.092(10) 0.063(7) 0.025(6) -0.056(7) -0.062(10)
C29 0.101(10) 0.065(8) 0.061(6) 0.020(5) -0.045(6) -0.044(7)
C30 0.041(6) 0.050(6) 0.047(6) 0.013(4) -0.017(5) -0.017(5)
C31 0.037(4) 0.026(5) 0.043(5) 0.001(4) -0.011(4) -0.004(3)
C32 0.031(4) 0.037(5) 0.042(5) 0.001(4) -0.010(3) -0.002(3)
C33 0.041(5) 0.035(4) 0.034(5) -0.008(4) -0.010(4) -0.002(4)
C34 0.035(5) 0.046(5) 0.043(5) -0.009(4) -0.005(4) -0.003(4)
C35 0.038(6) 0.047(6) 0.070(7) -0.009(5) 0.001(5) -0.004(4)
C36 0.030(5) 0.048(6) 0.065(6) -0.003(5) -0.008(4) 0.000(4)
C37 0.034(5) 0.038(5) 0.060(6) 0.001(4) -0.013(4) -0.002(4)
C38 0.045(6) 0.043(6) 0.028(5) 0.017(4) -0.008(4) -0.002(5)
C39 0.045(6) 0.036(5) 0.046(5) 0.012(4) -0.016(5) -0.017(4)
C40 0.062(8) 0.041(5) 0.081(8) 0.007(5) -0.032(7) -0.022(5)
C41 0.083(9) 0.037(5) 0.084(8) 0.012(5) -0.033(7) -0.027(5)
C42 0.069(8) 0.034(5) 0.078(7) 0.006(5) -0.023(6) -0.009(5)
C43 0.041(6) 0.029(4) 0.043(5) 0.012(3) -0.004(4) -0.005(4)
C44 0.032(5) 0.040(4) 0.037(4) 0.011(3) 0.003(4) 0.004(4)
C45 0.027(5) 0.039(4) 0.026(4) 0.014(3) 0.002(3) 0.005(3)
C46 0.034(6) 0.049(4) 0.025(4) 0.010(3) 0.000(4) 0.003(4)
C47 0.044(6) 0.063(5) 0.032(5) 0.022(4) 0.001(4) 0.001(4)
C48 0.044(7) 0.060(5) 0.038(5) 0.022(4) -0.002(5) 0.006(5)
C49 0.040(6) 0.046(5) 0.037(5) 0.018(4) 0.007(4) 0.010(4)
C50 0.085(10) 0.048(5) 0.057(8) 0.025(5) -0.006(7) -0.001(5)
C51 0.071(9) 0.091(9) 0.038(6) 0.027(6) -0.023(6) -0.007(7)
C52 0.044(6) 0.050(4) 0.030(5) 0.005(3) -0.005(4) -0.001(4)
C53 0.059(8) 0.063(5) 0.032(5) 0.002(4) -0.018(5) -0.005(5)
C54 0.059(8) 0.065(6) 0.057(6) -0.003(5) -0.017(6) -0.010(5)
C55 0.058(8) 0.042(5) 0.053(6) -0.009(4) -0.019(5) -0.005(5)
C56 0.044(6) 0.034(4) 0.045(6) -0.002(4) -0.015(5) -0.001(4)
P1 0.053(2) 0.064(2) 0.0465(19) 0.0209(16) -0.0201(16) -0.0265(16)
F1 0.058(4) 0.085(5) 0.053(4) 0.016(3) -0.015(3) -0.019(3)
F2 0.092(5) 0.074(4) 0.072(5) 0.022(3) -0.022(4) -0.043(4)
F3 0.091(5) 0.091(5) 0.058(4) 0.004(4) -0.034(4) -0.022(4)
F4 0.079(5) 0.070(4) 0.062(4) 0.029(3) -0.025(4) -0.027(3)
F5 0.065(4) 0.066(4) 0.047(3) 0.012(3) -0.015(3) -0.024(3)
F6 0.057(4) 0.113(6) 0.085(5) 0.021(4) -0.014(3) -0.027(4)
P2 0.071(3) 0.0378(19) 0.110(3) 0.014(2) -0.024(2) -0.0239(17)
F7 0.111(6) 0.064(4) 0.103(6) 0.010(4) -0.024(5) -0.021(4)
F8 0.106(6) 0.086(6) 0.120(6) 0.026(5) -0.044(5) -0.037(5)
F9 0.107(6) 0.103(6) 0.116(6) 0.019(5) -0.022(5) -0.010(5)
F10 0.129(7) 0.104(7) 0.213(9) 0.003(6) -0.082(6) -0.044(5)
F11 0.131(7) 0.172(9) 0.156(7) 0.068(6) -0.024(5) -0.066(6)
F12 0.144(7) 0.057(5) 0.209(9) -0.002(5) -0.069(6) -0.006(4)
N1S 0.076(8) 0.070(8) 0.077(8) 0.019(6) -0.005(6) -0.020(7)
C1S 0.052(8) 0.047(8) 0.069(9) 0.021(6) 0.001(6) -0.004(6)
C2S 0.060(9) 0.070(9) 0.077(9) 0.009(7) -0.010(7) 0.002(7)
N3S 0.063(7) 0.146(13) 0.083(10) -0.014(9) 0.015(6) 0.017(7)
C5S 0.062(7) 0.086(10) 0.058(9) 0.005(8) 0.015(6) 0.006(7)
C6S 0.060(7) 0.055(9) 0.130(13) -0.021(9) 0.035(8) -0.012(6)
N4S 0.093(12) 0.162(16) 0.123(12) -0.015(11) -0.022(10) -0.020(11)
C7S 0.083(12) 0.073(11) 0.115(12) -0.026(10) -0.013(10) -0.003(9)
C8S 0.23(3) 0.094(15) 0.137(14) -0.013(12) -0.070(14) -0.016(16)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 O1 2.013(7) . ?
Ir1 N1 2.066(8) . ?
Ir1 N3 2.017(7) . ?
Ir1 N4 2.049(9) . ?
Ir1 N5 2.023(8) . ?
Ir1 C19 1.971(10) . ?
Ir2 O2 2.036(7) . ?
Ir2 N6 2.007(8) . ?
Ir2 N8 2.074(7) . ?
Ir2 N9 2.051(8) . ?
Ir2 N10 2.073(8) . ?
Ir2 C45 1.966(9) . ?
O1 C3 1.290(13) . ?
O2 C33 1.308(11) . ?
N1 N2 1.390(11) . ?
N1 C1 1.312(12) . ?
N2 C8 1.364(12) . ?
N2 C12 1.455(12) . ?
N3 C8 1.380(11) . ?
N3 C11 1.319(11) . ?
N4 C13 1.344(14) . ?
N4 C17 1.391(13) . ?
N5 C26 1.411(13) . ?
N5 C30 1.365(12) . ?
N6 C10 1.387(11) . ?
N6 C11 1.325(11) . ?
N7 N8 1.398(10) . ?
N7 C10 1.365(12) . ?
N7 C38 1.453(11) . ?
N8 C31 1.273(12) . ?
N9 C39 1.349(12) . ?
N9 C43 1.403(12) . ?
N10 C52 1.370(12) . ?
N10 C56 1.318(12) . ?
C1 H1 0.9500 . ?
C1 C2 1.461(15) . ?
C2 C3 1.447(15) . ?
C2 C7 1.368(15) . ?
C3 C4 1.410(15) . ?
C4 H4 0.9500 . ?
C4 C5 1.325(17) . ?
C5 H5 0.9500 . ?
C5 C6 1.428(19) . ?
C6 H6 0.9500 . ?
C6 C7 1.368(17) . ?
C7 H7 0.9500 . ?
C8 C9 1.349(13) . ?
C9 H9 0.9500 . ?
C9 C10 1.384(13) . ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13 0.9500 . ?
C13 C14 1.414(16) . ?
C14 H14 0.9500 . ?
C14 C15 1.376(18) . ?
C15 H15 0.9500 . ?
C15 C16 1.342(17) . ?
C16 H16 0.9500 . ?
C16 C17 1.426(15) . ?
C17 C18 1.437(16) . ?
C18 C19 1.407(14) . ?
C18 C23 1.406(15) . ?
C19 C20 1.377(15) . ?
C20 C21 1.435(14) . ?
C20 C26 1.442(15) . ?
C21 C22 1.376(16) . ?
C21 C25 1.536(16) . ?
C22 H22 0.9500 . ?
C22 C23 1.407(17) . ?
C23 C24 1.468(15) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.347(16) . ?
C27 H27 0.9500 . ?
C27 C28 1.382(18) . ?
C28 H28 0.9500 . ?
C28 C29 1.398(17) . ?
C29 H29 0.9500 . ?
C29 C30 1.350(15) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C31 C32 1.446(14) . ?
C32 C33 1.425(14) . ?
C32 C37 1.417(14) . ?
C33 C34 1.434(14) . ?
C34 H34 0.9500 . ?
C34 C35 1.379(15) . ?
C35 H35 0.9500 . ?
C35 C36 1.366(16) . ?
C36 H36 0.9500 . ?
C36 C37 1.354(15) . ?
C37 H37 0.9500 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39 0.9500 . ?
C39 C40 1.336(14) . ?
C40 H40 0.9500 . ?
C40 C41 1.363(15) . ?
C41 H41 0.9500 . ?
C41 C42 1.403(16) . ?
C42 H42 0.9500 . ?
C42 C43 1.367(15) . ?
C43 C44 1.479(14) . ?
C44 C45 1.402(14) . ?
C44 C49 1.376(14) . ?
C45 C46 1.392(14) . ?
C46 C47 1.414(14) . ?
C46 C52 1.449(15) . ?
C47 C48 1.355(16) . ?
C47 C51 1.556(16) . ?
C48 H48 0.9500 . ?
C48 C49 1.393(16) . ?
C49 C50 1.525(16) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 C53 1.383(15) . ?
C53 H53 0.9500 . ?
C53 C54 1.357(16) . ?
C54 H54 0.9500 . ?
C54 C55 1.343(15) . ?
C55 H55 0.9500 . ?
C55 C56 1.365(14) . ?
C56 H56 0.9500 . ?
P1 F1 1.599(7) . ?
P1 F2 1.550(7) . ?
P1 F3 1.578(7) . ?
P1 F4 1.578(7) . ?
P1 F5 1.616(7) . ?
P1 F6 1.600(8) . ?
P2 F7 1.583(8) . ?
P2 F8 1.585(9) . ?
P2 F9 1.593(10) . ?
P2 F10 1.503(10) . ?
P2 F11 1.539(11) . ?
P2 F12 1.529(9) . ?
N1S C1S 1.133(10) . ?
C1S C2S 1.434(11) . ?
C2S H2SA 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?
N3S C5S 1.132(10) . ?
C5S C6S 1.430(11) . ?
C6S H6SA 0.9800 . ?
C6S H6SB 0.9800 . ?
C6S H6SC 0.9800 . ?
N4S C7S 1.134(10) . ?
C7S C8S 1.432(11) . ?
C8S H8SA 0.9800 . ?
C8S H8SB 0.9800 . ?
C8S H8SC 0.9800 . ?
N5S C9S 1.133(10) . ?
C9S C10S 1.444(15) . ?
C10S H10A 0.9800 . ?
C10S H10B 0.9800 . ?
C10S H10C 0.9800 . ?
N6S C11S 1.134(10) . ?
C11S C12S 1.433(11) . ?
C12S H12D 0.9800 . ?
C12S H12E 0.9800 . ?
C12S H12F 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ir1 N1 94.2(3) . . ?
O1 Ir1 N3 172.1(3) . . ?
O1 Ir1 N4 88.6(3) . . ?
O1 Ir1 N5 88.7(3) . . ?
N3 Ir1 N1 77.9(3) . . ?
N3 Ir1 N4 92.6(3) . . ?
N3 Ir1 N5 92.6(3) . . ?
N4 Ir1 N1 101.0(3) . . ?
N5 Ir1 N1 97.6(3) . . ?
N5 Ir1 N4 161.3(4) . . ?
C19 Ir1 O1 86.9(3) . . ?
C19 Ir1 N1 177.7(4) . . ?
C19 Ir1 N3 101.0(3) . . ?
C19 Ir1 N4 80.9(4) . . ?
C19 Ir1 N5 80.4(4) . . ?
O2 Ir2 N8 92.8(3) . . ?
O2 Ir2 N9 89.9(3) . . ?
O2 Ir2 N10 87.7(3) . . ?
N6 Ir2 O2 171.5(3) . . ?
N6 Ir2 N8 78.7(3) . . ?
N6 Ir2 N9 90.4(3) . . ?
N6 Ir2 N10 94.7(3) . . ?
N9 Ir2 N8 100.4(3) . . ?
N9 Ir2 N10 161.2(3) . . ?
N10 Ir2 N8 98.3(3) . . ?
C45 Ir2 O2 90.7(3) . . ?
C45 Ir2 N6 97.8(3) . . ?
C45 Ir2 N8 176.2(3) . . ?
C45 Ir2 N9 81.1(4) . . ?
C45 Ir2 N10 80.3(4) . . ?
C3 O1 Ir1 122.1(7) . . ?
C33 O2 Ir2 121.5(6) . . ?
N2 N1 Ir1 113.7(6) . . ?
C1 N1 Ir1 126.4(7) . . ?
C1 N1 N2 119.7(9) . . ?
N1 N2 C12 120.6(8) . . ?
C8 N2 N1 116.7(8) . . ?
C8 N2 C12 122.7(9) . . ?
C8 N3 Ir1 116.9(6) . . ?
C11 N3 Ir1 126.7(6) . . ?
C11 N3 C8 116.4(8) . . ?
C13 N4 Ir1 125.1(7) . . ?
C13 N4 C17 121.1(10) . . ?
C17 N4 Ir1 113.7(8) . . ?
C26 N5 Ir1 114.6(7) . . ?
C30 N5 Ir1 126.0(7) . . ?
C30 N5 C26 119.4(9) . . ?
C10 N6 Ir2 115.3(6) . . ?
C11 N6 Ir2 128.4(6) . . ?
C11 N6 C10 116.2(8) . . ?
N8 N7 C38 121.2(8) . . ?
C10 N7 N8 114.9(7) . . ?
C10 N7 C38 123.9(8) . . ?
N7 N8 Ir2 113.6(6) . . ?
C31 N8 Ir2 125.4(7) . . ?
C31 N8 N7 120.7(8) . . ?
C39 N9 Ir2 125.6(7) . . ?
C39 N9 C43 120.6(9) . . ?
C43 N9 Ir2 113.9(7) . . ?
C52 N10 Ir2 113.1(7) . . ?
C56 N10 Ir2 125.2(7) . . ?
C56 N10 C52 121.5(9) . . ?
N1 C1 H1 119.5 . . ?
N1 C1 C2 121.1(10) . . ?
C2 C1 H1 119.5 . . ?
C3 C2 C1 127.0(10) . . ?
C7 C2 C1 113.5(11) . . ?
C7 C2 C3 119.4(11) . . ?
O1 C3 C2 128.6(11) . . ?
O1 C3 C4 114.9(11) . . ?
C4 C3 C2 116.2(11) . . ?
C3 C4 H4 119.1 . . ?
C5 C4 C3 121.9(14) . . ?
C5 C4 H4 119.1 . . ?
C4 C5 H5 118.7 . . ?
C4 C5 C6 122.7(15) . . ?
C6 C5 H5 118.7 . . ?
C5 C6 H6 122.1 . . ?
C7 C6 C5 115.7(14) . . ?
C7 C6 H6 122.1 . . ?
C2 C7 H7 118.1 . . ?
C6 C7 C2 123.8(13) . . ?
C6 C7 H7 118.1 . . ?
N2 C8 N3 114.6(9) . . ?
C9 C8 N2 124.5(9) . . ?
C9 C8 N3 120.9(9) . . ?
C8 C9 H9 120.2 . . ?
C8 C9 C10 119.7(9) . . ?
C10 C9 H9 120.2 . . ?
N7 C10 N6 117.1(8) . . ?
N7 C10 C9 123.4(9) . . ?
C9 C10 N6 119.5(9) . . ?
N3 C11 N6 127.1(8) . . ?
N3 C11 H11 116.4 . . ?
N6 C11 H11 116.4 . . ?
N2 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
N2 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 H13 118.8 . . ?
N4 C13 C14 122.4(12) . . ?
C14 C13 H13 118.8 . . ?
C13 C14 H14 121.3 . . ?
C15 C14 C13 117.3(14) . . ?
C15 C14 H14 121.3 . . ?
C14 C15 H15 120.0 . . ?
C16 C15 C14 120.0(13) . . ?
C16 C15 H15 120.0 . . ?
C15 C16 H16 118.1 . . ?
C15 C16 C17 123.7(12) . . ?
C17 C16 H16 118.1 . . ?
N4 C17 C16 115.2(11) . . ?
N4 C17 C18 114.7(9) . . ?
C16 C17 C18 130.0(10) . . ?
C19 C18 C17 114.7(9) . . ?
C23 C18 C17 128.5(11) . . ?
C23 C18 C19 116.8(11) . . ?
C18 C19 Ir1 115.5(8) . . ?
C20 C19 Ir1 116.8(7) . . ?
C20 C19 C18 127.4(10) . . ?
C19 C20 C21 114.6(10) . . ?
C19 C20 C26 115.0(10) . . ?
C21 C20 C26 130.4(11) . . ?
C20 C21 C25 122.1(11) . . ?
C22 C21 C20 118.8(12) . . ?
C22 C21 C25 119.0(11) . . ?
C21 C22 H22 117.4 . . ?
C21 C22 C23 125.3(11) . . ?
C23 C22 H22 117.4 . . ?
C18 C23 C22 116.6(11) . . ?
C18 C23 C24 126.8(13) . . ?
C22 C23 C24 116.5(11) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 H25A 109.5 . . ?
C21 C25 H25B 109.5 . . ?
C21 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N5 C26 C20 113.2(10) . . ?
C27 C26 N5 117.2(11) . . ?
C27 C26 C20 129.2(11) . . ?
C26 C27 H27 119.0 . . ?
C26 C27 C28 122.1(12) . . ?
C28 C27 H27 119.0 . . ?
C27 C28 H28 119.5 . . ?
C27 C28 C29 121.1(13) . . ?
C29 C28 H28 119.5 . . ?
C28 C29 H29 122.1 . . ?
C30 C29 C28 115.7(12) . . ?
C30 C29 H29 122.1 . . ?
N5 C30 H30 117.8 . . ?
C29 C30 N5 124.3(11) . . ?
C29 C30 H30 117.8 . . ?
N8 C31 H31 117.8 . . ?
N8 C31 C32 124.4(10) . . ?
C32 C31 H31 117.8 . . ?
C33 C32 C31 125.6(10) . . ?
C37 C32 C31 115.3(10) . . ?
C37 C32 C33 119.1(10) . . ?
O2 C33 C32 128.8(10) . . ?
O2 C33 C34 114.2(10) . . ?
C32 C33 C34 117.0(10) . . ?
C33 C34 H34 119.7 . . ?
C35 C34 C33 120.5(11) . . ?
C35 C34 H34 119.7 . . ?
C34 C35 H35 119.3 . . ?
C36 C35 C34 121.3(12) . . ?
C36 C35 H35 119.3 . . ?
C35 C36 H36 119.9 . . ?
C37 C36 C35 120.1(11) . . ?
C37 C36 H36 119.9 . . ?
C32 C37 H37 119.2 . . ?
C36 C37 C32 121.6(11) . . ?
C36 C37 H37 119.2 . . ?
N7 C38 H38A 109.5 . . ?
N7 C38 H38B 109.5 . . ?
N7 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N9 C39 H39 119.2 . . ?
C40 C39 N9 121.7(10) . . ?
C40 C39 H39 119.2 . . ?
C39 C40 H40 120.1 . . ?
C39 C40 C41 119.9(12) . . ?
C41 C40 H40 120.1 . . ?
C40 C41 H41 120.0 . . ?
C40 C41 C42 119.9(12) . . ?
C42 C41 H41 120.0 . . ?
C41 C42 H42 120.0 . . ?
C43 C42 C41 120.0(11) . . ?
C43 C42 H42 120.0 . . ?
N9 C43 C44 114.2(9) . . ?
C42 C43 N9 117.9(10) . . ?
C42 C43 C44 127.8(10) . . ?
C45 C44 C43 113.4(9) . . ?
C49 C44 C43 130.2(11) . . ?
C49 C44 C45 116.4(11) . . ?
C44 C45 Ir2 117.2(8) . . ?
C46 C45 Ir2 117.0(8) . . ?
C46 C45 C44 125.7(9) . . ?
C45 C46 C47 115.5(11) . . ?
C45 C46 C52 113.7(9) . . ?
C47 C46 C52 130.8(11) . . ?
C46 C47 C51 122.6(11) . . ?
C48 C47 C46 119.3(12) . . ?
C48 C47 C51 118.1(10) . . ?
C47 C48 H48 117.9 . . ?
C47 C48 C49 124.1(11) . . ?
C49 C48 H48 117.9 . . ?
C44 C49 C48 119.0(11) . . ?
C44 C49 C50 123.2(11) . . ?
C48 C49 C50 117.7(10) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C47 C51 H51A 109.5 . . ?
C47 C51 H51B 109.5 . . ?
C47 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N10 C52 C46 115.8(10) . . ?
N10 C52 C53 115.7(10) . . ?
C53 C52 C46 128.4(10) . . ?
C52 C53 H53 119.4 . . ?
C54 C53 C52 121.2(11) . . ?
C54 C53 H53 119.4 . . ?
C53 C54 H54 119.0 . . ?
C55 C54 C53 122.1(12) . . ?
C55 C54 H54 119.0 . . ?
C54 C55 H55 122.0 . . ?
C54 C55 C56 115.9(11) . . ?
C56 C55 H55 122.0 . . ?
N10 C56 C55 123.5(10) . . ?
N10 C56 H56 118.2 . . ?
C55 C56 H56 118.2 . . ?
F1 P1 F5 89.5(4) . . ?
F1 P1 F6 179.4(4) . . ?
F2 P1 F1 91.3(4) . . ?
F2 P1 F3 91.1(4) . . ?
F2 P1 F4 177.8(5) . . ?
F2 P1 F5 89.3(4) . . ?
F2 P1 F6 89.1(4) . . ?
F3 P1 F1 90.5(4) . . ?
F3 P1 F4 90.2(4) . . ?
F3 P1 F5 179.6(4) . . ?
F3 P1 F6 89.1(4) . . ?
F4 P1 F1 90.5(4) . . ?
F4 P1 F5 89.4(4) . . ?
F4 P1 F6 89.1(4) . . ?
F6 P1 F5 91.0(4) . . ?
F7 P2 F8 90.4(5) . . ?
F7 P2 F9 86.0(5) . . ?
F8 P2 F9 89.8(5) . . ?
F10 P2 F7 90.2(5) . . ?
F10 P2 F8 178.0(6) . . ?
F10 P2 F9 92.2(6) . . ?
F10 P2 F11 90.9(6) . . ?
F10 P2 F12 92.0(6) . . ?
F11 P2 F7 91.7(6) . . ?
F11 P2 F8 87.2(6) . . ?
F11 P2 F9 176.1(6) . . ?
F12 P2 F7 174.7(6) . . ?
F12 P2 F8 87.7(5) . . ?
F12 P2 F9 89.0(6) . . ?
F12 P2 F11 93.2(7) . . ?
N1S C1S C2S 176.9(16) . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
N3S C5S C6S 177.0(17) . . ?
C5S C6S H6SA 109.5 . . ?
C5S C6S H6SB 109.5 . . ?
C5S C6S H6SC 109.5 . . ?
H6SA C6S H6SB 109.5 . . ?
H6SA C6S H6SC 109.5 . . ?
H6SB C6S H6SC 109.5 . . ?
N4S C7S C8S 178(2) . . ?
C7S C8S H8SA 109.5 . . ?
C7S C8S H8SB 109.5 . . ?
C7S C8S H8SC 109.5 . . ?
H8SA C8S H8SB 109.5 . . ?
H8SA C8S H8SC 109.5 . . ?
H8SB C8S H8SC 109.5 . . ?
N5S C9S C10S 171(3) . . ?
C9S C10S H10A 109.5 . . ?
C9S C10S H10B 109.5 . . ?
C9S C10S H10C 109.5 . . ?
H10A C10S H10B 109.5 . . ?
H10A C10S H10C 109.5 . . ?
H10B C10S H10C 109.5 . . ?
N6S C11S C12S 172(6) . . ?
C11S C12S H12D 109.5 . . ?
C11S C12S H12E 109.5 . . ?
C11S C12S H12F 109.5 . . ?
H12D C12S H12E 109.5 . . ?
H12D C12S H12F 109.5 . . ?
H12E C12S H12F 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N6 C10 N7 N8 5.8(12) . . . . ?
C1 N1 N2 C8 -179.1(9) . . . . ?
C1 N1 N2 C12 0.5(14) . . . . ?
C2 C1 N1 Ir1 4.0(13) . . . . ?
C2 C1 N1 N2 178.0(9) . . . . ?
C3 C2 C1 N1 2.9(17) . . . . ?
C7 C2 C1 N1 -179.3(10) . . . . ?
C8 N2 N1 Ir1 -4.5(11) . . . . ?
C9 C10 N7 N8 -173.2(9) . . . . ?
C9 C10 N7 C38 6.9(15) . . . . ?
C10 N7 N8 Ir2 -6.7(10) . . . . ?
C10 N7 N8 C31 168.1(9) . . . . ?
C12 N2 N1 Ir1 175.2(8) . . . . ?
C16 C17 C18 C19 -171.9(11) . . . . ?
C16 C17 C18 C23 9(2) . . . . ?
C19 C18 C17 N4 5.8(14) . . . . ?
C19 C20 C26 N5 -0.2(15) . . . . ?
C19 C20 C26 C27 -173.1(14) . . . . ?
C21 C20 C26 N5 176.9(11) . . . . ?
C21 C20 C26 C27 4(2) . . . . ?
C23 C18 C17 N4 -172.9(10) . . . . ?
C31 N8 N7 C38 -12.1(13) . . . . ?
C32 C31 N8 Ir2 -4.9(14) . . . . ?
C32 C31 N8 N7 -179.1(9) . . . . ?
C38 N7 N8 Ir2 173.2(7) . . . . ?
C38 N7 C10 N6 -174.1(9) . . . . ?
C42 C43 C44 C45 -179.3(11) . . . . ?
C42 C43 C44 C49 -1.5(19) . . . . ?
C45 C44 C43 N9 -1.4(13) . . . . ?
C45 C46 C52 N10 -1.3(14) . . . . ?
C45 C46 C52 C53 175.0(11) . . . . ?
C47 C46 C52 N10 177.4(10) . . . . ?
C47 C46 C52 C53 -6(2) . . . . ?
C49 C44 C43 N9 176.4(10) . . . . ?
_shelx_SHELXL_version_number 2014/7
_iucr_refine_instructions_details
;
TITL 16srv305 in P-1 #2
REM reset to P-1 #2
CELL 0.71073 12.72 14.3155 19.917 86.983 79.5381 78.2177
ZERR 2 0.0011 0.0012 0.0017 0.0025 0.0025 0.0024
LATT 1
SFAC C H F Ir N O P
UNIT 128 120 24 4 28 4 4
SADI 0.005 N1S C1S N4S C7S N3S C5S N5S C9S
SADI 0.005 C2S C1S C8S C7S C6S C5S
RIGU
ISOR 0.005 0.01 C5 C6
EADP C12S C11S
L.S. 9
PLAN 5
SIZE 0.02 0.09 0.12
TEMP -153.15
CONF C3 C2 C1 N1
CONF C7 C2 C1 N1
CONF C2 C1 N1 Ir1
CONF C2 C1 N1 N2
CONF C8 N2 N1 Ir1
CONF C1 N1 N2 C8
CONF C12 N2 N1 Ir1
CONF C1 N1 N2 C12
CONF N6 C10 N7 N8
CONF C9 C10 N7 N8
CONF C38 N7 C10 N6
CONF C9 C10 N7 C38
CONF C10 N7 N8 Ir2
CONF C38 N7 N8 Ir2
CONF C10 N7 N8 C31
CONF C31 N8 N7 C38
CONF C32 C31 N8 Ir2
CONF C32 C31 N8 N7
CONF C19 C20 C26 N5
CONF C21 C20 C26 N5
CONF C19 C20 C26 C27
CONF C21 C20 C26 C27
CONF C19 C18 C17 N4
CONF C16 C17 C18 C19
CONF C23 C18 C17 N4
CONF C16 C17 C18 C23
CONF C45 C44 C43 N9
CONF C42 C43 C44 C45
CONF C49 C44 C43 N9
CONF C42 C43 C44 C49
CONF C45 C46 C52 N10
CONF C47 C46 C52 N10
CONF C45 C46 C52 C53
CONF C47 C46 C52 C53
BOND $h
fmap 2
acta
OMIT -2 55
OMIT 1 1 0
OMIT 0 1 2
OMIT -1 -1 1
OMIT 0 -2 1
OMIT -1 0 2
OMIT 1 0 2
WGHT 0.084
FVAR 0.06113
REM
REM
REM
Ir1 4 0.46313 0.17458 0.19088 11.00000 0.03115 0.02644 0.04064 =
0.00988 -0.00638 -0.00808
Ir2 4 0.01350 0.38193 0.30610 11.00000 0.03330 0.02498 0.02481 =
0.00921 -0.00502 -0.00494
O1 6 0.60430 0.07814 0.17846 11.00000 0.03924 0.03070 0.06345 =
0.01598 -0.00712 -0.00670
O2 6 -0.13562 0.41921 0.36622 11.00000 0.03494 0.03458 0.03812 =
0.00346 -0.00311 -0.00387
N1 5 0.50590 0.24891 0.10174 11.00000 0.03271 0.02944 0.04282 =
0.00658 -0.00971 -0.01233
N2 5 0.42692 0.32784 0.09021 11.00000 0.04054 0.04363 0.03909 =
0.01623 -0.00590 -0.00960
N3 5 0.32997 0.27892 0.19076 11.00000 0.03753 0.01399 0.02634 =
0.00428 -0.00833 -0.00426
N4 5 0.39096 0.07562 0.15604 11.00000 0.03641 0.02077 0.06676 =
0.00441 -0.00684 -0.00467
N5 5 0.52504 0.24730 0.25359 11.00000 0.02400 0.04077 0.04072 =
0.00917 -0.00602 -0.00465
N6 5 0.15124 0.35883 0.23651 11.00000 0.03105 0.02218 0.02628 =
0.00599 -0.00660 -0.00815
N7 5 0.05654 0.48256 0.17521 11.00000 0.03483 0.03192 0.03047 =
0.01190 -0.00414 -0.00794
N8 5 -0.02434 0.48652 0.23338 11.00000 0.03120 0.02451 0.03289 =
0.00798 -0.00547 -0.00862
N9 5 -0.03598 0.27011 0.26913 11.00000 0.03023 0.02649 0.04219 =
0.00939 -0.00685 -0.00517
N10 5 0.07215 0.46262 0.36888 11.00000 0.03416 0.03513 0.02999 =
-0.00177 -0.00483 0.00112
C1 1 0.60038 0.23266 0.06047 11.00000 0.03529 0.03596 0.04522 =
-0.00457 -0.01219 -0.01966
AFIX 43
H1 2 0.61302 0.27391 0.02220 11.00000 -1.20000
AFIX 0
C2 1 0.68646 0.15214 0.07243 11.00000 0.03970 0.04137 0.05194 =
-0.00098 -0.01033 -0.01436
C3 1 0.68008 0.08010 0.12596 11.00000 0.04206 0.03565 0.06218 =
0.00049 -0.01105 -0.01607
C4 1 0.77285 0.00642 0.12456 11.00000 0.05170 0.04046 0.08394 =
0.00481 -0.00577 -0.00300
AFIX 43
H4 2 0.77247 -0.04207 0.15900 11.00000 -1.20000
AFIX 0
C5 1 0.86055 0.00292 0.07654 11.00000 0.07653 0.08756 0.09173 =
0.00902 -0.00353 -0.00707
AFIX 43
H5 2 0.91890 -0.05054 0.07590 11.00000 -1.20000
AFIX 0
C6 1 0.87091 0.07620 0.02573 11.00000 0.06919 0.07625 0.08416 =
0.00553 -0.00061 -0.00828
AFIX 43
H6 2 0.93675 0.07636 -0.00564 11.00000 -1.20000
AFIX 0
C7 1 0.78002 0.14615 0.02510 11.00000 0.04889 0.05898 0.07292 =
0.01046 0.00287 -0.01570
AFIX 43
H7 2 0.78197 0.19330 -0.01025 11.00000 -1.20000
AFIX 0
C8 1 0.33112 0.34130 0.13554 11.00000 0.03803 0.02539 0.02461 =
0.00995 -0.00622 -0.01173
C9 1 0.24356 0.41051 0.12975 11.00000 0.04098 0.03068 0.03677 =
0.01719 -0.00371 -0.00883
AFIX 43
H9 2 0.24574 0.45386 0.09196 11.00000 -1.20000
AFIX 0
C10 1 0.15052 0.41807 0.17913 11.00000 0.03440 0.02426 0.02953 =
0.00836 -0.00816 -0.01544
C11 1 0.23988 0.29166 0.23685 11.00000 0.03124 0.01753 0.02680 =
0.00276 -0.01023 -0.01032
AFIX 43
H11 2 0.23838 0.24790 0.27439 11.00000 -1.20000
AFIX 0
C12 1 0.44765 0.39216 0.03250 11.00000 0.05405 0.04567 0.03926 =
0.02427 0.00911 -0.00457
AFIX 137
H12A 2 0.51415 0.41576 0.03437 11.00000 -1.50000
H12B 2 0.38587 0.44615 0.03443 11.00000 -1.50000
H12C 2 0.45688 0.35792 -0.01016 11.00000 -1.50000
AFIX 0
C13 1 0.37703 0.06959 0.09121 11.00000 0.07206 0.03380 0.06261 =
0.00290 -0.00973 -0.01526
AFIX 43
H13 2 0.40597 0.11160 0.05766 11.00000 -1.20000
AFIX 0
C14 1 0.32090 0.00307 0.07110 11.00000 0.09372 0.05467 0.08097 =
-0.00610 -0.01666 -0.03210
AFIX 43
H14 2 0.31130 0.00012 0.02511 11.00000 -1.20000
AFIX 0
C15 1 0.28072 -0.05723 0.12083 11.00000 0.08864 0.05662 0.09457 =
0.00386 -0.01904 -0.03414
AFIX 43
H15 2 0.24102 -0.10197 0.10967 11.00000 -1.20000
AFIX 0
C16 1 0.29758 -0.05289 0.18506 11.00000 0.06916 0.03555 0.08879 =
0.00342 -0.00896 -0.02706
AFIX 43
H16 2 0.27027 -0.09637 0.21805 11.00000 -1.20000
AFIX 0
C17 1 0.35416 0.01329 0.20663 11.00000 0.03808 0.02277 0.07061 =
0.00692 0.00201 -0.00819
C18 1 0.37606 0.02780 0.27319 11.00000 0.02895 0.02616 0.06625 =
0.01423 -0.00132 -0.00696
C19 1 0.42185 0.10827 0.27796 11.00000 0.02883 0.02612 0.04670 =
0.01729 -0.00403 -0.00029
C20 1 0.45004 0.14006 0.33503 11.00000 0.04065 0.04357 0.04592 =
0.01710 -0.00840 -0.00681
C21 1 0.42116 0.08762 0.39668 11.00000 0.04692 0.05539 0.05135 =
0.02479 -0.00543 0.00212
C22 1 0.37963 0.00689 0.39282 11.00000 0.03884 0.05118 0.06410 =
0.02918 0.00296 -0.00109
AFIX 43
H22 2 0.36303 -0.02774 0.43408 11.00000 -1.20000
AFIX 0
C23 1 0.35975 -0.02850 0.33271 11.00000 0.04040 0.04827 0.07167 =
0.02810 0.00288 -0.00897
C24 1 0.32952 -0.12259 0.33804 11.00000 0.06245 0.05046 0.10101 =
0.03749 -0.00899 -0.01542
AFIX 137
H24A 2 0.26113 -0.11820 0.32091 11.00000 -1.50000
H24B 2 0.31992 -0.14396 0.38592 11.00000 -1.50000
H24C 2 0.38733 -0.16843 0.31084 11.00000 -1.50000
AFIX 0
C25 1 0.44046 0.11573 0.46613 11.00000 0.07149 0.07659 0.05212 =
0.02173 -0.00433 0.00091
AFIX 137
H25A 2 0.51864 0.09965 0.46776 11.00000 -1.50000
H25B 2 0.40097 0.08096 0.50265 11.00000 -1.50000
H25C 2 0.41408 0.18453 0.47231 11.00000 -1.50000
AFIX 0
C26 1 0.50764 0.21792 0.32277 11.00000 0.06051 0.04959 0.04026 =
0.01240 -0.01428 -0.01314
C27 1 0.55475 0.25839 0.36593 11.00000 0.13712 0.08278 0.04806 =
0.02666 -0.04630 -0.05413
AFIX 43
H27 2 0.54859 0.23677 0.41213 11.00000 -1.20000
AFIX 0
C28 1 0.61177 0.33039 0.34513 11.00000 0.14638 0.09230 0.06339 =
0.02453 -0.05647 -0.06211
AFIX 43
H28 2 0.64301 0.35758 0.37732 11.00000 -1.20000
AFIX 0
C29 1 0.62422 0.36383 0.27748 11.00000 0.10113 0.06491 0.06059 =
0.02020 -0.04502 -0.04399
AFIX 43
H29 2 0.66045 0.41506 0.26278 11.00000 -1.20000
AFIX 0
C30 1 0.58145 0.31863 0.23441 11.00000 0.04117 0.05021 0.04684 =
0.01324 -0.01695 -0.01738
AFIX 43
H30 2 0.59127 0.33775 0.18765 11.00000 -1.20000
AFIX 0
C31 1 -0.10774 0.55407 0.24076 11.00000 0.03691 0.02633 0.04294 =
0.00075 -0.01071 -0.00387
AFIX 43
H31 2 -0.11345 0.60076 0.20521 11.00000 -1.20000
AFIX 0
C32 1 -0.19430 0.56449 0.29957 11.00000 0.03143 0.03656 0.04188 =
0.00087 -0.01022 -0.00220
C33 1 -0.20262 0.49879 0.35563 11.00000 0.04051 0.03522 0.03449 =
-0.00794 -0.00994 -0.00171
C34 1 -0.29788 0.51977 0.40753 11.00000 0.03478 0.04644 0.04279 =
-0.00934 -0.00455 -0.00292
AFIX 43
H34 2 -0.30928 0.47558 0.44410 11.00000 -1.20000
AFIX 0
C35 1 -0.37309 0.60362 0.40475 11.00000 0.03800 0.04654 0.06961 =
-0.00859 0.00124 -0.00363
AFIX 43
H35 2 -0.43139 0.61966 0.44203 11.00000 -1.20000
AFIX 0
C36 1 -0.36541 0.66405 0.34946 11.00000 0.02986 0.04760 0.06466 =
-0.00276 -0.00796 -0.00022
AFIX 43
H36 2 -0.42171 0.71833 0.34664 11.00000 -1.20000
AFIX 0
C37 1 -0.27772 0.64673 0.29865 11.00000 0.03395 0.03838 0.06026 =
0.00117 -0.01261 -0.00202
AFIX 43
H37 2 -0.27199 0.69083 0.26146 11.00000 -1.20000
AFIX 0
C38 1 0.03903 0.54339 0.11592 11.00000 0.04548 0.04338 0.02789 =
0.01689 -0.00777 -0.00203
AFIX 137
H38A 2 -0.03575 0.54770 0.10819 11.00000 -1.50000
H38B 2 0.09058 0.51623 0.07571 11.00000 -1.50000
H38C 2 0.05045 0.60728 0.12385 11.00000 -1.50000
AFIX 0
C39 1 -0.08771 0.27451 0.21525 11.00000 0.04536 0.03550 0.04617 =
0.01210 -0.01589 -0.01674
AFIX 43
H39 2 -0.10360 0.33357 0.19149 11.00000 -1.20000
AFIX 0
C40 1 -0.11715 0.19792 0.19445 11.00000 0.06203 0.04080 0.08082 =
0.00683 -0.03249 -0.02162
AFIX 43
H40 2 -0.15588 0.20343 0.15743 11.00000 -1.20000
AFIX 0
C41 1 -0.09155 0.11193 0.22644 11.00000 0.08312 0.03724 0.08443 =
0.01167 -0.03336 -0.02661
AFIX 43
H41 2 -0.11184 0.05727 0.21149 11.00000 -1.20000
AFIX 0
C42 1 -0.03519 0.10418 0.28148 11.00000 0.06898 0.03395 0.07773 =
0.00556 -0.02270 -0.00932
AFIX 43
H42 2 -0.01571 0.04395 0.30311 11.00000 -1.20000
AFIX 0
C43 1 -0.00831 0.18331 0.30399 11.00000 0.04108 0.02900 0.04305 =
0.01154 -0.00407 -0.00530
C44 1 0.04451 0.19054 0.36330 11.00000 0.03217 0.03976 0.03686 =
0.01097 0.00349 0.00367
C45 1 0.05960 0.28295 0.37283 11.00000 0.02686 0.03866 0.02599 =
0.01425 0.00218 0.00486
C46 1 0.10105 0.31157 0.42673 11.00000 0.03355 0.04921 0.02538 =
0.01004 -0.00000 0.00251
C47 1 0.13277 0.23866 0.47395 11.00000 0.04362 0.06341 0.03174 =
0.02226 0.00111 0.00117
C48 1 0.12045 0.14876 0.46449 11.00000 0.04351 0.05980 0.03770 =
0.02187 -0.00159 0.00633
AFIX 43
H48 2 0.14270 0.10073 0.49663 11.00000 -1.20000
AFIX 0
C49 1 0.07718 0.12230 0.41058 11.00000 0.04017 0.04573 0.03734 =
0.01821 0.00746 0.00993
C50 1 0.06463 0.01886 0.40867 11.00000 0.08494 0.04810 0.05707 =
0.02491 -0.00636 -0.00129
AFIX 137
H50A 2 -0.01244 0.01682 0.41076 11.00000 -1.50000
H50B 2 0.09097 -0.01655 0.44780 11.00000 -1.50000
H50C 2 0.10729 -0.01018 0.36622 11.00000 -1.50000
AFIX 0
C51 1 0.17712 0.25803 0.53863 11.00000 0.07099 0.09136 0.03845 =
0.02704 -0.02301 -0.00650
AFIX 137
H51A 2 0.24304 0.28472 0.52490 11.00000 -1.50000
H51B 2 0.19467 0.19809 0.56408 11.00000 -1.50000
H51C 2 0.12158 0.30350 0.56766 11.00000 -1.50000
AFIX 0
C52 1 0.10611 0.41192 0.42398 11.00000 0.04354 0.05010 0.03016 =
0.00465 -0.00477 -0.00069
C53 1 0.13548 0.46420 0.47150 11.00000 0.05910 0.06316 0.03170 =
0.00193 -0.01831 -0.00515
AFIX 43
H53 2 0.15840 0.43295 0.51116 11.00000 -1.20000
AFIX 0
C54 1 0.13217 0.55932 0.46251 11.00000 0.05850 0.06534 0.05662 =
-0.00328 -0.01657 -0.00955
AFIX 43
H54 2 0.15292 0.59298 0.49620 11.00000 -1.20000
AFIX 0
C55 1 0.10049 0.60736 0.40751 11.00000 0.05784 0.04186 0.05291 =
-0.00892 -0.01857 -0.00528
AFIX 43
H55 2 0.10000 0.67362 0.40067 11.00000 -1.20000
AFIX 0
C56 1 0.06902 0.55519 0.36202 11.00000 0.04364 0.03401 0.04512 =
-0.00239 -0.01538 -0.00093
AFIX 43
H56 2 0.04351 0.58732 0.32335 11.00000 -1.20000
AFIX 0
P1 7 0.24157 0.54405 -0.07527 11.00000 0.05316 0.06432 0.04647 =
0.02095 -0.02011 -0.02650
F1 3 0.37089 0.51220 -0.09700 11.00000 0.05812 0.08501 0.05342 =
0.01590 -0.01454 -0.01945
F2 3 0.23299 0.44387 -0.04401 11.00000 0.09219 0.07373 0.07249 =
0.02242 -0.02193 -0.04317
F3 3 0.22500 0.51255 -0.14676 11.00000 0.09077 0.09055 0.05816 =
0.00358 -0.03447 -0.02223
F4 3 0.24678 0.64786 -0.10476 11.00000 0.07870 0.07030 0.06163 =
0.02868 -0.02490 -0.02675
F5 3 0.25872 0.57700 -0.00231 11.00000 0.06542 0.06646 0.04739 =
0.01231 -0.01505 -0.02432
F6 3 0.11211 0.57639 -0.05431 11.00000 0.05652 0.11306 0.08548 =
0.02086 -0.01396 -0.02737
P2 7 0.01450 0.79525 0.22915 11.00000 0.07115 0.03779 0.10995 =
0.01446 -0.02424 -0.02391
F7 3 0.07381 0.68725 0.21844 11.00000 0.11073 0.06445 0.10331 =
0.01006 -0.02411 -0.02122
F8 3 -0.07858 0.77847 0.19063 11.00000 0.10634 0.08614 0.12029 =
0.02596 -0.04445 -0.03697
F9 3 -0.04977 0.75942 0.29873 11.00000 0.10660 0.10292 0.11622 =
0.01918 -0.02184 -0.00991
F10 3 0.10432 0.81295 0.26354 11.00000 0.12905 0.10406 0.21333 =
0.00289 -0.08209 -0.04425
F11 3 0.07414 0.82476 0.15942 11.00000 0.13117 0.17178 0.15555 =
0.06836 -0.02399 -0.06598
F12 3 -0.05122 0.89620 0.24405 11.00000 0.14379 0.05704 0.20935 =
-0.00195 -0.06918 -0.00617
SAME 0.02 0.02 N5S C9S C10S
SAME 0.02 0.02 N4S C7S C8S
SAME 0.02 0.02 N3S C5S C6S
SAME 0.005 0.01 N6S C11S C12S
N1S 5 0.74030 0.02858 0.40922 11.00000 0.07623 0.07042 0.07653 =
0.01924 -0.00477 -0.02007
C1S 1 0.71830 -0.01013 0.36722 11.00000 0.05229 0.04717 0.06856 =
0.02088 0.00078 -0.00407
C2S 1 0.68444 -0.05782 0.31577 11.00000 0.06035 0.06957 0.07696 =
0.00949 -0.01028 0.00153
AFIX 137
H2SA 2 0.66346 -0.01175 0.28003 11.00000 -1.50000
H2SB 2 0.62195 -0.08616 0.33637 11.00000 -1.50000
H2SC 2 0.74476 -0.10816 0.29574 11.00000 -1.50000
AFIX 0
N3S 5 -0.37698 0.29367 0.52501 11.00000 0.06326 0.14582 0.08329 =
-0.01363 0.01546 0.01658
C5S 1 -0.29185 0.25823 0.50031 11.00000 0.06198 0.08611 0.05787 =
0.00509 0.01462 0.00565
C6S 1 -0.18503 0.21640 0.46600 11.00000 0.06049 0.05517 0.12961 =
-0.02069 0.03494 -0.01236
AFIX 137
H6SA 2 -0.16667 0.25265 0.42386 11.00000 -1.50000
H6SB 2 -0.18329 0.15018 0.45484 11.00000 -1.50000
H6SC 2 -0.13192 0.21772 0.49577 11.00000 -1.50000
AFIX 0
N4S 5 0.14806 0.22633 0.10742 11.00000 0.09275 0.16201 0.12303 =
-0.01525 -0.02205 -0.01962
C7S 1 0.12160 0.23823 0.05573 11.00000 0.08303 0.07283 0.11462 =
-0.02634 -0.01289 -0.00316
C8S 1 0.09101 0.25609 -0.01017 11.00000 0.23330 0.09431 0.13662 =
-0.01319 -0.07037 -0.01580
AFIX 137
H8SA 2 0.15668 0.25290 -0.04510 11.00000 -1.50000
H8SB 2 0.04464 0.31968 -0.01130 11.00000 -1.50000
H8SC 2 0.05079 0.20793 -0.01924 11.00000 -1.50000
AFIX 0
PART 2
N5S 5 0.32387 0.46087 0.27269 10.70000 0.08068
C9S 1 0.35686 0.50868 0.30377 10.70000 0.09357
C10S 1 0.39351 0.55969 0.35286 10.70000 0.15935
AFIX 137
H10A 2 0.45978 0.58187 0.33119 10.70000 -1.50000
H10B 2 0.40922 0.51714 0.39151 10.70000 -1.50000
H10C 2 0.33640 0.61466 0.36917 10.70000 -1.50000
AFIX 0
PART 0
PART 1
N6S 5 0.34081 0.44141 0.31402 10.30000 0.08043
C11S 1 0.37627 0.44574 0.36182 10.30000 0.18929
C12S 1 0.43563 0.44906 0.41603 10.30000 0.18929
AFIX 137
H12D 2 0.51407 0.43472 0.39802 10.30000 -1.50000
H12E 2 0.41788 0.40181 0.45145 10.30000 -1.50000
H12F 2 0.41554 0.51292 0.43569 10.30000 -1.50000
AFIX 0
HKLF 4
END
;
# start Validation Reply Form
_vrf_PLAT602_Ir2dpyx2L5_16srv305
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! Info
RESPONSE: No meaningful peaks could be seen in these voids. According to the
Platon SQUEEZE, the structure contains about 40 additional independent electrons
per unit cell, however, the application of SQUEEZE didn't result in any improvement
of refinement parameters. Keeping also in mind general weakness of the data, the
SQUEEZE correction deemed to be unnecessary and wasn't applied.
;
# end Validation Reply Form
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_Ir2dpyF2L6_20srv027
_database_code_depnum_ccdc_archive 'CCDC 2006849'
loop_
_audit_author_name
_audit_author_address
'Dmitry Yufit'
;Durham University
United Kingdom
;
_audit_update_record
;
2020-07-07 deposited with the CCDC. 2020-07-10 downloaded from the CCDC.
;
_audit_creation_date 2020-01-27
_audit_creation_method
;
Olex2 1.3-beta
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety
'C60 H52 F4 Ir2 N10 O2, 2(F6 P), C4 H10 O, 3(C2 H3 N)'
_chemical_formula_sum 'C70 H71 F16 Ir2 N13 O3 P2'
_chemical_formula_weight 1892.73
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 12.4261(12)
_cell_length_b 15.8044(15)
_cell_length_c 19.8347(19)
_cell_angle_alpha 76.196(3)
_cell_angle_beta 74.210(3)
_cell_angle_gamma 81.438(3)
_cell_volume 3625.3(6)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 8254
_cell_measurement_temperature 120.0
_cell_measurement_theta_max 23.20
_cell_measurement_theta_min 2.26
_shelx_estimated_absorpt_T_max 0.928
_shelx_estimated_absorpt_T_min 0.273
_exptl_absorpt_coefficient_mu 3.809
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.6482
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1535 before and 0.0909 after correction.
The Ratio of minimum to maximum transmission is 0.6482.
The \l/2 correction factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear light yellow'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier light
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.734
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 1868
_exptl_crystal_size_max 0.46
_exptl_crystal_size_mid 0.04
_exptl_crystal_size_min 0.02
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.1711
_diffrn_reflns_av_unetI/netI 0.1842
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_number 64406
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.000
_diffrn_reflns_theta_min 1.989
_diffrn_ambient_temperature 120.0
_diffrn_detector 'Bruker PHOTON 100 CMOS'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type 'CMOS sensor'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device '3-circle diffractometer'
_diffrn_measurement_device_type 'Bruker D8 Venture'
_diffrn_measurement_method \w-scan
_diffrn_radiation_monochromator 'focusing mirrors'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_current 1.0
_diffrn_source_power 0.05
_diffrn_source_type 'Incoatec I\mS microsource'
_diffrn_source_voltage 50.0
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 8554
_reflns_number_total 15791
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_bruker_data_scaling 'SADABS V2012/1 (Bruker AXS Inc.)'
_computing_cell_refinement 'SAINT v8.38A (Bruker AXS, 2018)'
_computing_data_collection 'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_reduction 'SAINT v8.38A (Bruker AXS, 2018)'
_computing_molecular_graphics 'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max 1.541
_refine_diff_density_min -1.366
_refine_diff_density_rms 0.182
_refine_ls_extinction_coef 0.00097(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref 0.989
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 966
_refine_ls_number_reflns 15791
_refine_ls_number_restraints 198
_refine_ls_R_factor_all 0.1505
_refine_ls_R_factor_gt 0.0640
_refine_ls_restrained_S_all 1.002
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1165
_refine_ls_wR_factor_ref 0.1398
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F22) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
O1S, C3S, C4S, C5S, C6S
with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
P1, F11, F12, F13, F14, F15, F16
with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
P2, F21, F22, F23, F24, F25, F26
with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
N1S, C1S, C2S
with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
N3S, C13S, C14S
with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
N2S, C11S, C12S
with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
C25, C26, C27, C28
with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Riding coordinates:
C2S(H2SA,H2SB,H2SC), C12S(H12D,H12E,H12F), C14S(H14A,H14B,H14C)
4.b Secondary CH2 refined with riding coordinates:
C3S(H3SA,H3SB), C5S(H5SA,H5SB)
4.c Aromatic/amide H refined with riding coordinates:
C1(H1), C4(H4), C5(H5), C7(H7), C14(H14), C16(H16), C18(H18), C21(H21),
C22(H22), C24(H24), C29(H29), C30(H30), C31(H31), C32(H32), C38(H38), C41(H41),
C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
C54(H54), C57(H57), C58(H58), C59(H59), C60(H60)
4.d Idealised Me refined as rotating group:
C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
H12C), C17(H17A,H17B,H17C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
H28B,H28C), C4S(H4SA,H4SB,H4SC), C6S(H6SA,H6SB,H6SC)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.73978(3) 0.58454(2) 0.31858(2) 0.02711(13) Uani 1 1 d . . . . .
Ir2 Ir 0.40364(3) 0.75261(3) 0.15282(2) 0.03017(14) Uani 1 1 d . . . . .
F1 F 0.6915(5) 0.8951(4) 0.3792(3) 0.0508(16) Uani 1 1 d . . . . .
F2 F 0.3892(4) 0.7254(4) 0.4842(3) 0.0472(16) Uani 1 1 d . . . . .
F3 F 0.4170(5) 0.9916(4) 0.2927(3) 0.0579(18) Uani 1 1 d . . . . .
F4 F 0.1984(5) 0.7612(4) 0.4202(3) 0.0567(18) Uani 1 1 d . . . . .
O1 O 0.8084(5) 0.5401(4) 0.4035(3) 0.0323(16) Uani 1 1 d . . . . .
O2 O 0.2668(5) 0.8224(4) 0.1264(3) 0.0358(17) Uani 1 1 d . . . . .
N1 N 0.8273(6) 0.4881(5) 0.2645(4) 0.0300(19) Uani 1 1 d . . . . .
N2 N 0.8050(6) 0.4941(5) 0.1988(4) 0.032(2) Uani 1 1 d . . . . .
N3 N 0.6775(6) 0.6110(5) 0.2307(4) 0.0279(19) Uani 1 1 d . . . . .
N4 N 0.8548(6) 0.6764(5) 0.2809(4) 0.0245(18) Uani 1 1 d . . . . .
N5 N 0.5940(6) 0.5284(6) 0.3742(4) 0.033(2) Uani 1 1 d . . . . .
N6 N 0.5427(6) 0.6767(5) 0.1667(4) 0.0290(19) Uani 1 1 d . . . . .
N7 N 0.5392(7) 0.6363(5) 0.0616(4) 0.038(2) Uani 1 1 d . . . . .
N8 N 0.4472(6) 0.6983(5) 0.0629(4) 0.0295(19) Uani 1 1 d . . . . .
N9 N 0.4899(6) 0.8598(5) 0.1125(4) 0.036(2) Uani 1 1 d . . . . .
N10 N 0.3052(6) 0.6599(5) 0.2236(4) 0.0297(19) Uani 1 1 d . . . . .
C1 C 0.9013(7) 0.4286(6) 0.2868(5) 0.031(2) Uani 1 1 d . . . . .
H1 H 0.940292 0.389854 0.256412 0.037 Uiso 1 1 calc R U . . .
C2 C 0.9279(7) 0.4179(6) 0.3552(5) 0.031(2) Uani 1 1 d . . . . .
C3 C 0.8824(7) 0.4715(6) 0.4054(4) 0.025(2) Uani 1 1 d . . . . .
C4 C 0.9209(7) 0.4463(6) 0.4692(5) 0.032(2) Uani 1 1 d . . . . .
H4 H 0.891563 0.479139 0.505599 0.038 Uiso 1 1 calc R U . . .
C5 C 0.9987(7) 0.3763(6) 0.4806(5) 0.033(2) Uani 1 1 d . . . . .
H5 H 1.021852 0.363364 0.524065 0.040 Uiso 1 1 calc R U . . .
C6 C 1.0450(8) 0.3237(6) 0.4307(5) 0.035(3) Uani 1 1 d . . . . .
C7 C 1.0084(7) 0.3475(6) 0.3689(5) 0.033(2) Uani 1 1 d . . . . .
H7 H 1.039505 0.314277 0.332886 0.040 Uiso 1 1 calc R U . . .
C8 C 1.1273(8) 0.2464(7) 0.4476(5) 0.041(3) Uani 1 1 d . . . . .
C9 C 1.1708(9) 0.1982(7) 0.3844(6) 0.056(3) Uani 1 1 d . . . . .
H9A H 1.107434 0.176893 0.374759 0.084 Uiso 1 1 calc R U . . .
H9B H 1.224296 0.148535 0.396874 0.084 Uiso 1 1 calc R U . . .
H9C H 1.208181 0.238619 0.341530 0.084 Uiso 1 1 calc R U . . .
C10 C 1.0766(9) 0.1794(7) 0.5134(6) 0.055(3) Uani 1 1 d . . . . .
H10A H 1.047219 0.207827 0.554394 0.083 Uiso 1 1 calc R U . . .
H10B H 1.134503 0.132506 0.523913 0.083 Uiso 1 1 calc R U . . .
H10C H 1.015378 0.154754 0.504237 0.083 Uiso 1 1 calc R U . . .
C11 C 1.2313(8) 0.2767(7) 0.4586(6) 0.052(3) Uani 1 1 d . . . . .
H11A H 1.270415 0.313113 0.413838 0.079 Uiso 1 1 calc R U . . .
H11B H 1.281692 0.225547 0.472781 0.079 Uiso 1 1 calc R U . . .
H11C H 1.208628 0.310776 0.496279 0.079 Uiso 1 1 calc R U . . .
C12 C 0.8490(8) 0.4241(6) 0.1596(5) 0.046(3) Uani 1 1 d . . . . .
H12A H 0.925221 0.434520 0.130560 0.070 Uiso 1 1 calc R U . . .
H12B H 0.800598 0.422778 0.128338 0.070 Uiso 1 1 calc R U . . .
H12C H 0.850793 0.367882 0.193627 0.070 Uiso 1 1 calc R U . . .
C13 C 0.7237(7) 0.5566(6) 0.1830(5) 0.029(2) Uani 1 1 d . . . . .
C14 C 0.6860(7) 0.5694(6) 0.1207(4) 0.032(2) Uani 1 1 d . . . . .
H14 H 0.724331 0.540124 0.083161 0.039 Uiso 1 1 calc R U . . .
C15 C 0.5906(8) 0.6264(6) 0.1156(5) 0.033(2) Uani 1 1 d . . . . .
C16 C 0.5928(7) 0.6681(6) 0.2192(4) 0.029(2) Uani 1 1 d . . . . .
H16 H 0.565074 0.706685 0.251362 0.035 Uiso 1 1 calc R U . . .
C17 C 0.5733(10) 0.5867(7) 0.0060(5) 0.061(4) Uani 1 1 d . . . . .
H17A H 0.506621 0.571895 -0.004532 0.092 Uiso 1 1 calc R U . . .
H17B H 0.617937 0.532754 0.022070 0.092 Uiso 1 1 calc R U . . .
H17C H 0.618576 0.621476 -0.037236 0.092 Uiso 1 1 calc R U . . .
C18 C 0.3979(8) 0.7177(6) 0.0104(5) 0.038(3) Uani 1 1 d . . . . .
H18 H 0.424525 0.687979 -0.028124 0.045 Uiso 1 1 calc R U . . .
C19 C 0.3035(8) 0.7835(6) 0.0093(5) 0.035(2) Uani 1 1 d . . . . .
C20 C 0.2464(8) 0.8306(6) 0.0628(5) 0.033(2) Uani 1 1 d . . . . .
C21 C 0.1611(9) 0.8920(7) 0.0487(5) 0.050(3) Uani 1 1 d . . . . .
H21 H 0.120732 0.923853 0.084133 0.061 Uiso 1 1 calc R U . . .
C22 C 0.1311(9) 0.9093(8) -0.0184(6) 0.060(3) Uani 1 1 d . . . . .
H22 H 0.072642 0.953448 -0.026822 0.072 Uiso 1 1 calc R U . . .
C23 C 0.1849(8) 0.8634(6) -0.0714(5) 0.037(3) Uani 1 1 d . . . . .
C24 C 0.2686(8) 0.8011(6) -0.0556(5) 0.043(3) Uani 1 1 d . . . . .
H24 H 0.305898 0.767344 -0.090327 0.051 Uiso 1 1 calc R U . . .
C25 C 0.1538(11) 0.8814(8) -0.1419(6) 0.065(3) Uani 1 1 d . . . . .
C26 C 0.2512(12) 0.9105(10) -0.2011(7) 0.116(5) Uani 1 1 d . . . . .
H26A H 0.279719 0.959965 -0.191585 0.175 Uiso 1 1 calc R U . . .
H26B H 0.227914 0.928708 -0.246193 0.175 Uiso 1 1 calc R U . . .
H26C H 0.310475 0.862223 -0.204661 0.175 Uiso 1 1 calc R U . . .
C27 C 0.1135(13) 0.8050(8) -0.1520(7) 0.097(4) Uani 1 1 d . . . . .
H27A H 0.169502 0.754886 -0.146497 0.145 Uiso 1 1 calc R U . . .
H27B H 0.100715 0.816423 -0.200114 0.145 Uiso 1 1 calc R U . . .
H27C H 0.042891 0.792103 -0.116187 0.145 Uiso 1 1 calc R U . . .
C28 C 0.0679(12) 0.9583(9) -0.1504(7) 0.097(4) Uani 1 1 d . . . . .
H28A H -0.001040 0.947011 -0.112492 0.146 Uiso 1 1 calc R U . . .
H28B H 0.051278 0.967164 -0.197239 0.146 Uiso 1 1 calc R U . . .
H28C H 0.097299 1.010842 -0.146834 0.146 Uiso 1 1 calc R U . . .
C29 C 0.9565(8) 0.6676(6) 0.2360(5) 0.036(3) Uani 1 1 d . . . . .
H29 H 0.978579 0.615697 0.217675 0.043 Uiso 1 1 calc R U . . .
C30 C 1.0299(8) 0.7318(7) 0.2157(5) 0.035(2) Uani 1 1 d . . . . .
H30 H 1.100467 0.725372 0.182606 0.042 Uiso 1 1 calc R U . . .
C31 C 0.9984(9) 0.8056(7) 0.2448(6) 0.048(3) Uani 1 1 d . . . . .
H31 H 1.049932 0.848479 0.234039 0.058 Uiso 1 1 calc R U . . .
C32 C 0.8937(8) 0.8178(7) 0.2889(5) 0.038(3) Uani 1 1 d . . . . .
H32 H 0.870231 0.870214 0.306434 0.046 Uiso 1 1 calc R U . . .
C33 C 0.8241(8) 0.7522(6) 0.3069(5) 0.035(3) Uani 1 1 d . . . . .
C34 C 0.7094(7) 0.7543(6) 0.3530(5) 0.026(2) Uani 1 1 d . . . . .
C35 C 0.6580(7) 0.6791(6) 0.3644(4) 0.028(2) Uani 1 1 d . . . . .
C36 C 0.5499(8) 0.6650(6) 0.4080(5) 0.031(2) Uani 1 1 d . . . . .
C37 C 0.4927(8) 0.7341(7) 0.4411(5) 0.036(3) Uani 1 1 d . . . . .
C38 C 0.5419(9) 0.8100(7) 0.4306(5) 0.046(3) Uani 1 1 d . . . . .
H38 H 0.502842 0.856240 0.453192 0.055 Uiso 1 1 calc R U . . .
C39 C 0.6467(9) 0.8183(7) 0.3876(5) 0.037(3) Uani 1 1 d . . . . .
C40 C 0.5127(8) 0.5807(7) 0.4104(5) 0.037(3) Uani 1 1 d . . . . .
C41 C 0.4104(8) 0.5503(7) 0.4459(5) 0.034(2) Uani 1 1 d . . . . .
H41 H 0.354529 0.586382 0.472029 0.041 Uiso 1 1 calc R U . . .
C42 C 0.3870(8) 0.4686(7) 0.4444(5) 0.040(3) Uani 1 1 d . . . . .
H42 H 0.315816 0.448100 0.469448 0.048 Uiso 1 1 calc R U . . .
C43 C 0.4698(8) 0.4154(7) 0.4051(5) 0.039(3) Uani 1 1 d . . . . .
H43 H 0.455868 0.359009 0.402268 0.047 Uiso 1 1 calc R U . . .
C44 C 0.5699(8) 0.4480(7) 0.3716(5) 0.034(3) Uani 1 1 d . . . . .
H44 H 0.626461 0.413021 0.344860 0.041 Uiso 1 1 calc R U . . .
C45 C 0.5591(8) 0.8826(6) 0.0466(5) 0.039(3) Uani 1 1 d . . . . .
H45 H 0.566729 0.845890 0.013697 0.047 Uiso 1 1 calc R U . . .
C46 C 0.6183(9) 0.9540(7) 0.0241(5) 0.043(3) Uani 1 1 d . . . . .
H46 H 0.667066 0.965850 -0.022508 0.052 Uiso 1 1 calc R U . . .
C47 C 0.6055(9) 1.0092(7) 0.0713(6) 0.048(3) Uani 1 1 d . . . . .
H47 H 0.643308 1.060984 0.057030 0.058 Uiso 1 1 calc R U . . .
C48 C 0.5378(9) 0.9876(7) 0.1384(6) 0.048(3) Uani 1 1 d . . . . .
H48 H 0.530829 1.024092 0.171402 0.058 Uiso 1 1 calc R U . . .
C49 C 0.4783(8) 0.9134(7) 0.1601(5) 0.035(3) Uani 1 1 d . . . . .
C50 C 0.4092(8) 0.8803(7) 0.2319(5) 0.036(3) Uani 1 1 d . . . . .
C51 C 0.3658(8) 0.8023(6) 0.2384(5) 0.034(2) Uani 1 1 d . . . . .
C52 C 0.2940(7) 0.7591(6) 0.3002(5) 0.029(2) Uani 1 1 d . . . . .
C53 C 0.2686(8) 0.7985(7) 0.3565(5) 0.041(3) Uani 1 1 d . . . . .
C54 C 0.3087(8) 0.8754(7) 0.3552(6) 0.043(3) Uani 1 1 d . . . . .
H54 H 0.287946 0.900423 0.396520 0.052 Uiso 1 1 calc R U . . .
C55 C 0.3790(8) 0.9155(7) 0.2935(6) 0.041(3) Uani 1 1 d . . . . .
C56 C 0.2623(7) 0.6788(6) 0.2912(5) 0.032(2) Uani 1 1 d . . . . .
C57 C 0.1949(8) 0.6193(7) 0.3437(5) 0.039(3) Uani 1 1 d . . . . .
H57 H 0.163417 0.631418 0.390074 0.047 Uiso 1 1 calc R U . . .
C58 C 0.1740(8) 0.5444(7) 0.3290(5) 0.048(3) Uani 1 1 d . . . . .
H58 H 0.127912 0.504842 0.365208 0.057 Uiso 1 1 calc R U . . .
C59 C 0.2183(8) 0.5252(7) 0.2627(5) 0.042(3) Uani 1 1 d . . . . .
H59 H 0.204797 0.472887 0.251974 0.050 Uiso 1 1 calc R U . . .
C60 C 0.2835(8) 0.5852(7) 0.2122(5) 0.035(2) Uani 1 1 d . . . . .
H60 H 0.315162 0.572542 0.166000 0.041 Uiso 1 1 calc R U . . .
P1 P 0.5034(3) 0.3575(2) 0.20954(16) 0.0575(8) Uani 1 1 d . . . . .
F11 F 0.5015(7) 0.2650(5) 0.1919(4) 0.091(2) Uani 1 1 d . . . . .
F12 F 0.5930(7) 0.3169(5) 0.2532(4) 0.110(2) Uani 1 1 d . . . . .
F13 F 0.4065(6) 0.3350(5) 0.2796(4) 0.094(2) Uani 1 1 d . . . . .
F14 F 0.4141(7) 0.3970(5) 0.1656(4) 0.101(2) Uani 1 1 d . . . . .
F15 F 0.5986(7) 0.3779(5) 0.1392(4) 0.099(2) Uani 1 1 d . . . . .
F16 F 0.5027(6) 0.4502(4) 0.2280(3) 0.0731(17) Uani 1 1 d . . . . .
P2 P 1.1327(3) 0.5505(3) 0.06595(17) 0.0657(9) Uani 1 1 d . . . . .
F21 F 1.1407(6) 0.4593(5) 0.0422(4) 0.092(2) Uani 1 1 d . . . . .
F22 F 1.2557(6) 0.5249(6) 0.0799(4) 0.105(2) Uani 1 1 d . U . . .
F23 F 1.0838(6) 0.5033(4) 0.1483(3) 0.0776(18) Uani 1 1 d . . . . .
F24 F 1.0093(6) 0.5724(5) 0.0584(4) 0.097(2) Uani 1 1 d . . . . .
F25 F 1.1858(8) 0.5916(6) -0.0122(4) 0.117(2) Uani 1 1 d . . . . .
F26 F 1.1283(6) 0.6398(5) 0.0912(3) 0.0752(17) Uani 1 1 d . . . . .
O1S O -0.0336(8) 1.1027(6) 0.3301(5) 0.094(3) Uani 1 1 d . . . . .
C3S C 0.0384(11) 1.0180(9) 0.3276(8) 0.094(4) Uani 1 1 d . . . . .
H3SA H -0.004154 0.972160 0.323284 0.113 Uiso 1 1 calc R U . . .
H3SB H 0.067543 0.997577 0.371033 0.113 Uiso 1 1 calc R U . . .
C4S C 0.1382(12) 1.0418(11) 0.2576(8) 0.122(6) Uani 1 1 d . . . . .
H4SA H 0.106907 1.075292 0.217786 0.183 Uiso 1 1 calc R U . . .
H4SB H 0.179977 0.987838 0.244883 0.183 Uiso 1 1 calc R U . . .
H4SC H 0.188888 1.076945 0.267170 0.183 Uiso 1 1 calc R U . . .
C5S C -0.1267(13) 1.0933(10) 0.3838(8) 0.097(4) Uani 1 1 d . . . . .
H5SA H -0.104946 1.066705 0.429260 0.116 Uiso 1 1 calc R U . . .
H5SB H -0.172781 1.052660 0.375405 0.116 Uiso 1 1 calc R U . . .
C6S C -0.1954(11) 1.1776(9) 0.3910(8) 0.101(5) Uani 1 1 d . . . . .
H6SA H -0.209473 1.207670 0.344519 0.152 Uiso 1 1 calc R U . . .
H6SB H -0.154872 1.214508 0.407172 0.152 Uiso 1 1 calc R U . . .
H6SC H -0.267080 1.166285 0.426071 0.152 Uiso 1 1 calc R U . . .
N1S N 0.3677(9) 1.0039(7) 0.4728(6) 0.073(3) Uani 1 1 d . . . . .
C1S C 0.4276(11) 1.0496(9) 0.4313(7) 0.058(3) Uani 1 1 d . . . . .
C2S C 0.5080(11) 1.1096(8) 0.3793(6) 0.080(4) Uani 1 1 d . . . . .
H2SA H 0.485479 1.169485 0.386623 0.119 Uiso 1 1 d R U . . .
H2SB H 0.507919 1.107265 0.330383 0.119 Uiso 1 1 d R U . . .
H2SC H 0.583659 1.091436 0.386623 0.119 Uiso 1 1 d R U . . .
N2S N 0.7221(16) 0.7901(13) -0.0768(10) 0.197(9) Uani 1 1 d . . . . .
C11S C 0.7550(17) 0.7593(12) -0.1217(10) 0.126(7) Uani 1 1 d . . . . .
C12S C 0.8076(13) 0.7132(10) -0.1788(8) 0.120(6) Uani 1 1 d . . . . .
H12D H 0.811179 0.753270 -0.225297 0.180 Uiso 1 1 d R U . . .
H12E H 0.763689 0.664801 -0.174847 0.180 Uiso 1 1 d R U . . .
H12F H 0.883769 0.689960 -0.174847 0.180 Uiso 1 1 d R U . . .
N3S N 0.7441(10) 0.8125(8) 0.1604(7) 0.093(4) Uani 1 1 d . . . . .
C13S C 0.8096(12) 0.7977(9) 0.1093(8) 0.080(4) Uani 1 1 d . . . . .
C14S C 0.8858(12) 0.7759(10) 0.0478(8) 0.111(6) Uani 1 1 d . . . . .
H14A H 0.865735 0.812659 0.004884 0.166 Uiso 1 1 d R U . . .
H14B H 0.961816 0.785649 0.047824 0.166 Uiso 1 1 d R U . . .
H14C H 0.883096 0.714199 0.047824 0.166 Uiso 1 1 d R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ir1 0.0203(2) 0.0389(3) 0.0204(2) -0.00652(18) -0.00489(16) 0.00324(19)
Ir2 0.0220(2) 0.0412(3) 0.0230(2) -0.00138(18) -0.00566(17) 0.0021(2)
F1 0.053(4) 0.045(4) 0.057(4) -0.020(3) -0.016(3) 0.005(3)
F2 0.034(3) 0.055(4) 0.043(4) -0.015(3) -0.002(3) 0.020(3)
F3 0.081(5) 0.054(4) 0.046(4) -0.022(3) -0.016(3) -0.014(4)
F4 0.045(4) 0.090(5) 0.030(3) -0.014(3) 0.002(3) -0.010(4)
O1 0.029(4) 0.038(4) 0.030(4) -0.012(3) -0.013(3) 0.015(3)
O2 0.032(4) 0.049(4) 0.021(4) 0.003(3) -0.010(3) 0.002(3)
N1 0.030(5) 0.036(5) 0.028(4) -0.012(4) -0.015(4) 0.007(4)
N2 0.025(4) 0.046(5) 0.024(4) -0.014(4) -0.007(4) 0.010(4)
N3 0.018(4) 0.039(5) 0.022(4) -0.006(4) -0.005(3) 0.010(4)
N4 0.022(4) 0.028(5) 0.032(4) -0.017(4) -0.014(3) 0.005(4)
N5 0.016(4) 0.052(6) 0.033(5) -0.013(4) -0.007(4) 0.004(4)
N6 0.026(4) 0.040(5) 0.022(4) -0.010(4) -0.005(4) 0.004(4)
N7 0.044(5) 0.042(5) 0.030(5) -0.009(4) -0.020(4) 0.013(4)
N8 0.029(5) 0.033(5) 0.033(5) -0.007(4) -0.020(4) 0.000(4)
N9 0.036(5) 0.049(6) 0.023(4) -0.010(4) -0.012(4) 0.009(4)
N10 0.022(4) 0.037(5) 0.028(5) 0.002(4) -0.013(4) 0.002(4)
C1 0.020(5) 0.037(6) 0.038(6) -0.011(5) -0.011(4) 0.004(5)
C2 0.020(5) 0.044(6) 0.025(5) 0.001(5) -0.006(4) 0.001(5)
C3 0.020(5) 0.032(6) 0.026(5) -0.013(4) -0.002(4) -0.007(4)
C4 0.020(5) 0.047(7) 0.031(6) -0.009(5) -0.014(4) 0.002(5)
C5 0.026(5) 0.046(7) 0.027(5) 0.002(5) -0.015(4) -0.001(5)
C6 0.027(6) 0.045(7) 0.028(6) 0.007(5) -0.010(5) -0.005(5)
C7 0.025(5) 0.033(6) 0.034(6) -0.002(5) -0.001(4) 0.001(5)
C8 0.027(6) 0.049(7) 0.040(6) -0.006(5) -0.007(5) 0.010(5)
C9 0.045(7) 0.061(8) 0.077(8) -0.029(7) -0.042(7) 0.025(6)
C10 0.046(7) 0.046(7) 0.066(8) 0.008(6) -0.016(6) -0.007(6)
C11 0.031(6) 0.074(9) 0.056(7) -0.021(6) -0.020(6) 0.016(6)
C12 0.051(7) 0.054(7) 0.044(7) -0.027(6) -0.026(6) 0.019(6)
C13 0.018(5) 0.041(6) 0.024(5) -0.003(4) -0.006(4) 0.004(5)
C14 0.029(5) 0.047(7) 0.019(5) -0.005(4) -0.008(4) 0.003(5)
C15 0.029(6) 0.040(6) 0.027(6) -0.003(5) -0.002(4) -0.009(5)
C16 0.018(5) 0.037(6) 0.027(6) -0.007(5) 0.000(4) 0.003(5)
C17 0.072(9) 0.073(9) 0.049(7) -0.033(7) -0.032(7) 0.024(7)
C18 0.038(6) 0.044(7) 0.035(6) -0.010(5) -0.015(5) 0.001(5)
C19 0.033(6) 0.045(7) 0.027(6) -0.002(5) -0.014(5) -0.002(5)
C20 0.027(6) 0.042(7) 0.027(6) 0.004(5) -0.006(5) -0.008(5)
C21 0.040(7) 0.076(9) 0.028(6) -0.014(6) -0.003(5) 0.012(6)
C22 0.043(7) 0.071(9) 0.058(8) -0.006(7) -0.011(6) 0.010(7)
C23 0.042(6) 0.032(6) 0.038(6) -0.002(5) -0.022(5) 0.003(5)
C24 0.045(7) 0.040(7) 0.048(7) -0.007(5) -0.029(6) 0.014(5)
C25 0.089(7) 0.071(7) 0.046(6) -0.013(5) -0.046(5) 0.014(5)
C26 0.100(8) 0.168(12) 0.070(8) 0.019(8) -0.043(6) -0.004(7)
C27 0.150(11) 0.081(7) 0.091(10) -0.021(7) -0.088(9) 0.006(7)
C28 0.127(9) 0.090(7) 0.097(10) -0.032(7) -0.078(7) 0.039(7)
C29 0.028(6) 0.039(6) 0.039(6) -0.011(5) -0.013(5) 0.015(5)
C30 0.027(6) 0.045(7) 0.031(6) -0.001(5) -0.005(4) -0.006(5)
C31 0.040(7) 0.051(8) 0.057(7) 0.002(6) -0.021(6) -0.016(6)
C32 0.035(6) 0.043(7) 0.039(6) -0.002(5) -0.015(5) -0.011(5)
C33 0.040(6) 0.038(7) 0.024(5) 0.003(5) -0.016(5) 0.006(5)
C34 0.016(5) 0.034(6) 0.031(5) -0.009(5) -0.015(4) 0.011(5)
C35 0.022(5) 0.041(6) 0.018(5) 0.000(4) -0.006(4) -0.006(5)
C36 0.026(5) 0.039(6) 0.029(5) -0.005(5) -0.010(4) 0.003(5)
C37 0.022(5) 0.061(8) 0.016(5) -0.009(5) 0.002(4) 0.011(5)
C38 0.059(8) 0.035(7) 0.034(6) -0.010(5) -0.002(6) 0.012(6)
C39 0.038(6) 0.042(7) 0.033(6) -0.005(5) -0.015(5) 0.000(6)
C40 0.023(5) 0.056(7) 0.029(6) -0.010(5) -0.007(4) 0.008(5)
C41 0.025(6) 0.053(7) 0.023(5) -0.011(5) -0.006(4) 0.002(5)
C42 0.023(5) 0.071(8) 0.023(5) -0.002(5) -0.007(4) -0.001(6)
C43 0.035(6) 0.046(7) 0.035(6) 0.003(5) -0.013(5) -0.009(5)
C44 0.023(5) 0.047(7) 0.026(5) -0.004(5) -0.006(4) 0.008(5)
C45 0.038(6) 0.039(7) 0.030(6) 0.001(5) 0.002(5) -0.007(5)
C46 0.050(7) 0.044(7) 0.028(6) 0.005(5) -0.007(5) -0.006(6)
C47 0.065(8) 0.037(7) 0.040(7) 0.015(5) -0.021(6) -0.015(6)
C48 0.066(8) 0.037(7) 0.044(7) -0.003(5) -0.025(6) 0.001(6)
C49 0.027(6) 0.042(7) 0.036(6) -0.008(5) -0.017(5) 0.017(5)
C50 0.023(5) 0.048(7) 0.036(6) -0.012(5) -0.006(5) 0.009(5)
C51 0.025(5) 0.038(6) 0.040(6) -0.009(5) -0.013(5) 0.006(5)
C52 0.027(5) 0.031(6) 0.028(5) -0.011(5) -0.004(4) 0.007(5)
C53 0.038(6) 0.050(7) 0.028(6) -0.002(5) -0.013(5) 0.016(6)
C54 0.039(7) 0.050(8) 0.043(7) -0.012(6) -0.016(5) 0.002(6)
C55 0.031(6) 0.045(7) 0.044(7) -0.006(6) -0.012(5) 0.006(5)
C56 0.019(5) 0.046(7) 0.025(5) 0.004(5) -0.006(4) -0.002(5)
C57 0.031(6) 0.040(7) 0.036(6) 0.003(5) -0.001(5) -0.002(5)
C58 0.031(6) 0.058(8) 0.037(7) 0.025(6) -0.005(5) -0.012(6)
C59 0.040(6) 0.052(7) 0.033(6) 0.005(5) -0.014(5) -0.011(6)
C60 0.037(6) 0.041(7) 0.028(6) -0.004(5) -0.016(5) 0.000(5)
P1 0.060(2) 0.072(2) 0.0414(17) -0.0098(15) -0.0135(13) -0.0104(17)
F11 0.108(6) 0.087(3) 0.080(5) -0.035(3) -0.007(4) -0.019(3)
F12 0.110(4) 0.123(5) 0.112(4) -0.026(4) -0.068(4) 0.016(4)
F13 0.104(4) 0.108(5) 0.061(3) -0.026(3) 0.014(3) -0.037(4)
F14 0.111(4) 0.129(5) 0.084(4) -0.039(4) -0.059(3) 0.015(4)
F15 0.108(4) 0.102(5) 0.071(3) -0.032(3) 0.022(3) -0.025(4)
F16 0.080(5) 0.084(3) 0.058(4) -0.023(3) -0.008(3) -0.017(3)
P2 0.0548(18) 0.104(3) 0.0478(16) -0.0343(17) -0.0073(15) -0.0155(18)
F21 0.081(5) 0.129(4) 0.082(4) -0.066(4) -0.005(4) -0.022(3)
F22 0.058(3) 0.161(6) 0.123(5) -0.091(4) -0.024(3) 0.006(3)
F23 0.087(4) 0.088(4) 0.054(2) -0.024(2) -0.010(3) 0.007(4)
F24 0.078(3) 0.118(5) 0.111(5) -0.019(4) -0.052(3) -0.012(3)
F25 0.152(5) 0.161(6) 0.047(2) -0.044(3) 0.008(3) -0.064(5)
F26 0.078(4) 0.101(3) 0.052(4) -0.033(3) -0.003(3) -0.018(3)
O1S 0.097(7) 0.092(6) 0.098(7) -0.031(6) -0.031(5) 0.005(5)
C3S 0.080(8) 0.088(7) 0.137(11) -0.047(8) -0.047(6) -0.002(6)
C4S 0.096(10) 0.152(14) 0.118(11) -0.035(9) -0.045(7) 0.037(9)
C5S 0.105(8) 0.114(9) 0.096(9) -0.065(8) -0.025(6) -0.016(6)
C6S 0.086(9) 0.107(9) 0.126(12) -0.069(9) -0.003(8) -0.031(7)
N1S 0.066(7) 0.083(8) 0.073(8) -0.025(6) -0.022(5) 0.011(5)
C1S 0.060(7) 0.070(8) 0.054(7) -0.037(5) -0.022(5) 0.016(5)
C2S 0.080(9) 0.100(9) 0.063(8) -0.030(6) -0.016(6) -0.002(7)
N2S 0.182(18) 0.25(2) 0.166(13) -0.139(13) 0.021(13) 0.000(15)
C11S 0.151(17) 0.108(13) 0.099(11) -0.043(9) 0.018(11) -0.007(12)
C12S 0.138(15) 0.114(13) 0.091(10) -0.040(9) 0.007(10) 0.002(11)
N3S 0.059(8) 0.130(10) 0.089(8) 0.004(8) -0.039(5) -0.010(7)
C13S 0.060(9) 0.084(10) 0.086(9) 0.022(8) -0.034(5) -0.013(8)
C14S 0.075(10) 0.125(13) 0.110(10) 0.007(9) -0.010(7) -0.016(9)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 O1 2.024(6) . ?
Ir1 N1 2.076(7) . ?
Ir1 N3 2.025(7) . ?
Ir1 N4 2.057(7) . ?
Ir1 N5 2.051(8) . ?
Ir1 C35 1.945(9) . ?
Ir2 O2 2.008(6) . ?
Ir2 N6 1.997(7) . ?
Ir2 N8 2.068(7) . ?
Ir2 N9 2.021(8) . ?
Ir2 N10 2.057(7) . ?
Ir2 C51 1.951(9) . ?
F1 C39 1.366(11) . ?
F2 C37 1.343(10) . ?
F3 C55 1.351(11) . ?
F4 C53 1.380(10) . ?
O1 C3 1.314(9) . ?
O2 C20 1.326(10) . ?
N1 N2 1.383(9) . ?
N1 C1 1.300(10) . ?
N2 C12 1.458(11) . ?
N2 C13 1.350(10) . ?
N3 C13 1.382(11) . ?
N3 C16 1.313(10) . ?
N4 C29 1.343(10) . ?
N4 C33 1.377(11) . ?
N5 C40 1.364(11) . ?
N5 C44 1.363(12) . ?
N6 C15 1.390(11) . ?
N6 C16 1.322(10) . ?
N7 N8 1.388(10) . ?
N7 C15 1.356(11) . ?
N7 C17 1.439(11) . ?
N8 C18 1.300(11) . ?
N9 C45 1.354(11) . ?
N9 C49 1.380(11) . ?
N10 C56 1.387(11) . ?
N10 C60 1.332(11) . ?
C1 H1 0.9500 . ?
C1 C2 1.446(12) . ?
C2 C3 1.409(12) . ?
C2 C7 1.409(12) . ?
C3 C4 1.422(11) . ?
C4 H4 0.9500 . ?
C4 C5 1.374(12) . ?
C5 H5 0.9500 . ?
C5 C6 1.393(12) . ?
C6 C7 1.373(12) . ?
C6 C8 1.505(12) . ?
C7 H7 0.9500 . ?
C8 C9 1.553(13) . ?
C8 C10 1.521(13) . ?
C8 C11 1.529(13) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.398(11) . ?
C14 H14 0.9500 . ?
C14 C15 1.389(12) . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18 0.9500 . ?
C18 C19 1.449(12) . ?
C19 C20 1.413(12) . ?
C19 C24 1.419(12) . ?
C20 C21 1.367(12) . ?
C21 H21 0.9500 . ?
C21 C22 1.432(14) . ?
C22 H22 0.9500 . ?
C22 C23 1.382(13) . ?
C23 C24 1.370(12) . ?
C23 C25 1.503(13) . ?
C24 H24 0.9500 . ?
C25 C26 1.479(17) . ?
C25 C27 1.448(16) . ?
C25 C28 1.503(15) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29 0.9500 . ?
C29 C30 1.379(13) . ?
C30 H30 0.9500 . ?
C30 C31 1.380(13) . ?
C31 H31 0.9500 . ?
C31 C32 1.372(13) . ?
C32 H32 0.9500 . ?
C32 C33 1.368(13) . ?
C33 C34 1.470(12) . ?
C34 C35 1.375(12) . ?
C34 C39 1.380(12) . ?
C35 C36 1.403(12) . ?
C36 C37 1.408(12) . ?
C36 C40 1.460(13) . ?
C37 C38 1.374(14) . ?
C38 H38 0.9500 . ?
C38 C39 1.353(13) . ?
C40 C41 1.370(12) . ?
C41 H41 0.9500 . ?
C41 C42 1.375(13) . ?
C42 H42 0.9500 . ?
C42 C43 1.411(13) . ?
C43 H43 0.9500 . ?
C43 C44 1.354(12) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C45 C46 1.358(13) . ?
C46 H46 0.9500 . ?
C46 C47 1.389(13) . ?
C47 H47 0.9500 . ?
C47 C48 1.362(13) . ?
C48 H48 0.9500 . ?
C48 C49 1.397(13) . ?
C49 C50 1.467(13) . ?
C50 C51 1.384(13) . ?
C50 C55 1.397(13) . ?
C51 C52 1.397(12) . ?
C52 C53 1.347(12) . ?
C52 C56 1.446(13) . ?
C53 C54 1.373(14) . ?
C54 H54 0.9500 . ?
C54 C55 1.370(13) . ?
C56 C57 1.400(12) . ?
C57 H57 0.9500 . ?
C57 C58 1.362(14) . ?
C58 H58 0.9500 . ?
C58 C59 1.367(13) . ?
C59 H59 0.9500 . ?
C59 C60 1.375(12) . ?
C60 H60 0.9500 . ?
P1 F11 1.586(7) . ?
P1 F12 1.565(8) . ?
P1 F13 1.577(7) . ?
P1 F14 1.561(7) . ?
P1 F15 1.566(7) . ?
P1 F16 1.592(7) . ?
P2 F21 1.603(8) . ?
P2 F22 1.602(8) . ?
P2 F23 1.616(7) . ?
P2 F24 1.561(8) . ?
P2 F25 1.533(8) . ?
P2 F26 1.595(7) . ?
O1S C3S 1.498(14) . ?
O1S C5S 1.342(15) . ?
C3S H3SA 0.9900 . ?
C3S H3SB 0.9900 . ?
C3S C4S 1.601(17) . ?
C4S H4SA 0.9800 . ?
C4S H4SB 0.9800 . ?
C4S H4SC 0.9800 . ?
C5S H5SA 0.9900 . ?
C5S H5SB 0.9900 . ?
C5S C6S 1.488(16) . ?
C6S H6SA 0.9800 . ?
C6S H6SB 0.9800 . ?
C6S H6SC 0.9800 . ?
N1S C1S 1.138(14) . ?
C1S C2S 1.489(16) . ?
C2S H2SA 0.9802 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?
N2S C11S 1.070(18) . ?
C11S C12S 1.447(19) . ?
C12S H12D 0.9800 . ?
C12S H12E 0.9800 . ?
C12S H12F 0.9800 . ?
N3S C13S 1.162(16) . ?
C13S C14S 1.407(18) . ?
C14S H14A 0.9801 . ?
C14S H14B 0.9799 . ?
C14S H14C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ir1 N1 94.1(3) . . ?
O1 Ir1 N3 171.6(3) . . ?
O1 Ir1 N4 87.7(3) . . ?
O1 Ir1 N5 91.4(3) . . ?
N3 Ir1 N1 78.1(3) . . ?
N3 Ir1 N4 96.5(3) . . ?
N3 Ir1 N5 87.2(3) . . ?
N4 Ir1 N1 99.2(3) . . ?
N5 Ir1 N1 101.5(3) . . ?
N5 Ir1 N4 159.2(3) . . ?
C35 Ir1 O1 88.5(3) . . ?
C35 Ir1 N1 177.0(3) . . ?
C35 Ir1 N3 99.4(3) . . ?
C35 Ir1 N4 79.3(3) . . ?
C35 Ir1 N5 79.9(4) . . ?
O2 Ir2 N8 93.3(3) . . ?
O2 Ir2 N9 89.9(3) . . ?
O2 Ir2 N10 90.3(3) . . ?
N6 Ir2 O2 172.0(3) . . ?
N6 Ir2 N8 78.7(3) . . ?
N6 Ir2 N9 91.6(3) . . ?
N6 Ir2 N10 90.8(3) . . ?
N9 Ir2 N8 98.9(3) . . ?
N9 Ir2 N10 161.2(3) . . ?
N10 Ir2 N8 99.9(3) . . ?
C51 Ir2 O2 88.1(3) . . ?
C51 Ir2 N6 99.9(3) . . ?
C51 Ir2 N8 178.6(3) . . ?
C51 Ir2 N9 81.1(4) . . ?
C51 Ir2 N10 80.0(4) . . ?
C3 O1 Ir1 120.8(5) . . ?
C20 O2 Ir2 122.5(6) . . ?
N2 N1 Ir1 114.1(5) . . ?
C1 N1 Ir1 124.8(6) . . ?
C1 N1 N2 121.0(8) . . ?
N1 N2 C12 119.8(7) . . ?
C13 N2 N1 115.2(7) . . ?
C13 N2 C12 123.5(8) . . ?
C13 N3 Ir1 114.7(5) . . ?
C16 N3 Ir1 126.2(6) . . ?
C16 N3 C13 118.7(8) . . ?
C29 N4 Ir1 126.1(6) . . ?
C29 N4 C33 118.3(8) . . ?
C33 N4 Ir1 115.6(6) . . ?
C40 N5 Ir1 115.6(7) . . ?
C44 N5 Ir1 125.0(6) . . ?
C44 N5 C40 119.1(8) . . ?
C15 N6 Ir2 115.5(6) . . ?
C16 N6 Ir2 127.6(6) . . ?
C16 N6 C15 116.9(8) . . ?
N8 N7 C17 120.1(7) . . ?
C15 N7 N8 115.7(8) . . ?
C15 N7 C17 124.2(8) . . ?
N7 N8 Ir2 113.5(5) . . ?
C18 N8 Ir2 126.3(7) . . ?
C18 N8 N7 120.3(8) . . ?
C45 N9 Ir2 128.1(7) . . ?
C45 N9 C49 117.5(9) . . ?
C49 N9 Ir2 114.4(6) . . ?
C56 N10 Ir2 113.6(6) . . ?
C60 N10 Ir2 127.6(6) . . ?
C60 N10 C56 118.8(8) . . ?
N1 C1 H1 118.0 . . ?
N1 C1 C2 123.9(9) . . ?
C2 C1 H1 118.0 . . ?
C3 C2 C1 125.8(8) . . ?
C3 C2 C7 120.2(8) . . ?
C7 C2 C1 114.0(9) . . ?
O1 C3 C2 130.4(8) . . ?
O1 C3 C4 114.6(8) . . ?
C2 C3 C4 114.9(8) . . ?
C3 C4 H4 118.6 . . ?
C5 C4 C3 122.8(9) . . ?
C5 C4 H4 118.6 . . ?
C4 C5 H5 118.7 . . ?
C4 C5 C6 122.6(9) . . ?
C6 C5 H5 118.7 . . ?
C5 C6 C8 119.8(8) . . ?
C7 C6 C5 115.1(9) . . ?
C7 C6 C8 125.1(9) . . ?
C2 C7 H7 117.8 . . ?
C6 C7 C2 124.4(9) . . ?
C6 C7 H7 117.8 . . ?
C6 C8 C9 111.5(8) . . ?
C6 C8 C10 112.6(8) . . ?
C6 C8 C11 110.4(9) . . ?
C10 C8 C9 107.2(9) . . ?
C10 C8 C11 109.3(9) . . ?
C11 C8 C9 105.6(8) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
N2 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 N3 117.7(8) . . ?
N2 C13 C14 123.2(8) . . ?
N3 C13 C14 119.1(8) . . ?
C13 C14 H14 121.1 . . ?
C15 C14 C13 117.8(8) . . ?
C15 C14 H14 121.1 . . ?
N7 C15 N6 116.4(8) . . ?
N7 C15 C14 123.0(9) . . ?
C14 C15 N6 120.6(9) . . ?
N3 C16 N6 125.9(8) . . ?
N3 C16 H16 117.1 . . ?
N6 C16 H16 117.1 . . ?
N7 C17 H17A 109.5 . . ?
N7 C17 H17B 109.5 . . ?
N7 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N8 C18 H18 119.2 . . ?
N8 C18 C19 121.7(9) . . ?
C19 C18 H18 119.2 . . ?
C20 C19 C18 128.2(9) . . ?
C20 C19 C24 118.7(9) . . ?
C24 C19 C18 113.0(9) . . ?
O2 C20 C19 126.9(9) . . ?
O2 C20 C21 115.3(9) . . ?
C21 C20 C19 117.8(9) . . ?
C20 C21 H21 119.2 . . ?
C20 C21 C22 121.5(10) . . ?
C22 C21 H21 119.2 . . ?
C21 C22 H22 119.1 . . ?
C23 C22 C21 121.8(10) . . ?
C23 C22 H22 119.1 . . ?
C22 C23 C25 122.0(10) . . ?
C24 C23 C22 115.7(9) . . ?
C24 C23 C25 122.2(10) . . ?
C19 C24 H24 117.8 . . ?
C23 C24 C19 124.4(10) . . ?
C23 C24 H24 117.8 . . ?
C23 C25 C28 113.0(10) . . ?
C26 C25 C23 110.0(11) . . ?
C26 C25 C28 102.0(11) . . ?
C27 C25 C23 111.0(10) . . ?
C27 C25 C26 111.0(12) . . ?
C27 C25 C28 109.5(12) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N4 C29 H29 119.0 . . ?
N4 C29 C30 122.0(9) . . ?
C30 C29 H29 119.0 . . ?
C29 C30 H30 120.8 . . ?
C29 C30 C31 118.4(9) . . ?
C31 C30 H30 120.8 . . ?
C30 C31 H31 119.5 . . ?
C32 C31 C30 121.0(10) . . ?
C32 C31 H31 119.5 . . ?
C31 C32 H32 121.0 . . ?
C33 C32 C31 117.9(10) . . ?
C33 C32 H32 121.0 . . ?
N4 C33 C34 112.4(9) . . ?
C32 C33 N4 122.3(9) . . ?
C32 C33 C34 125.3(10) . . ?
C35 C34 C33 114.0(8) . . ?
C35 C34 C39 115.4(9) . . ?
C39 C34 C33 130.6(9) . . ?
C34 C35 Ir1 118.6(6) . . ?
C34 C35 C36 124.3(9) . . ?
C36 C35 Ir1 117.1(7) . . ?
C35 C36 C37 116.1(9) . . ?
C35 C36 C40 114.1(8) . . ?
C37 C36 C40 129.8(9) . . ?
F2 C37 C36 119.7(10) . . ?
F2 C37 C38 119.4(9) . . ?
C38 C37 C36 120.9(9) . . ?
C37 C38 H38 120.4 . . ?
C39 C38 C37 119.2(10) . . ?
C39 C38 H38 120.4 . . ?
F1 C39 C34 119.2(9) . . ?
C38 C39 F1 116.7(9) . . ?
C38 C39 C34 124.1(10) . . ?
N5 C40 C36 113.0(9) . . ?
N5 C40 C41 119.6(10) . . ?
C41 C40 C36 127.3(9) . . ?
C40 C41 H41 119.4 . . ?
C40 C41 C42 121.2(9) . . ?
C42 C41 H41 119.4 . . ?
C41 C42 H42 120.4 . . ?
C41 C42 C43 119.2(10) . . ?
C43 C42 H42 120.4 . . ?
C42 C43 H43 121.4 . . ?
C44 C43 C42 117.3(10) . . ?
C44 C43 H43 121.4 . . ?
N5 C44 H44 118.2 . . ?
C43 C44 N5 123.5(9) . . ?
C43 C44 H44 118.2 . . ?
N9 C45 H45 117.5 . . ?
N9 C45 C46 124.9(10) . . ?
C46 C45 H45 117.5 . . ?
C45 C46 H46 121.0 . . ?
C45 C46 C47 117.9(10) . . ?
C47 C46 H46 121.0 . . ?
C46 C47 H47 120.6 . . ?
C48 C47 C46 118.8(10) . . ?
C48 C47 H47 120.6 . . ?
C47 C48 H48 119.1 . . ?
C47 C48 C49 121.9(11) . . ?
C49 C48 H48 119.1 . . ?
N9 C49 C48 119.0(9) . . ?
N9 C49 C50 114.0(9) . . ?
C48 C49 C50 126.9(10) . . ?
C51 C50 C49 113.7(9) . . ?
C51 C50 C55 115.7(9) . . ?
C55 C50 C49 130.6(10) . . ?
C50 C51 Ir2 116.8(7) . . ?
C50 C51 C52 124.9(9) . . ?
C52 C51 Ir2 118.3(7) . . ?
C51 C52 C56 112.6(8) . . ?
C53 C52 C51 115.1(9) . . ?
C53 C52 C56 132.2(9) . . ?
C52 C53 F4 119.8(10) . . ?
C52 C53 C54 124.0(10) . . ?
C54 C53 F4 116.1(9) . . ?
C53 C54 H54 120.5 . . ?
C55 C54 C53 118.9(10) . . ?
C55 C54 H54 120.5 . . ?
F3 C55 C50 120.3(9) . . ?
F3 C55 C54 118.4(10) . . ?
C54 C55 C50 121.3(11) . . ?
N10 C56 C52 115.4(8) . . ?
N10 C56 C57 118.1(9) . . ?
C57 C56 C52 126.5(9) . . ?
C56 C57 H57 119.6 . . ?
C58 C57 C56 120.8(9) . . ?
C58 C57 H57 119.6 . . ?
C57 C58 H58 119.6 . . ?
C57 C58 C59 120.8(9) . . ?
C59 C58 H58 119.6 . . ?
C58 C59 H59 121.5 . . ?
C58 C59 C60 117.0(10) . . ?
C60 C59 H59 121.5 . . ?
N10 C60 C59 124.5(9) . . ?
N10 C60 H60 117.8 . . ?
C59 C60 H60 117.8 . . ?
F11 P1 F16 178.9(5) . . ?
F12 P1 F11 89.9(4) . . ?
F12 P1 F13 90.0(4) . . ?
F12 P1 F15 90.5(5) . . ?
F12 P1 F16 90.7(4) . . ?
F13 P1 F11 90.6(4) . . ?
F13 P1 F16 88.4(4) . . ?
F14 P1 F11 89.5(4) . . ?
F14 P1 F12 179.4(5) . . ?
F14 P1 F13 90.1(5) . . ?
F14 P1 F15 89.4(5) . . ?
F14 P1 F16 89.9(4) . . ?
F15 P1 F11 88.0(4) . . ?
F15 P1 F13 178.5(5) . . ?
F15 P1 F16 93.0(4) . . ?
F21 P2 F23 89.8(4) . . ?
F22 P2 F21 89.3(4) . . ?
F22 P2 F23 87.4(4) . . ?
F24 P2 F21 90.9(4) . . ?
F24 P2 F22 175.7(5) . . ?
F24 P2 F23 88.3(4) . . ?
F24 P2 F26 91.0(4) . . ?
F25 P2 F21 88.5(4) . . ?
F25 P2 F22 89.5(5) . . ?
F25 P2 F23 176.5(5) . . ?
F25 P2 F24 94.8(5) . . ?
F25 P2 F26 92.2(4) . . ?
F26 P2 F21 177.9(5) . . ?
F26 P2 F22 88.7(4) . . ?
F26 P2 F23 89.3(4) . . ?
C5S O1S C3S 111.6(11) . . ?
O1S C3S H3SA 111.1 . . ?
O1S C3S H3SB 111.1 . . ?
O1S C3S C4S 103.5(11) . . ?
H3SA C3S H3SB 109.0 . . ?
C4S C3S H3SA 111.1 . . ?
C4S C3S H3SB 111.1 . . ?
C3S C4S H4SA 109.5 . . ?
C3S C4S H4SB 109.5 . . ?
C3S C4S H4SC 109.5 . . ?
H4SA C4S H4SB 109.5 . . ?
H4SA C4S H4SC 109.5 . . ?
H4SB C4S H4SC 109.5 . . ?
O1S C5S H5SA 109.0 . . ?
O1S C5S H5SB 109.0 . . ?
O1S C5S C6S 112.7(13) . . ?
H5SA C5S H5SB 107.8 . . ?
C6S C5S H5SA 109.0 . . ?
C6S C5S H5SB 109.0 . . ?
C5S C6S H6SA 109.5 . . ?
C5S C6S H6SB 109.5 . . ?
C5S C6S H6SC 109.5 . . ?
H6SA C6S H6SB 109.5 . . ?
H6SA C6S H6SC 109.5 . . ?
H6SB C6S H6SC 109.5 . . ?
N1S C1S C2S 177.8(14) . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
N2S C11S C12S 174(3) . . ?
C11S C12S H12D 109.8 . . ?
C11S C12S H12E 109.4 . . ?
C11S C12S H12F 109.2 . . ?
H12D C12S H12E 109.5 . . ?
H12D C12S H12F 109.5 . . ?
H12E C12S H12F 109.5 . . ?
N3S C13S C14S 176.9(18) . . ?
C13S C14S H14A 109.5 . . ?
C13S C14S H14B 109.3 . . ?
C13S C14S H14C 109.6 . . ?
H14A C14S H14B 109.5 . . ?
H14A C14S H14C 109.5 . . ?
H14B C14S H14C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 C13 N2 N1 4.4(12) . . . . ?
N6 C15 N7 N8 2.3(12) . . . . ?
C1 N1 N2 C12 11.2(13) . . . . ?
C1 N1 N2 C13 177.8(9) . . . . ?
C2 C1 N1 Ir1 4.2(13) . . . . ?
C2 C1 N1 N2 -179.2(8) . . . . ?
C3 C2 C1 N1 -3.0(15) . . . . ?
C5 C6 C8 C9 -178.5(9) . . . . ?
C5 C6 C8 C10 61.0(13) . . . . ?
C5 C6 C8 C11 -61.5(12) . . . . ?
C7 C2 C1 N1 178.2(9) . . . . ?
C7 C6 C8 C9 2.5(14) . . . . ?
C7 C6 C8 C10 -118.0(11) . . . . ?
C7 C6 C8 C11 119.6(11) . . . . ?
C12 N2 N1 Ir1 -171.8(7) . . . . ?
C12 N2 C13 N3 170.4(8) . . . . ?
C13 N2 N1 Ir1 -5.3(10) . . . . ?
C14 C13 N2 N1 -176.8(8) . . . . ?
C14 C13 N2 C12 -10.8(15) . . . . ?
C14 C15 N7 N8 -177.7(8) . . . . ?
C14 C15 N7 C17 3.2(16) . . . . ?
C15 N7 N8 Ir2 -5.0(10) . . . . ?
C15 N7 N8 C18 174.4(9) . . . . ?
C17 N7 N8 Ir2 174.1(8) . . . . ?
C17 N7 N8 C18 -6.5(14) . . . . ?
C17 N7 C15 N6 -176.7(9) . . . . ?
C19 C18 N8 Ir2 0.8(14) . . . . ?
C19 C18 N8 N7 -178.5(8) . . . . ?
C20 C19 C18 N8 -4.8(17) . . . . ?
C22 C23 C25 C26 118.6(13) . . . . ?
C22 C23 C25 C27 -118.1(13) . . . . ?
C22 C23 C25 C28 5.3(18) . . . . ?
C24 C19 C18 N8 174.3(9) . . . . ?
C24 C23 C25 C26 -61.0(15) . . . . ?
C24 C23 C25 C27 62.3(16) . . . . ?
C24 C23 C25 C28 -174.3(11) . . . . ?
C32 C33 C34 C35 -178.4(9) . . . . ?
C32 C33 C34 C39 0.0(16) . . . . ?
C35 C34 C33 N4 3.4(11) . . . . ?
C35 C36 C40 N5 5.0(11) . . . . ?
C35 C36 C40 C41 -177.2(9) . . . . ?
C37 C36 C40 N5 -176.9(9) . . . . ?
C37 C36 C40 C41 1.0(16) . . . . ?
C39 C34 C33 N4 -178.2(9) . . . . ?
C48 C49 C50 C51 -176.3(9) . . . . ?
C48 C49 C50 C55 5.0(16) . . . . ?
C51 C50 C49 N9 -1.6(11) . . . . ?
C51 C52 C56 N10 -1.7(11) . . . . ?
C51 C52 C56 C57 177.5(8) . . . . ?
C53 C52 C56 N10 179.4(9) . . . . ?
C53 C52 C56 C57 -1.4(16) . . . . ?
C55 C50 C49 N9 179.8(9) . . . . ?
_iucr_refine_instructions_details
;
TITL 20srv027_a.res in P-1
REM Old TITL 20srv027 in P-1 #2
REM SHELXT solution in P-1
REM R1 0.197, Rweak 0.025, Alpha 0.062, Orientation as input
REM Formula found by SHELXT: C67 N16 O2 F18 Ir2
CELL 0.71073 12.4261 15.8044 19.8347 76.196 74.21 81.438
ZERR 2 0.0012 0.0015 0.0019 0.003 0.003 0.003
LATT 1
SFAC C H F Ir N O P
UNIT 140 142 32 4 26 6 4
RIGU 0.001 0.001 O1S > C6S
RIGU 0.001 0.001 P1 > F16
RIGU 0.001 0.001 P2 > F26
RIGU 0.001 0.001 N1S C1S C2S
RIGU 0.001 0.001 N3S C13S C14S
RIGU 0.001 0.001 N2S C11S C12S
RIGU 0.001 0.001 C25 > C28
ISOR 0.01 0.02 F22
L.S. 9
PLAN 1
SIZE 0.02 0.04 0.46
TEMP -153.15
CONF C22 C23 C25 C26
CONF C24 C23 C25 C26
CONF C22 C23 C25 C27
CONF C24 C23 C25 C27
CONF C22 C23 C25 C28
CONF C24 C23 C25 C28
CONF C20 C19 C18 N8
CONF C24 C19 C18 N8
CONF C19 C18 N8 Ir2
CONF C19 C18 N8 N7
CONF C15 N7 N8 Ir2
CONF C17 N7 N8 Ir2
CONF C15 N7 N8 C18
CONF C17 N7 N8 C18
CONF N6 C15 N7 N8
CONF C14 C15 N7 N8
CONF C17 N7 C15 N6
CONF C14 C15 N7 C17
CONF N3 C13 N2 N1
CONF C14 C13 N2 N1
CONF C12 N2 C13 N3
CONF C14 C13 N2 C12
CONF C12 N2 N1 Ir1
CONF C1 N1 N2 C12
CONF C13 N2 N1 Ir1
CONF C1 N1 N2 C13
CONF C2 C1 N1 Ir1
CONF C2 C1 N1 N2
CONF C3 C2 C1 N1
CONF C7 C2 C1 N1
CONF C5 C6 C8 C9
CONF C7 C6 C8 C9
CONF C5 C6 C8 C10
CONF C7 C6 C8 C10
CONF C5 C6 C8 C11
CONF C7 C6 C8 C11
CONF C51 C52 C56 C57
CONF C53 C52 C56 C57
CONF C51 C52 C56 N10
CONF C53 C52 C56 N10
CONF C48 C49 C50 C51
CONF C51 C50 C49 N9
CONF C48 C49 C50 C55
CONF C55 C50 C49 N9
CONF C35 C36 C40 C41
CONF C37 C36 C40 C41
CONF C35 C36 C40 N5
CONF C37 C36 C40 N5
CONF C35 C34 C33 N4
CONF C32 C33 C34 C35
CONF C39 C34 C33 N4
CONF C32 C33 C34 C39
BOND $h
fmap 2 53
acta
EXTI 0.00097
OMIT -2 54
OMIT 1 1 0
OMIT -1 2 0
WGHT 0.036
FVAR 0.19215
REM
REM
REM
Ir1 4 0.73978 0.58454 0.31858 11.00000 0.02028 0.03886 0.02040 =
-0.00652 -0.00489 0.00324
Ir2 4 0.40364 0.75261 0.15282 11.00000 0.02205 0.04119 0.02299 =
-0.00138 -0.00566 0.00207
F1 3 0.69146 0.89507 0.37922 11.00000 0.05303 0.04545 0.05746 =
-0.01991 -0.01639 0.00516
F2 3 0.38915 0.72537 0.48419 11.00000 0.03405 0.05453 0.04311 =
-0.01514 -0.00181 0.02039
F3 3 0.41701 0.99162 0.29269 11.00000 0.08140 0.05447 0.04616 =
-0.02161 -0.01568 -0.01379
F4 3 0.19841 0.76124 0.42023 11.00000 0.04514 0.08964 0.03045 =
-0.01384 0.00230 -0.01010
O1 6 0.80840 0.54013 0.40354 11.00000 0.02871 0.03849 0.02970 =
-0.01191 -0.01288 0.01516
O2 6 0.26676 0.82239 0.12642 11.00000 0.03207 0.04906 0.02108 =
0.00295 -0.01024 0.00228
N1 5 0.82731 0.48805 0.26454 11.00000 0.02974 0.03647 0.02797 =
-0.01173 -0.01477 0.00702
N2 5 0.80501 0.49407 0.19885 11.00000 0.02532 0.04607 0.02367 =
-0.01365 -0.00659 0.01009
N3 5 0.67752 0.61104 0.23072 11.00000 0.01790 0.03936 0.02248 =
-0.00641 -0.00514 0.00966
N4 5 0.85483 0.67643 0.28088 11.00000 0.02188 0.02751 0.03159 =
-0.01655 -0.01369 0.00511
N5 5 0.59401 0.52841 0.37420 11.00000 0.01595 0.05184 0.03270 =
-0.01323 -0.00740 0.00398
N6 5 0.54272 0.67666 0.16674 11.00000 0.02573 0.03954 0.02162 =
-0.01041 -0.00548 0.00369
N7 5 0.53916 0.63633 0.06162 11.00000 0.04412 0.04195 0.02989 =
-0.00937 -0.01988 0.01347
N8 5 0.44718 0.69827 0.06291 11.00000 0.02875 0.03337 0.03291 =
-0.00747 -0.01958 -0.00003
N9 5 0.48987 0.85976 0.11249 11.00000 0.03621 0.04935 0.02268 =
-0.00962 -0.01200 0.00886
N10 5 0.30517 0.65993 0.22361 11.00000 0.02167 0.03740 0.02793 =
0.00224 -0.01315 0.00229
C1 1 0.90132 0.42860 0.28683 11.00000 0.02044 0.03707 0.03763 =
-0.01090 -0.01075 0.00361
AFIX 43
H1 2 0.94029 0.38985 0.25641 11.00000 -1.20000
AFIX 0
C2 1 0.92789 0.41790 0.35516 11.00000 0.01970 0.04448 0.02488 =
0.00055 -0.00637 0.00059
C3 1 0.88241 0.47149 0.40542 11.00000 0.01976 0.03231 0.02561 =
-0.01259 -0.00154 -0.00662
C4 1 0.92089 0.44626 0.46924 11.00000 0.01980 0.04692 0.03117 =
-0.00898 -0.01367 0.00206
AFIX 43
H4 2 0.89156 0.47914 0.50560 11.00000 -1.20000
AFIX 0
C5 1 0.99872 0.37632 0.48055 11.00000 0.02578 0.04622 0.02674 =
0.00193 -0.01459 -0.00097
AFIX 43
H5 2 1.02185 0.36336 0.52407 11.00000 -1.20000
AFIX 0
C6 1 1.04502 0.32367 0.43072 11.00000 0.02711 0.04522 0.02762 =
0.00666 -0.01001 -0.00509
C7 1 1.00842 0.34750 0.36886 11.00000 0.02528 0.03315 0.03403 =
-0.00169 -0.00110 0.00077
AFIX 43
H7 2 1.03950 0.31428 0.33289 11.00000 -1.20000
AFIX 0
C8 1 1.12726 0.24643 0.44757 11.00000 0.02706 0.04913 0.03954 =
-0.00565 -0.00693 0.01001
C9 1 1.17081 0.19817 0.38435 11.00000 0.04458 0.06100 0.07740 =
-0.02879 -0.04189 0.02549
AFIX 137
H9A 2 1.10743 0.17689 0.37476 11.00000 -1.50000
H9B 2 1.22430 0.14854 0.39687 11.00000 -1.50000
H9C 2 1.20818 0.23862 0.34153 11.00000 -1.50000
AFIX 0
C10 1 1.07658 0.17942 0.51338 11.00000 0.04561 0.04615 0.06581 =
0.00760 -0.01617 -0.00725
AFIX 137
H10A 2 1.04722 0.20783 0.55439 11.00000 -1.50000
H10B 2 1.13450 0.13251 0.52391 11.00000 -1.50000
H10C 2 1.01538 0.15475 0.50424 11.00000 -1.50000
AFIX 0
C11 1 1.23134 0.27668 0.45861 11.00000 0.03105 0.07360 0.05557 =
-0.02115 -0.01991 0.01596
AFIX 137
H11A 2 1.27042 0.31311 0.41384 11.00000 -1.50000
H11B 2 1.28169 0.22555 0.47278 11.00000 -1.50000
H11C 2 1.20863 0.31078 0.49628 11.00000 -1.50000
AFIX 0
C12 1 0.84901 0.42407 0.15963 11.00000 0.05092 0.05413 0.04420 =
-0.02680 -0.02629 0.01901
AFIX 137
H12A 2 0.92522 0.43452 0.13056 11.00000 -1.50000
H12B 2 0.80060 0.42278 0.12834 11.00000 -1.50000
H12C 2 0.85079 0.36788 0.19363 11.00000 -1.50000
AFIX 0
C13 1 0.72365 0.55658 0.18305 11.00000 0.01778 0.04085 0.02367 =
-0.00344 -0.00573 0.00429
C14 1 0.68596 0.56941 0.12074 11.00000 0.02863 0.04716 0.01894 =
-0.00458 -0.00793 0.00301
AFIX 43
H14 2 0.72433 0.54012 0.08316 11.00000 -1.20000
AFIX 0
C15 1 0.59062 0.62636 0.11555 11.00000 0.02861 0.03997 0.02673 =
-0.00350 -0.00170 -0.00924
C16 1 0.59284 0.66809 0.21916 11.00000 0.01794 0.03687 0.02737 =
-0.00739 -0.00046 0.00278
AFIX 43
H16 2 0.56507 0.70669 0.25136 11.00000 -1.20000
AFIX 0
C17 1 0.57330 0.58665 0.00605 11.00000 0.07236 0.07325 0.04868 =
-0.03261 -0.03186 0.02427
AFIX 137
H17A 2 0.50662 0.57190 -0.00453 11.00000 -1.50000
H17B 2 0.61794 0.53275 0.02207 11.00000 -1.50000
H17C 2 0.61858 0.62148 -0.03724 11.00000 -1.50000
AFIX 0
C18 1 0.39792 0.71770 0.01044 11.00000 0.03782 0.04381 0.03498 =
-0.00993 -0.01549 0.00114
AFIX 43
H18 2 0.42452 0.68798 -0.02812 11.00000 -1.20000
AFIX 0
C19 1 0.30351 0.78351 0.00926 11.00000 0.03252 0.04484 0.02684 =
-0.00219 -0.01370 -0.00207
C20 1 0.24635 0.83059 0.06283 11.00000 0.02708 0.04206 0.02695 =
0.00351 -0.00627 -0.00848
C21 1 0.16105 0.89196 0.04866 11.00000 0.03960 0.07646 0.02827 =
-0.01426 -0.00279 0.01167
AFIX 43
H21 2 0.12073 0.92385 0.08413 11.00000 -1.20000
AFIX 0
C22 1 0.13111 0.90925 -0.01845 11.00000 0.04253 0.07086 0.05765 =
-0.00644 -0.01139 0.01048
AFIX 43
H22 2 0.07264 0.95345 -0.02682 11.00000 -1.20000
AFIX 0
C23 1 0.18489 0.86344 -0.07136 11.00000 0.04214 0.03242 0.03830 =
-0.00228 -0.02219 0.00308
C24 1 0.26865 0.80108 -0.05556 11.00000 0.04469 0.03966 0.04756 =
-0.00676 -0.02904 0.01351
AFIX 43
H24 2 0.30590 0.76734 -0.09033 11.00000 -1.20000
AFIX 0
C25 1 0.15383 0.88139 -0.14191 11.00000 0.08888 0.07074 0.04558 =
-0.01253 -0.04631 0.01391
C26 1 0.25120 0.91053 -0.20108 11.00000 0.10015 0.16754 0.06954 =
0.01873 -0.04271 -0.00425
AFIX 137
H26A 2 0.27972 0.95996 -0.19159 11.00000 -1.50000
H26B 2 0.22791 0.92871 -0.24619 11.00000 -1.50000
H26C 2 0.31048 0.86222 -0.20466 11.00000 -1.50000
AFIX 0
C27 1 0.11347 0.80503 -0.15199 11.00000 0.15018 0.08108 0.09081 =
-0.02109 -0.08831 0.00601
AFIX 137
H27A 2 0.16950 0.75489 -0.14650 11.00000 -1.50000
H27B 2 0.10072 0.81642 -0.20011 11.00000 -1.50000
H27C 2 0.04289 0.79210 -0.11619 11.00000 -1.50000
AFIX 0
C28 1 0.06786 0.95830 -0.15035 11.00000 0.12664 0.08974 0.09674 =
-0.03224 -0.07752 0.03934
AFIX 137
H28A 2 -0.00104 0.94701 -0.11249 11.00000 -1.50000
H28B 2 0.05128 0.96716 -0.19724 11.00000 -1.50000
H28C 2 0.09730 1.01084 -0.14683 11.00000 -1.50000
AFIX 0
C29 1 0.95652 0.66764 0.23601 11.00000 0.02835 0.03858 0.03935 =
-0.01069 -0.01250 0.01470
AFIX 43
H29 2 0.97858 0.61570 0.21768 11.00000 -1.20000
AFIX 0
C30 1 1.02992 0.73179 0.21574 11.00000 0.02676 0.04474 0.03065 =
-0.00126 -0.00468 -0.00583
AFIX 43
H30 2 1.10047 0.72537 0.18261 11.00000 -1.20000
AFIX 0
C31 1 0.99836 0.80555 0.24478 11.00000 0.04011 0.05094 0.05671 =
0.00162 -0.02108 -0.01647
AFIX 43
H31 2 1.04993 0.84848 0.23404 11.00000 -1.20000
AFIX 0
C32 1 0.89369 0.81780 0.28890 11.00000 0.03548 0.04274 0.03902 =
-0.00239 -0.01477 -0.01101
AFIX 43
H32 2 0.87023 0.87021 0.30643 11.00000 -1.20000
AFIX 0
C33 1 0.82411 0.75220 0.30688 11.00000 0.03972 0.03783 0.02394 =
0.00335 -0.01551 0.00563
C34 1 0.70939 0.75431 0.35300 11.00000 0.01628 0.03448 0.03124 =
-0.00936 -0.01547 0.01095
C35 1 0.65798 0.67911 0.36435 11.00000 0.02219 0.04090 0.01756 =
0.00042 -0.00595 -0.00558
C36 1 0.54987 0.66504 0.40800 11.00000 0.02591 0.03880 0.02896 =
-0.00513 -0.01028 0.00290
C37 1 0.49271 0.73409 0.44111 11.00000 0.02235 0.06123 0.01600 =
-0.00911 0.00172 0.01106
C38 1 0.54191 0.81003 0.43058 11.00000 0.05855 0.03479 0.03440 =
-0.01032 -0.00244 0.01163
AFIX 43
H38 2 0.50284 0.85624 0.45319 11.00000 -1.20000
AFIX 0
C39 1 0.64668 0.81825 0.38762 11.00000 0.03803 0.04224 0.03288 =
-0.00495 -0.01509 0.00006
C40 1 0.51272 0.58071 0.41044 11.00000 0.02311 0.05612 0.02881 =
-0.01021 -0.00653 0.00850
C41 1 0.41036 0.55031 0.44590 11.00000 0.02504 0.05310 0.02339 =
-0.01114 -0.00591 0.00204
AFIX 43
H41 2 0.35453 0.58638 0.47203 11.00000 -1.20000
AFIX 0
C42 1 0.38695 0.46856 0.44436 11.00000 0.02268 0.07093 0.02273 =
-0.00167 -0.00669 -0.00135
AFIX 43
H42 2 0.31582 0.44810 0.46945 11.00000 -1.20000
AFIX 0
C43 1 0.46979 0.41540 0.40510 11.00000 0.03471 0.04595 0.03538 =
0.00289 -0.01253 -0.00860
AFIX 43
H43 2 0.45587 0.35901 0.40227 11.00000 -1.20000
AFIX 0
C44 1 0.56993 0.44803 0.37161 11.00000 0.02288 0.04747 0.02645 =
-0.00351 -0.00630 0.00752
AFIX 43
H44 2 0.62646 0.41302 0.34486 11.00000 -1.20000
AFIX 0
C45 1 0.55907 0.88258 0.04663 11.00000 0.03839 0.03911 0.03014 =
0.00108 0.00193 -0.00701
AFIX 43
H45 2 0.56673 0.84589 0.01370 11.00000 -1.20000
AFIX 0
C46 1 0.61834 0.95400 0.02409 11.00000 0.04983 0.04366 0.02810 =
0.00492 -0.00696 -0.00609
AFIX 43
H46 2 0.66707 0.96585 -0.02251 11.00000 -1.20000
AFIX 0
C47 1 0.60553 1.00917 0.07129 11.00000 0.06497 0.03705 0.03968 =
0.01485 -0.02144 -0.01542
AFIX 43
H47 2 0.64331 1.06098 0.05703 11.00000 -1.20000
AFIX 0
C48 1 0.53778 0.98762 0.13841 11.00000 0.06632 0.03729 0.04423 =
-0.00305 -0.02544 0.00095
AFIX 43
H48 2 0.53083 1.02409 0.17140 11.00000 -1.20000
AFIX 0
C49 1 0.47825 0.91344 0.16010 11.00000 0.02695 0.04151 0.03627 =
-0.00770 -0.01665 0.01663
C50 1 0.40915 0.88034 0.23194 11.00000 0.02261 0.04804 0.03562 =
-0.01241 -0.00590 0.00928
C51 1 0.36579 0.80226 0.23837 11.00000 0.02451 0.03770 0.04039 =
-0.00913 -0.01254 0.00610
C52 1 0.29398 0.75909 0.30017 11.00000 0.02653 0.03138 0.02812 =
-0.01095 -0.00448 0.00748
C53 1 0.26863 0.79846 0.35648 11.00000 0.03762 0.04954 0.02835 =
-0.00246 -0.01250 0.01558
C54 1 0.30868 0.87540 0.35524 11.00000 0.03936 0.04988 0.04337 =
-0.01179 -0.01562 0.00159
AFIX 43
H54 2 0.28795 0.90042 0.39652 11.00000 -1.20000
AFIX 0
C55 1 0.37904 0.91549 0.29348 11.00000 0.03091 0.04485 0.04384 =
-0.00610 -0.01232 0.00611
C56 1 0.26231 0.67879 0.29120 11.00000 0.01900 0.04598 0.02508 =
0.00358 -0.00600 -0.00225
C57 1 0.19490 0.61932 0.34367 11.00000 0.03083 0.04027 0.03618 =
0.00317 -0.00148 -0.00209
AFIX 43
H57 2 0.16342 0.63142 0.39007 11.00000 -1.20000
AFIX 0
C58 1 0.17395 0.54435 0.32895 11.00000 0.03067 0.05806 0.03659 =
0.02470 -0.00515 -0.01175
AFIX 43
H58 2 0.12791 0.50484 0.36521 11.00000 -1.20000
AFIX 0
C59 1 0.21833 0.52524 0.26267 11.00000 0.03974 0.05160 0.03325 =
0.00495 -0.01441 -0.01150
AFIX 43
H59 2 0.20480 0.47289 0.25197 11.00000 -1.20000
AFIX 0
C60 1 0.28348 0.58525 0.21219 11.00000 0.03713 0.04103 0.02756 =
-0.00385 -0.01603 -0.00004
AFIX 43
H60 2 0.31516 0.57254 0.16600 11.00000 -1.20000
AFIX 0
P1 7 0.50337 0.35747 0.20955 11.00000 0.06017 0.07190 0.04136 =
-0.00983 -0.01354 -0.01043
F11 3 0.50152 0.26504 0.19185 11.00000 0.10773 0.08657 0.08045 =
-0.03451 -0.00678 -0.01852
F12 3 0.59305 0.31693 0.25321 11.00000 0.11039 0.12273 0.11213 =
-0.02624 -0.06776 0.01616
F13 3 0.40653 0.33495 0.27962 11.00000 0.10406 0.10791 0.06147 =
-0.02577 0.01408 -0.03679
F14 3 0.41412 0.39697 0.16564 11.00000 0.11139 0.12911 0.08398 =
-0.03890 -0.05887 0.01503
F15 3 0.59859 0.37792 0.13917 11.00000 0.10783 0.10232 0.07103 =
-0.03181 0.02195 -0.02471
F16 3 0.50266 0.45023 0.22805 11.00000 0.08049 0.08355 0.05760 =
-0.02326 -0.00826 -0.01690
P2 7 1.13273 0.55051 0.06595 11.00000 0.05477 0.10382 0.04776 =
-0.03430 -0.00728 -0.01549
F21 3 1.14068 0.45927 0.04217 11.00000 0.08105 0.12913 0.08210 =
-0.06560 -0.00455 -0.02224
F22 3 1.25569 0.52494 0.07988 11.00000 0.05811 0.16082 0.12349 =
-0.09122 -0.02357 0.00552
F23 3 1.08376 0.50331 0.14835 11.00000 0.08700 0.08823 0.05352 =
-0.02440 -0.00990 0.00652
F24 3 1.00930 0.57243 0.05841 11.00000 0.07842 0.11819 0.11066 =
-0.01895 -0.05150 -0.01170
F25 3 1.18577 0.59158 -0.01221 11.00000 0.15179 0.16139 0.04689 =
-0.04414 0.00769 -0.06369
F26 3 1.12832 0.63980 0.09119 11.00000 0.07759 0.10071 0.05181 =
-0.03292 -0.00331 -0.01823
O1S 6 -0.03356 1.10270 0.33006 11.00000 0.09673 0.09213 0.09800 =
-0.03141 -0.03117 0.00497
C3S 1 0.03836 1.01802 0.32761 11.00000 0.08033 0.08843 0.13730 =
-0.04695 -0.04741 -0.00213
AFIX 23
H3SA 2 -0.00415 0.97216 0.32328 11.00000 -1.20000
H3SB 2 0.06754 0.99758 0.37103 11.00000 -1.20000
AFIX 0
C4S 1 0.13821 1.04183 0.25757 11.00000 0.09551 0.15167 0.11764 =
-0.03522 -0.04490 0.03693
AFIX 137
H4SA 2 0.10691 1.07529 0.21779 11.00000 -1.50000
H4SB 2 0.17998 0.98784 0.24488 11.00000 -1.50000
H4SC 2 0.18889 1.07695 0.26717 11.00000 -1.50000
AFIX 0
C5S 1 -0.12666 1.09325 0.38380 11.00000 0.10469 0.11392 0.09587 =
-0.06515 -0.02490 -0.01584
AFIX 23
H5SA 2 -0.10495 1.06671 0.42926 11.00000 -1.20000
H5SB 2 -0.17278 1.05266 0.37540 11.00000 -1.20000
AFIX 0
C6S 1 -0.19539 1.17763 0.39100 11.00000 0.08626 0.10740 0.12618 =
-0.06878 -0.00312 -0.03112
AFIX 137
H6SA 2 -0.20947 1.20767 0.34452 11.00000 -1.50000
H6SB 2 -0.15487 1.21451 0.40717 11.00000 -1.50000
H6SC 2 -0.26708 1.16629 0.42607 11.00000 -1.50000
AFIX 0
N1S 5 0.36773 1.00389 0.47282 11.00000 0.06588 0.08256 0.07260 =
-0.02480 -0.02166 0.01084
C1S 1 0.42759 1.04962 0.43135 11.00000 0.05961 0.07009 0.05419 =
-0.03740 -0.02246 0.01570
C2S 1 0.50804 1.10956 0.37930 11.00000 0.08006 0.09968 0.06309 =
-0.02978 -0.01620 -0.00244
AFIX 3
H2SA 2 0.48548 1.16948 0.38662 11.00000 -1.50000
H2SB 2 0.50792 1.10726 0.33038 11.00000 -1.50000
H2SC 2 0.58366 1.09144 0.38662 11.00000 -1.50000
AFIX 0
N2S 5 0.72209 0.79009 -0.07677 11.00000 0.18220 0.24876 0.16597 =
-0.13854 0.02129 0.00021
C11S 1 0.75497 0.75934 -0.12165 11.00000 0.15109 0.10821 0.09929 =
-0.04282 0.01803 -0.00665
C12S 1 0.80759 0.71318 -0.17883 11.00000 0.13819 0.11410 0.09060 =
-0.03971 0.00720 0.00246
AFIX 3
H12D 2 0.81118 0.75327 -0.22530 11.00000 -1.50000
H12E 2 0.76369 0.66480 -0.17485 11.00000 -1.50000
H12F 2 0.88377 0.68996 -0.17485 11.00000 -1.50000
AFIX 0
N3S 5 0.74414 0.81249 0.16037 11.00000 0.05885 0.12968 0.08875 =
0.00410 -0.03898 -0.01022
C13S 1 0.80960 0.79772 0.10933 11.00000 0.05981 0.08398 0.08622 =
0.02191 -0.03392 -0.01259
C14S 1 0.88579 0.77587 0.04779 11.00000 0.07547 0.12509 0.10993 =
0.00748 -0.00980 -0.01576
AFIX 3
H14A 2 0.86574 0.81266 0.00488 11.00000 -1.50000
H14B 2 0.96182 0.78565 0.04782 11.00000 -1.50000
H14C 2 0.88310 0.71420 0.04782 11.00000 -1.50000
AFIX 0
HKLF 4
END
;
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_H2L7_16srv303
_database_code_depnum_ccdc_archive 'CCDC 2006846'
loop_
_audit_author_name
_audit_author_address
'Dmitry Yufit'
;Durham University
United Kingdom
;
_audit_update_record
;
2020-06-01 deposited with the CCDC. 2020-07-10 downloaded from the CCDC.
;
_audit_creation_date 2016-08-18
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.07.26 svn.r3321 for OlexSys, GUI svn.r5206)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C36 H52 N6 O2'
_chemical_formula_sum 'C36 H52 N6 O2'
_chemical_formula_weight 600.83
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 12.1186(12)
_cell_length_b 12.2241(10)
_cell_length_c 12.9851(11)
_cell_angle_alpha 72.172(3)
_cell_angle_beta 77.714(3)
_cell_angle_gamma 88.934(3)
_cell_volume 1787.0(3)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 2715
_cell_measurement_temperature 120.0
_cell_measurement_theta_max 30.75
_cell_measurement_theta_min 2.39
_shelx_estimated_absorpt_T_max 0.996
_shelx_estimated_absorpt_T_min 0.978
_exptl_absorpt_coefficient_mu 0.070
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.9063
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1384 before and 0.0494 after correction.
The Ratio of minimum to maximum transmission is 0.9063.
The \l/2 correction factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.117
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description prism
_exptl_crystal_F_000 652
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.11
_exptl_crystal_size_min 0.05
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0442
_diffrn_reflns_av_unetI/netI 0.0629
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 28016
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.000
_diffrn_reflns_theta_min 2.395
_diffrn_ambient_temperature 120.0
_diffrn_detector 'Bruker PHOTON 100 CMOS'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type 'CMOS sensor'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device '3-circle diffractometer'
_diffrn_measurement_device_type 'Bruker D8 Venture'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator 'focusing mirrors'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_type 'Incoatec I\mS microsource'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 6374
_reflns_number_total 9488
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing.bruker_data_scaling 'SADABS V2012/1 (Bruker AXS Inc.)'
_computing_cell_refinement 'APEX2 v.2013.4_1 (Bruker, 2013)'
_computing_data_collection 'APEX2 v.2013.4_1 (Bruker, 2013)'
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max 0.350
_refine_diff_density_min -0.323
_refine_diff_density_rms 0.050
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.021
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 417
_refine_ls_number_reflns 9488
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0964
_refine_ls_R_factor_gt 0.0556
_refine_ls_restrained_S_all 1.021
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.4700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1208
_refine_ls_wR_factor_ref 0.1369
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H) groups
2. Restrained distances
O2-H2 = O1-H1
0.95 with sigma of 0.005
3.a Aromatic/amide H refined with riding coordinates:
C1(H1A), C5(H5), C7(H7), C18(H18), C20(H20), C22(H22), C26(H26), C28(H28)
3.b Idealised Me refined as rotating group:
C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C21(H21A,
H21B,H21C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C),
C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary iterative
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.62599(9) 0.12922(9) 0.75468(9) 0.0219(2) Uani 1 1 d D . . . .
H1 H 0.6089(15) 0.0512(6) 0.7966(13) 0.033 Uiso 1 1 d DR . . . .
O2 O 0.32316(9) 0.04765(9) 0.69711(9) 0.0231(2) Uani 1 1 d D . . . .
H2 H 0.3698(13) -0.0132(11) 0.6886(15) 0.035 Uiso 1 1 d DR . . . .
N1 N 0.60648(10) -0.06622(10) 0.91915(10) 0.0167(3) Uani 1 1 d . . . . .
N2 N 0.58380(11) -0.18307(10) 0.96522(10) 0.0184(3) Uani 1 1 d . . . . .
N3 N 0.57050(10) -0.35606(10) 0.93052(10) 0.0192(3) Uani 1 1 d . . . . .
N4 N 0.53301(10) -0.36699(10) 0.76012(10) 0.0190(3) Uani 1 1 d . . . . .
N5 N 0.48169(10) -0.20877(10) 0.63083(10) 0.0181(3) Uani 1 1 d . . . . .
N6 N 0.42012(10) -0.11219(10) 0.61953(10) 0.0165(3) Uani 1 1 d . . . . .
C1 C 0.64696(12) -0.01015(13) 0.97360(12) 0.0185(3) Uani 1 1 d . . . . .
H1A H 0.6546 -0.0496 1.0469 0.022 Uiso 1 1 calc R . . . .
C2 C 0.68128(12) 0.11184(12) 0.92611(12) 0.0167(3) Uani 1 1 d . . . . .
C3 C 0.67365(12) 0.17809(12) 0.81817(12) 0.0172(3) Uani 1 1 d . . . . .
C4 C 0.71439(12) 0.29428(12) 0.77434(12) 0.0173(3) Uani 1 1 d . . . . .
C5 C 0.76017(12) 0.33907(13) 0.84354(12) 0.0181(3) Uani 1 1 d . . . . .
H5 H 0.7882 0.4170 0.8154 0.022 Uiso 1 1 calc R . . . .
C6 C 0.76772(12) 0.27656(13) 0.95252(12) 0.0175(3) Uani 1 1 d . . . . .
C7 C 0.72795(12) 0.16276(13) 0.99132(12) 0.0184(3) Uani 1 1 d . . . . .
H7 H 0.7324 0.1179 1.0642 0.022 Uiso 1 1 calc R . . . .
C8 C 0.70794(13) 0.36802(13) 0.65598(12) 0.0185(3) Uani 1 1 d . . . . .
C9 C 0.77126(13) 0.31227(14) 0.56979(13) 0.0244(3) Uani 1 1 d . . . . .
H9A H 0.8510 0.3067 0.5740 0.037 Uiso 1 1 calc GR . . . .
H9B H 0.7654 0.3597 0.4953 0.037 Uiso 1 1 calc GR . . . .
H9C H 0.7375 0.2351 0.5854 0.037 Uiso 1 1 calc GR . . . .
C10 C 0.58274(13) 0.38242(13) 0.64758(13) 0.0213(3) Uani 1 1 d . . . . .
H10A H 0.5451 0.3065 0.6657 0.032 Uiso 1 1 calc GR . . . .
H10B H 0.5790 0.4281 0.5720 0.032 Uiso 1 1 calc GR . . . .
H10C H 0.5448 0.4217 0.6998 0.032 Uiso 1 1 calc GR . . . .
C11 C 0.76280(14) 0.48913(13) 0.62514(13) 0.0248(4) Uani 1 1 d . . . . .
H11A H 0.7232 0.5287 0.6764 0.037 Uiso 1 1 calc GR . . . .
H11B H 0.7578 0.5327 0.5493 0.037 Uiso 1 1 calc GR . . . .
H11C H 0.8424 0.4833 0.6300 0.037 Uiso 1 1 calc GR . . . .
C12 C 0.82188(12) 0.33337(13) 1.02140(12) 0.0182(3) Uani 1 1 d . . . . .
C13 C 0.81104(17) 0.25483(15) 1.14075(14) 0.0331(4) Uani 1 1 d . . . . .
H13A H 0.7311 0.2337 1.1752 0.050 Uiso 1 1 calc GR . . . .
H13B H 0.8429 0.2955 1.1830 0.050 Uiso 1 1 calc GR . . . .
H13C H 0.8522 0.1851 1.1404 0.050 Uiso 1 1 calc GR . . . .
C14 C 0.94807(14) 0.36146(16) 0.96759(16) 0.0323(4) Uani 1 1 d . . . . .
H14A H 0.9851 0.2907 0.9629 0.048 Uiso 1 1 calc GR . . . .
H14B H 0.9834 0.3955 1.0126 0.048 Uiso 1 1 calc GR . . . .
H14C H 0.9562 0.4161 0.8930 0.048 Uiso 1 1 calc GR . . . .
C15 C 0.76411(14) 0.44546(14) 1.02598(14) 0.0256(4) Uani 1 1 d . . . . .
H15A H 0.7735 0.4990 0.9507 0.038 Uiso 1 1 calc GR . . . .
H15B H 0.7987 0.4804 1.0709 0.038 Uiso 1 1 calc GR . . . .
H15C H 0.6834 0.4283 1.0593 0.038 Uiso 1 1 calc GR . . . .
C16 C 0.61295(15) -0.24424(13) 1.07068(13) 0.0250(4) Uani 1 1 d . . . . .
H16A H 0.6941 -0.2322 1.0646 0.038 Uiso 1 1 calc GR . . . .
H16B H 0.5942 -0.3266 1.0894 0.038 Uiso 1 1 calc GR . . . .
H16C H 0.5701 -0.2150 1.1289 0.038 Uiso 1 1 calc GR . . . .
C17 C 0.55966(12) -0.24104(12) 0.89578(12) 0.0157(3) Uani 1 1 d . . . . .
C18 C 0.52820(12) -0.18485(12) 0.79602(12) 0.0162(3) Uani 1 1 d . . . . .
H18 H 0.5167 -0.1047 0.7739 0.019 Uiso 1 1 calc R . . . .
C19 C 0.51472(12) -0.25338(12) 0.73092(12) 0.0162(3) Uani 1 1 d . . . . .
C20 C 0.55747(13) -0.41034(13) 0.85944(13) 0.0206(3) Uani 1 1 d . . . . .
H20 H 0.5669 -0.4909 0.8825 0.025 Uiso 1 1 calc R . . . .
C21 C 0.48856(14) -0.27446(14) 0.55345(13) 0.0245(3) Uani 1 1 d . . . . .
H21A H 0.4126 -0.3032 0.5564 0.037 Uiso 1 1 calc GR . . . .
H21B H 0.5365 -0.3396 0.5736 0.037 Uiso 1 1 calc GR . . . .
H21C H 0.5212 -0.2249 0.4782 0.037 Uiso 1 1 calc GR . . . .
C22 C 0.37222(12) -0.07432(12) 0.53627(12) 0.0171(3) Uani 1 1 d . . . . .
H22 H 0.3862 -0.1096 0.4793 0.021 Uiso 1 1 calc R . . . .
C23 C 0.29710(12) 0.02141(12) 0.52762(12) 0.0164(3) Uani 1 1 d . . . . .
C24 C 0.27038(12) 0.07672(13) 0.60955(12) 0.0178(3) Uani 1 1 d . . . . .
C25 C 0.18884(13) 0.16116(13) 0.60304(12) 0.0196(3) Uani 1 1 d . . . . .
C26 C 0.13920(12) 0.18851(13) 0.51096(12) 0.0191(3) Uani 1 1 d . . . . .
H26 H 0.0851 0.2461 0.5049 0.023 Uiso 1 1 calc R . . . .
C27 C 0.16419(12) 0.13625(13) 0.42702(12) 0.0170(3) Uani 1 1 d . . . . .
C28 C 0.24379(12) 0.05284(12) 0.43724(12) 0.0168(3) Uani 1 1 d . . . . .
H28 H 0.2629 0.0159 0.3817 0.020 Uiso 1 1 calc R . . . .
C29 C 0.15579(14) 0.21873(14) 0.69469(13) 0.0247(4) Uani 1 1 d . . . . .
C30 C 0.11150(16) 0.12671(16) 0.80789(14) 0.0342(4) Uani 1 1 d . . . . .
H30A H 0.0446 0.0851 0.8047 0.051 Uiso 1 1 calc GR . . . .
H30B H 0.0913 0.1642 0.8657 0.051 Uiso 1 1 calc GR . . . .
H30C H 0.1705 0.0725 0.8251 0.051 Uiso 1 1 calc GR . . . .
C31 C 0.25863(15) 0.28824(15) 0.69857(14) 0.0300(4) Uani 1 1 d . . . . .
H31A H 0.3193 0.2363 0.7160 0.045 Uiso 1 1 calc GR . . . .
H31B H 0.2368 0.3262 0.7558 0.045 Uiso 1 1 calc GR . . . .
H31C H 0.2853 0.3464 0.6264 0.045 Uiso 1 1 calc GR . . . .
C32 C 0.06004(15) 0.30228(17) 0.67383(15) 0.0341(4) Uani 1 1 d . . . . .
H32A H 0.0844 0.3617 0.6020 0.051 Uiso 1 1 calc GR . . . .
H32B H 0.0425 0.3385 0.7327 0.051 Uiso 1 1 calc GR . . . .
H32C H -0.0075 0.2596 0.6735 0.051 Uiso 1 1 calc GR . . . .
C33 C 0.09922(12) 0.16810(13) 0.33293(12) 0.0188(3) Uani 1 1 d . . . . .
C34 C 0.13245(16) 0.09537(18) 0.25468(16) 0.0390(5) Uani 1 1 d . . . . .
H34A H 0.2139 0.1065 0.2229 0.059 Uiso 1 1 calc GR . . . .
H34B H 0.0910 0.1192 0.1949 0.059 Uiso 1 1 calc GR . . . .
H34C H 0.1137 0.0140 0.2961 0.059 Uiso 1 1 calc GR . . . .
C35 C -0.02803(13) 0.14788(16) 0.38213(14) 0.0303(4) Uani 1 1 d . . . . .
H35A H -0.0449 0.0667 0.4254 0.045 Uiso 1 1 calc GR . . . .
H35B H -0.0692 0.1682 0.3221 0.045 Uiso 1 1 calc GR . . . .
H35C H -0.0514 0.1959 0.4304 0.045 Uiso 1 1 calc GR . . . .
C36 C 0.12537(17) 0.29491(16) 0.26416(15) 0.0388(5) Uani 1 1 d . . . . .
H36A H 0.1001 0.3436 0.3114 0.058 Uiso 1 1 calc GR . . . .
H36B H 0.0857 0.3139 0.2030 0.058 Uiso 1 1 calc GR . . . .
H36C H 0.2070 0.3083 0.2341 0.058 Uiso 1 1 calc GR . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0339(6) 0.0167(5) 0.0202(6) -0.0067(4) -0.0152(5) -0.0003(5)
O2 0.0300(6) 0.0263(6) 0.0196(6) -0.0105(5) -0.0151(5) 0.0114(5)
N1 0.0195(6) 0.0141(6) 0.0174(6) -0.0047(5) -0.0064(5) 0.0017(5)
N2 0.0255(7) 0.0134(6) 0.0172(6) -0.0029(5) -0.0095(5) 0.0003(5)
N3 0.0226(7) 0.0136(6) 0.0203(6) -0.0023(5) -0.0066(5) -0.0001(5)
N4 0.0204(6) 0.0144(6) 0.0236(7) -0.0069(5) -0.0064(5) 0.0013(5)
N5 0.0230(7) 0.0167(6) 0.0190(6) -0.0087(5) -0.0096(5) 0.0047(5)
N6 0.0162(6) 0.0151(6) 0.0182(6) -0.0047(5) -0.0047(5) 0.0004(5)
C1 0.0216(8) 0.0191(7) 0.0164(7) -0.0057(6) -0.0073(6) 0.0032(6)
C2 0.0181(7) 0.0168(7) 0.0186(7) -0.0083(6) -0.0071(6) 0.0031(6)
C3 0.0203(7) 0.0190(7) 0.0173(7) -0.0099(6) -0.0086(6) 0.0037(6)
C4 0.0193(7) 0.0186(7) 0.0158(7) -0.0061(6) -0.0071(6) 0.0044(6)
C5 0.0214(7) 0.0158(7) 0.0193(7) -0.0068(6) -0.0074(6) 0.0014(6)
C6 0.0179(7) 0.0203(8) 0.0181(7) -0.0089(6) -0.0077(6) 0.0022(6)
C7 0.0219(8) 0.0196(7) 0.0164(7) -0.0064(6) -0.0086(6) 0.0033(6)
C8 0.0237(8) 0.0187(7) 0.0153(7) -0.0058(6) -0.0080(6) 0.0013(6)
C9 0.0260(8) 0.0304(9) 0.0194(8) -0.0099(7) -0.0076(7) 0.0027(7)
C10 0.0269(8) 0.0217(8) 0.0178(7) -0.0065(6) -0.0100(6) 0.0036(6)
C11 0.0328(9) 0.0231(8) 0.0176(8) -0.0026(6) -0.0089(7) -0.0040(7)
C12 0.0222(8) 0.0193(7) 0.0177(7) -0.0078(6) -0.0111(6) 0.0017(6)
C13 0.0548(12) 0.0269(9) 0.0242(9) -0.0059(7) -0.0253(8) -0.0044(8)
C14 0.0245(9) 0.0426(11) 0.0412(11) -0.0272(9) -0.0106(8) 0.0004(8)
C15 0.0322(9) 0.0258(8) 0.0259(8) -0.0137(7) -0.0136(7) 0.0062(7)
C16 0.0376(9) 0.0196(8) 0.0186(8) -0.0018(6) -0.0137(7) -0.0021(7)
C17 0.0149(7) 0.0160(7) 0.0161(7) -0.0044(6) -0.0038(6) -0.0010(6)
C18 0.0183(7) 0.0118(7) 0.0194(7) -0.0045(6) -0.0065(6) 0.0020(6)
C19 0.0146(7) 0.0176(7) 0.0170(7) -0.0062(6) -0.0033(6) -0.0005(6)
C20 0.0217(8) 0.0137(7) 0.0260(8) -0.0046(6) -0.0064(6) 0.0000(6)
C21 0.0322(9) 0.0250(8) 0.0235(8) -0.0144(7) -0.0117(7) 0.0064(7)
C22 0.0175(7) 0.0187(7) 0.0161(7) -0.0060(6) -0.0044(6) -0.0020(6)
C23 0.0150(7) 0.0171(7) 0.0159(7) -0.0029(6) -0.0041(6) -0.0026(6)
C24 0.0190(7) 0.0201(7) 0.0142(7) -0.0030(6) -0.0066(6) -0.0006(6)
C25 0.0197(7) 0.0234(8) 0.0170(7) -0.0069(6) -0.0058(6) 0.0019(6)
C26 0.0178(7) 0.0205(8) 0.0185(7) -0.0043(6) -0.0058(6) 0.0019(6)
C27 0.0158(7) 0.0212(7) 0.0129(7) -0.0022(6) -0.0050(6) -0.0034(6)
C28 0.0173(7) 0.0193(7) 0.0131(7) -0.0039(6) -0.0034(6) -0.0033(6)
C29 0.0301(9) 0.0312(9) 0.0175(8) -0.0113(7) -0.0108(7) 0.0127(7)
C30 0.0394(10) 0.0432(11) 0.0195(8) -0.0106(8) -0.0053(8) 0.0125(9)
C31 0.0416(10) 0.0318(9) 0.0270(9) -0.0165(8) -0.0192(8) 0.0116(8)
C32 0.0384(10) 0.0464(11) 0.0270(9) -0.0209(8) -0.0147(8) 0.0229(9)
C33 0.0194(7) 0.0232(8) 0.0142(7) -0.0038(6) -0.0072(6) -0.0018(6)
C34 0.0416(11) 0.0569(13) 0.0340(10) -0.0262(10) -0.0246(9) 0.0165(9)
C35 0.0203(8) 0.0453(11) 0.0222(8) -0.0023(8) -0.0095(7) -0.0018(7)
C36 0.0470(11) 0.0354(10) 0.0297(10) 0.0073(8) -0.0231(9) -0.0143(9)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 H1 0.944(5) . ?
O1 C3 1.3737(17) . ?
O2 H2 0.945(5) . ?
O2 C24 1.3719(17) . ?
N1 N2 1.3766(17) . ?
N1 C1 1.2912(18) . ?
N2 C16 1.4590(18) . ?
N2 C17 1.3826(18) . ?
N3 C17 1.3518(18) . ?
N3 C20 1.3258(19) . ?
N4 C19 1.3504(18) . ?
N4 C20 1.3306(19) . ?
N5 N6 1.3711(16) . ?
N5 C19 1.3877(18) . ?
N5 C21 1.4551(18) . ?
N6 C22 1.2926(18) . ?
C1 H1A 0.9500 . ?
C1 C2 1.459(2) . ?
C2 C3 1.409(2) . ?
C2 C7 1.401(2) . ?
C3 C4 1.413(2) . ?
C4 C5 1.393(2) . ?
C4 C8 1.543(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.409(2) . ?
C6 C7 1.383(2) . ?
C6 C12 1.5364(19) . ?
C7 H7 0.9500 . ?
C8 C9 1.545(2) . ?
C8 C10 1.547(2) . ?
C8 C11 1.534(2) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.532(2) . ?
C12 C14 1.537(2) . ?
C12 C15 1.539(2) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.3968(19) . ?
C18 H18 0.9500 . ?
C18 C19 1.393(2) . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22 0.9500 . ?
C22 C23 1.461(2) . ?
C23 C24 1.407(2) . ?
C23 C28 1.4070(19) . ?
C24 C25 1.412(2) . ?
C25 C26 1.399(2) . ?
C25 C29 1.540(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.402(2) . ?
C27 C28 1.387(2) . ?
C27 C33 1.5398(19) . ?
C28 H28 0.9500 . ?
C29 C30 1.545(2) . ?
C29 C31 1.540(2) . ?
C29 C32 1.544(2) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.533(2) . ?
C33 C35 1.531(2) . ?
C33 C36 1.533(2) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 O1 H1 106.3(11) . . ?
C24 O2 H2 106.2(11) . . ?
C1 N1 N2 119.31(12) . . ?
N1 N2 C16 120.31(12) . . ?
N1 N2 C17 116.35(11) . . ?
C17 N2 C16 121.45(12) . . ?
C20 N3 C17 115.20(13) . . ?
C20 N4 C19 114.87(12) . . ?
N6 N5 C19 116.24(11) . . ?
N6 N5 C21 120.75(12) . . ?
C19 N5 C21 121.52(12) . . ?
C22 N6 N5 120.42(12) . . ?
N1 C1 H1A 119.0 . . ?
N1 C1 C2 122.10(13) . . ?
C2 C1 H1A 119.0 . . ?
C3 C2 C1 123.43(13) . . ?
C7 C2 C1 117.12(13) . . ?
C7 C2 C3 119.41(13) . . ?
O1 C3 C2 119.65(13) . . ?
O1 C3 C4 119.51(12) . . ?
C2 C3 C4 120.83(13) . . ?
C3 C4 C8 121.68(12) . . ?
C5 C4 C3 116.64(13) . . ?
C5 C4 C8 121.67(13) . . ?
C4 C5 H5 117.8 . . ?
C4 C5 C6 124.39(14) . . ?
C6 C5 H5 117.8 . . ?
C5 C6 C12 120.34(13) . . ?
C7 C6 C5 116.86(13) . . ?
C7 C6 C12 122.76(13) . . ?
C2 C7 H7 119.1 . . ?
C6 C7 C2 121.85(14) . . ?
C6 C7 H7 119.1 . . ?
C4 C8 C9 110.60(12) . . ?
C4 C8 C10 109.69(12) . . ?
C9 C8 C10 110.43(12) . . ?
C11 C8 C4 112.05(12) . . ?
C11 C8 C9 106.80(13) . . ?
C11 C8 C10 107.18(12) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C6 C12 C14 109.29(12) . . ?
C6 C12 C15 110.19(12) . . ?
C13 C12 C6 111.90(13) . . ?
C13 C12 C14 108.55(13) . . ?
C13 C12 C15 107.84(13) . . ?
C14 C12 C15 109.02(13) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N2 C16 H16A 109.5 . . ?
N2 C16 H16B 109.5 . . ?
N2 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 C17 C18 122.56(13) . . ?
N3 C17 N2 115.14(12) . . ?
N3 C17 C18 122.29(13) . . ?
C17 C18 H18 122.0 . . ?
C19 C18 C17 116.04(13) . . ?
C19 C18 H18 122.0 . . ?
N4 C19 N5 115.41(12) . . ?
N4 C19 C18 122.71(13) . . ?
N5 C19 C18 121.89(13) . . ?
N3 C20 N4 128.64(14) . . ?
N3 C20 H20 115.7 . . ?
N4 C20 H20 115.7 . . ?
N5 C21 H21A 109.5 . . ?
N5 C21 H21B 109.5 . . ?
N5 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N6 C22 H22 119.2 . . ?
N6 C22 C23 121.66(13) . . ?
C23 C22 H22 119.2 . . ?
C24 C23 C22 122.61(13) . . ?
C24 C23 C28 119.44(13) . . ?
C28 C23 C22 117.79(13) . . ?
O2 C24 C23 119.77(13) . . ?
O2 C24 C25 119.65(13) . . ?
C23 C24 C25 120.57(13) . . ?
C24 C25 C29 120.88(13) . . ?
C26 C25 C24 117.06(14) . . ?
C26 C25 C29 122.05(13) . . ?
C25 C26 H26 117.9 . . ?
C25 C26 C27 124.15(14) . . ?
C27 C26 H26 117.9 . . ?
C26 C27 C33 119.68(13) . . ?
C28 C27 C26 116.93(13) . . ?
C28 C27 C33 123.31(13) . . ?
C23 C28 H28 119.1 . . ?
C27 C28 C23 121.82(14) . . ?
C27 C28 H28 119.1 . . ?
C25 C29 C30 110.15(13) . . ?
C25 C29 C32 111.76(12) . . ?
C31 C29 C25 109.73(13) . . ?
C31 C29 C30 110.57(13) . . ?
C31 C29 C32 107.77(14) . . ?
C32 C29 C30 106.79(14) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C27 111.66(13) . . ?
C34 C33 C36 107.86(14) . . ?
C35 C33 C27 109.63(12) . . ?
C35 C33 C34 108.26(14) . . ?
C35 C33 C36 109.43(14) . . ?
C36 C33 C27 109.95(12) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 N1 0.944(5) 1.782(10) 2.6470(16) 150.9(16) .
O2 H2 N6 0.945(5) 1.745(10) 2.6132(16) 151.2(16) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 C17 N2 N1 161.35(12) . . . . ?
N4 C19 N5 N6 154.42(12) . . . . ?
C1 N1 N2 C16 -4.5(2) . . . . ?
C1 N1 N2 C17 -169.06(13) . . . . ?
C2 C1 N1 N2 175.02(13) . . . . ?
C3 C2 C1 N1 -0.2(2) . . . . ?
C3 C4 C8 C9 -58.06(18) . . . . ?
C3 C4 C8 C10 63.99(17) . . . . ?
C3 C4 C8 C11 -177.10(13) . . . . ?
C5 C4 C8 C9 122.26(15) . . . . ?
C5 C4 C8 C10 -115.70(15) . . . . ?
C5 C4 C8 C11 3.2(2) . . . . ?
C5 C6 C12 C13 174.35(14) . . . . ?
C5 C6 C12 C14 -65.39(18) . . . . ?
C5 C6 C12 C15 54.38(18) . . . . ?
C7 C2 C1 N1 -177.70(14) . . . . ?
C7 C6 C12 C13 -7.9(2) . . . . ?
C7 C6 C12 C14 112.40(16) . . . . ?
C7 C6 C12 C15 -127.83(15) . . . . ?
C16 N2 C17 N3 -3.0(2) . . . . ?
C18 C17 N2 N1 -17.6(2) . . . . ?
C18 C17 N2 C16 178.01(14) . . . . ?
C18 C19 N5 N6 -25.8(2) . . . . ?
C18 C19 N5 C21 168.04(14) . . . . ?
C19 N5 N6 C22 -170.12(13) . . . . ?
C21 N5 N6 C22 -3.8(2) . . . . ?
C21 N5 C19 N4 -11.8(2) . . . . ?
C23 C22 N6 N5 173.89(13) . . . . ?
C24 C23 C22 N6 -1.3(2) . . . . ?
C24 C25 C29 C30 -57.82(19) . . . . ?
C24 C25 C29 C31 64.13(18) . . . . ?
C24 C25 C29 C32 -176.37(15) . . . . ?
C26 C25 C29 C30 121.37(16) . . . . ?
C26 C25 C29 C31 -116.67(16) . . . . ?
C26 C25 C29 C32 2.8(2) . . . . ?
C26 C27 C33 C34 -175.71(14) . . . . ?
C26 C27 C33 C35 -55.74(18) . . . . ?
C26 C27 C33 C36 64.61(18) . . . . ?
C28 C23 C22 N6 -176.59(13) . . . . ?
C28 C27 C33 C34 0.8(2) . . . . ?
C28 C27 C33 C35 120.81(16) . . . . ?
C28 C27 C33 C36 -118.84(17) . . . . ?
_shelx_SHELXL_version_number 2014/7
_iucr_refine_instructions_details
;
TITL 16srv303
CELL 0.71073 12.1186 12.2241 12.9851 72.172 77.714 88.934
ZERR 2 0.0012 0.001 0.0011 0.003 0.003 0.003
LATT 1
SFAC C H N O
UNIT 72 104 12 4
DFIX 0.95 0.005 O2 H2 O1 H1
L.S. 9
PLAN 5
SIZE 0.05 0.11 0.32
TEMP -153.15
CONF C3 C2 C1 N1
CONF C7 C2 C1 N1
CONF C2 C1 N1 N2
CONF C1 N1 N2 C16
CONF C1 N1 N2 C17
CONF N3 C17 N2 N1
CONF C18 C17 N2 N1
CONF C16 N2 C17 N3
CONF C18 C17 N2 C16
CONF N4 C19 N5 N6
CONF C18 C19 N5 N6
CONF C21 N5 C19 N4
CONF C18 C19 N5 C21
CONF C19 N5 N6 C22
CONF C21 N5 N6 C22
CONF C23 C22 N6 N5
CONF C24 C23 C22 N6
CONF C28 C23 C22 N6
CONF C3 C4 C8 C9
CONF C5 C4 C8 C9
CONF C3 C4 C8 C10
CONF C5 C4 C8 C10
CONF C3 C4 C8 C11
CONF C5 C4 C8 C11
CONF C5 C6 C12 C13
CONF C5 C6 C12 C14
CONF C5 C6 C12 C15
CONF C7 C6 C12 C13
CONF C7 C6 C12 C14
CONF C7 C6 C12 C15
CONF C24 C25 C29 C30
CONF C26 C25 C29 C30
CONF C24 C25 C29 C31
CONF C26 C25 C29 C31
CONF C24 C25 C29 C32
CONF C26 C25 C29 C32
CONF C26 C27 C33 C34
CONF C28 C27 C33 C34
CONF C26 C27 C33 C35
CONF C28 C27 C33 C35
CONF C26 C27 C33 C36
CONF C28 C27 C33 C36
HTAB O1 N1
HTAB O2 N6
BOND $h
fmap 2
acta
OMIT -2 58
OMIT 0 1 1
WGHT 0.06 0.47
FVAR 0.26656
REM
REM
REM
O1 4 0.62599 0.12922 0.75468 11.00000 0.03386 0.01670 0.02016 =
-0.00669 -0.01524 -0.00035
H1 2 0.60889 0.05117 0.79664 11.00000 -1.50000
O2 4 0.32316 0.04765 0.69711 11.00000 0.03004 0.02624 0.01958 =
-0.01047 -0.01515 0.01135
H2 2 0.36984 -0.01320 0.68858 11.00000 -1.50000
N1 3 0.60648 -0.06622 0.91915 11.00000 0.01947 0.01405 0.01742 =
-0.00465 -0.00640 0.00172
N2 3 0.58380 -0.18307 0.96522 11.00000 0.02553 0.01342 0.01721 =
-0.00287 -0.00948 0.00026
N3 3 0.57050 -0.35606 0.93052 11.00000 0.02263 0.01363 0.02028 =
-0.00234 -0.00661 -0.00006
N4 3 0.53302 -0.36699 0.76012 11.00000 0.02039 0.01442 0.02354 =
-0.00691 -0.00637 0.00127
N5 3 0.48169 -0.20877 0.63083 11.00000 0.02304 0.01668 0.01901 =
-0.00874 -0.00963 0.00468
N6 3 0.42012 -0.11219 0.61953 11.00000 0.01623 0.01505 0.01824 =
-0.00466 -0.00468 0.00045
C1 1 0.64696 -0.01015 0.97360 11.00000 0.02161 0.01909 0.01637 =
-0.00574 -0.00734 0.00317
AFIX 43
H1a 2 0.65464 -0.04960 1.04691 11.00000 -1.20000
AFIX 0
C2 1 0.68128 0.11184 0.92611 11.00000 0.01811 0.01675 0.01854 =
-0.00829 -0.00712 0.00312
C3 1 0.67365 0.17809 0.81817 11.00000 0.02032 0.01903 0.01727 =
-0.00992 -0.00863 0.00372
C4 1 0.71439 0.29429 0.77434 11.00000 0.01932 0.01862 0.01574 =
-0.00609 -0.00710 0.00439
C5 1 0.76018 0.33907 0.84354 11.00000 0.02137 0.01584 0.01928 =
-0.00680 -0.00740 0.00143
AFIX 43
H5 2 0.78820 0.41701 0.81537 11.00000 -1.20000
AFIX 0
C6 1 0.76772 0.27656 0.95252 11.00000 0.01794 0.02027 0.01813 =
-0.00886 -0.00772 0.00221
C7 1 0.72794 0.16276 0.99132 11.00000 0.02190 0.01959 0.01636 =
-0.00639 -0.00859 0.00333
AFIX 43
H7 2 0.73240 0.11787 1.06421 11.00000 -1.20000
AFIX 0
C8 1 0.70794 0.36802 0.65597 11.00000 0.02364 0.01866 0.01528 =
-0.00576 -0.00799 0.00126
C9 1 0.77126 0.31227 0.56979 11.00000 0.02600 0.03036 0.01940 =
-0.00989 -0.00760 0.00271
AFIX 137
H9a 2 0.85105 0.30667 0.57401 11.00000 -1.50000
H9b 2 0.76544 0.35966 0.49531 11.00000 -1.50000
H9c 2 0.73745 0.23512 0.58540 11.00000 -1.50000
AFIX 0
C10 1 0.58274 0.38242 0.64758 11.00000 0.02690 0.02170 0.01780 =
-0.00649 -0.01003 0.00360
AFIX 137
H10a 2 0.54515 0.30651 0.66568 11.00000 -1.50000
H10b 2 0.57896 0.42810 0.57196 11.00000 -1.50000
H10c 2 0.54481 0.42175 0.69976 11.00000 -1.50000
AFIX 0
C11 1 0.76280 0.48913 0.62514 11.00000 0.03273 0.02312 0.01762 =
-0.00262 -0.00887 -0.00396
AFIX 137
H11a 2 0.72323 0.52871 0.67643 11.00000 -1.50000
H11b 2 0.75780 0.53268 0.54928 11.00000 -1.50000
H11c 2 0.84240 0.48335 0.63001 11.00000 -1.50000
AFIX 0
C12 1 0.82188 0.33337 1.02140 11.00000 0.02217 0.01926 0.01771 =
-0.00775 -0.01113 0.00165
C13 1 0.81104 0.25484 1.14075 11.00000 0.05473 0.02691 0.02419 =
-0.00587 -0.02530 -0.00438
AFIX 137
H13a 2 0.73107 0.23365 1.17520 11.00000 -1.50000
H13b 2 0.84289 0.29548 1.18297 11.00000 -1.50000
H13c 2 0.85224 0.18515 1.14042 11.00000 -1.50000
AFIX 0
C14 1 0.94807 0.36146 0.96759 11.00000 0.02452 0.04260 0.04119 =
-0.02721 -0.01062 0.00045
AFIX 137
H14a 2 0.98509 0.29066 0.96286 11.00000 -1.50000
H14b 2 0.98337 0.39550 1.01264 11.00000 -1.50000
H14c 2 0.95620 0.41612 0.89297 11.00000 -1.50000
AFIX 0
C15 1 0.76411 0.44545 1.02598 11.00000 0.03216 0.02575 0.02592 =
-0.01366 -0.01360 0.00618
AFIX 137
H15a 2 0.77351 0.49902 0.95071 11.00000 -1.50000
H15b 2 0.79866 0.48040 1.07086 11.00000 -1.50000
H15c 2 0.68336 0.42834 1.05927 11.00000 -1.50000
AFIX 0
C16 1 0.61295 -0.24424 1.07068 11.00000 0.03760 0.01963 0.01860 =
-0.00182 -0.01370 -0.00209
AFIX 137
H16a 2 0.69411 -0.23217 1.06458 11.00000 -1.50000
H16b 2 0.59421 -0.32665 1.08941 11.00000 -1.50000
H16c 2 0.57012 -0.21500 1.12891 11.00000 -1.50000
AFIX 0
C17 1 0.55966 -0.24104 0.89579 11.00000 0.01489 0.01595 0.01612 =
-0.00438 -0.00378 -0.00101
C18 1 0.52820 -0.18485 0.79602 11.00000 0.01835 0.01177 0.01940 =
-0.00449 -0.00655 0.00201
AFIX 43
H18 2 0.51668 -0.10466 0.77387 11.00000 -1.20000
AFIX 0
C19 1 0.51472 -0.25338 0.73091 11.00000 0.01460 0.01760 0.01695 =
-0.00623 -0.00328 -0.00045
C20 1 0.55747 -0.41034 0.85944 11.00000 0.02165 0.01370 0.02599 =
-0.00460 -0.00642 -0.00000
AFIX 43
H20 2 0.56686 -0.49091 0.88250 11.00000 -1.20000
AFIX 0
C21 1 0.48856 -0.27446 0.55345 11.00000 0.03216 0.02504 0.02352 =
-0.01440 -0.01166 0.00638
AFIX 137
H21a 2 0.41260 -0.30315 0.55642 11.00000 -1.50000
H21b 2 0.53654 -0.33958 0.57363 11.00000 -1.50000
H21c 2 0.52116 -0.22488 0.47819 11.00000 -1.50000
AFIX 0
C22 1 0.37222 -0.07432 0.53627 11.00000 0.01749 0.01871 0.01606 =
-0.00595 -0.00439 -0.00204
AFIX 43
H22 2 0.38622 -0.10963 0.47926 11.00000 -1.20000
AFIX 0
C23 1 0.29710 0.02141 0.52762 11.00000 0.01503 0.01712 0.01589 =
-0.00294 -0.00415 -0.00255
C24 1 0.27038 0.07672 0.60955 11.00000 0.01902 0.02010 0.01421 =
-0.00299 -0.00657 -0.00057
C25 1 0.18884 0.16116 0.60303 11.00000 0.01973 0.02343 0.01697 =
-0.00694 -0.00584 0.00193
C26 1 0.13920 0.18851 0.51096 11.00000 0.01779 0.02050 0.01853 =
-0.00430 -0.00583 0.00193
AFIX 43
H26 2 0.08513 0.24613 0.50492 11.00000 -1.20000
AFIX 0
C27 1 0.16419 0.13625 0.42702 11.00000 0.01578 0.02116 0.01288 =
-0.00220 -0.00504 -0.00338
C28 1 0.24379 0.05284 0.43724 11.00000 0.01733 0.01928 0.01310 =
-0.00387 -0.00344 -0.00327
AFIX 43
H28 2 0.26286 0.01590 0.38167 11.00000 -1.20000
AFIX 0
C29 1 0.15579 0.21873 0.69469 11.00000 0.03012 0.03117 0.01746 =
-0.01128 -0.01077 0.01265
C30 1 0.11151 0.12671 0.80789 11.00000 0.03941 0.04320 0.01951 =
-0.01057 -0.00526 0.01252
AFIX 137
H30a 2 0.04458 0.08513 0.80471 11.00000 -1.50000
H30b 2 0.09135 0.16417 0.86566 11.00000 -1.50000
H30c 2 0.17051 0.07247 0.82509 11.00000 -1.50000
AFIX 0
C31 1 0.25863 0.28824 0.69857 11.00000 0.04153 0.03177 0.02695 =
-0.01647 -0.01922 0.01156
AFIX 137
H31a 2 0.31933 0.23633 0.71601 11.00000 -1.50000
H31b 2 0.23678 0.32621 0.75579 11.00000 -1.50000
H31c 2 0.28526 0.34643 0.62638 11.00000 -1.50000
AFIX 0
C32 1 0.06004 0.30228 0.67383 11.00000 0.03837 0.04642 0.02696 =
-0.02092 -0.01474 0.02288
AFIX 137
H32a 2 0.08435 0.36174 0.60203 11.00000 -1.50000
H32b 2 0.04249 0.33852 0.73271 11.00000 -1.50000
H32c 2 -0.00751 0.25964 0.67352 11.00000 -1.50000
AFIX 0
C33 1 0.09922 0.16809 0.33293 11.00000 0.01941 0.02316 0.01421 =
-0.00378 -0.00721 -0.00183
C34 1 0.13246 0.09537 0.25467 11.00000 0.04158 0.05688 0.03404 =
-0.02615 -0.02457 0.01645
AFIX 137
H34a 2 0.21391 0.10653 0.22293 11.00000 -1.50000
H34b 2 0.09103 0.11915 0.19494 11.00000 -1.50000
H34c 2 0.11367 0.01395 0.29613 11.00000 -1.50000
AFIX 0
C35 1 -0.02803 0.14788 0.38213 11.00000 0.02032 0.04527 0.02215 =
-0.00233 -0.00952 -0.00183
AFIX 137
H35a 2 -0.04490 0.06666 0.42543 11.00000 -1.50000
H35b 2 -0.06917 0.16815 0.32209 11.00000 -1.50000
H35c 2 -0.05143 0.19589 0.43036 11.00000 -1.50000
AFIX 0
C36 1 0.12537 0.29491 0.26416 11.00000 0.04694 0.03542 0.02969 =
0.00727 -0.02305 -0.01429
AFIX 137
H36a 2 0.10009 0.34361 0.31135 11.00000 -1.50000
H36b 2 0.08572 0.31386 0.20303 11.00000 -1.50000
H36c 2 0.20701 0.30831 0.23416 11.00000 -1.50000
AFIX 0
HKLF 4
END
;
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_H2L5_16srv249
_database_code_depnum_ccdc_archive 'CCDC 2006845'
loop_
_audit_author_name
_audit_author_address
'Dmitry Yufit'
;Durham University
United Kingdom
;
_audit_update_record
;
2020-06-01 deposited with the CCDC. 2020-07-10 downloaded from the CCDC.
;
_audit_creation_date 2016-06-30
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C20 H20 N6 O2'
_chemical_formula_sum 'C20 H20 N6 O2'
_chemical_formula_weight 376.42
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_H-M_alt 'I 1 2/c 1'
_space_group_name_Hall '-I 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, -y+1/2, z'
_cell_length_a 15.5025(12)
_cell_length_b 10.4734(8)
_cell_length_c 11.3532(9)
_cell_angle_alpha 90
_cell_angle_beta 93.231(7)
_cell_angle_gamma 90
_cell_volume 1840.4(3)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 1607
_cell_measurement_temperature 120.0
_cell_measurement_theta_max 31.4460
_cell_measurement_theta_min 2.3410
_shelx_estimated_absorpt_T_max 0.994
_shelx_estimated_absorpt_T_min 0.971
_exptl_absorpt_coefficient_mu 0.092
_exptl_absorpt_correction_T_max 0.754
_exptl_absorpt_correction_T_min 0.274
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb 9 2015,16:26:32)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'dull yellow'
_exptl_crystal_colour_lustre dull
_exptl_crystal_colour_modifier .
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.359
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description irregular
_exptl_crystal_F_000 792
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.06
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.1019
_diffrn_reflns_av_unetI/netI 0.0686
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 15142
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.993
_diffrn_reflns_theta_min 2.348
_diffrn_ambient_temperature 120.0
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 8.0756
_diffrn_detector_type Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -32.00 47.00 1.0000 17.5000
omega____ theta____ kappa____ phi______ frames
- 28.9587 -57.0000 120.0000 79
#__ type_ start__ end____ width___ exp.time_
2 omega 14.00 71.00 1.0000 17.5000
omega____ theta____ kappa____ phi______ frames
- 28.9587 -100.0000 -120.0000 57
#__ type_ start__ end____ width___ exp.time_
3 omega 40.00 67.00 1.0000 17.5000
omega____ theta____ kappa____ phi______ frames
- 28.9587 -100.0000 0.0000 27
#__ type_ start__ end____ width___ exp.time_
4 omega -4.00 71.00 1.0000 17.5000
omega____ theta____ kappa____ phi______ frames
- 28.9587 -100.0000 90.0000 75
#__ type_ start__ end____ width___ exp.time_
5 omega 11.00 98.00 1.0000 17.5000
omega____ theta____ kappa____ phi______ frames
- 28.9587 57.0000 0.0000 87
#__ type_ start__ end____ width___ exp.time_
6 omega -43.00 69.00 1.0000 17.5000
omega____ theta____ kappa____ phi______ frames
- 28.9587 -19.0000 -180.0000 112
#__ type_ start__ end____ width___ exp.time_
7 omega -1.00 99.00 1.0000 17.5000
omega____ theta____ kappa____ phi______ frames
- 28.9587 77.0000 90.0000 100
#__ type_ start__ end____ width___ exp.time_
8 omega 9.00 98.00 1.0000 17.5000
omega____ theta____ kappa____ phi______ frames
- 28.9587 57.0000 -60.0000 89
#__ type_ start__ end____ width___ exp.time_
9 omega 35.00 88.00 1.0000 17.5000
omega____ theta____ kappa____ phi______ frames
- 28.9587 178.0000 90.0000 53
#__ type_ start__ end____ width___ exp.time_
10 omega 9.00 98.00 1.0000 17.5000
omega____ theta____ kappa____ phi______ frames
- 28.9587 57.0000 -150.0000 89
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Xcalibur, Sapphire3'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 -0.0189028000
_diffrn_orient_matrix_UB_12 0.0597339000
_diffrn_orient_matrix_UB_13 0.0127529000
_diffrn_orient_matrix_UB_21 -0.0289812000
_diffrn_orient_matrix_UB_22 -0.0066404000
_diffrn_orient_matrix_UB_23 -0.0502631000
_diffrn_orient_matrix_UB_31 -0.0300277000
_diffrn_orient_matrix_UB_32 -0.0312226000
_diffrn_orient_matrix_UB_33 0.0350462000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 1438
_reflns_number_total 2446
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 30.44
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb 9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb 9 2015,16:26:32)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb 9 2015,16:26:32)
;
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max 0.260
_refine_diff_density_min -0.224
_refine_diff_density_rms 0.052
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.020
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 133
_refine_ls_number_reflns 2446
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1101
_refine_ls_R_factor_gt 0.0565
_refine_ls_restrained_S_all 1.020
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+0.1500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1088
_refine_ls_wR_factor_ref 0.1299
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11)
2.b Idealised Me refined as rotating group:
C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary iterative
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.40564(9) -0.11401(14) 0.30705(12) 0.0400(4) Uani 1 1 d . . . . .
N1 N 0.46655(9) 0.41420(14) 0.34259(13) 0.0249(4) Uani 1 1 d . . . . .
N2 N 0.43000(9) 0.22788(13) 0.43630(13) 0.0230(4) Uani 1 1 d . . . . .
N3 N 0.41328(9) 0.10016(13) 0.42730(12) 0.0212(3) Uani 1 1 d . . . . .
C1 C 0.46638(11) 0.28536(16) 0.34119(15) 0.0202(4) Uani 1 1 d . . . . .
C2 C 0.5000 0.2162(2) 0.2500 0.0210(5) Uani 1 2 d S T P . .
H2 H 0.5000 0.1254 0.2500 0.025 Uiso 1 2 calc RS T P . .
C3 C 0.5000 0.4686(2) 0.2500 0.0254(6) Uani 1 2 d S T P . .
H3 H 0.5000 0.5593 0.2500 0.031 Uiso 1 2 calc RS T P . .
C4 C 0.41273(12) 0.29810(18) 0.54299(15) 0.0270(4) Uani 1 1 d . . . . .
H4A H 0.3504 0.2983 0.5537 0.041 Uiso 1 1 calc GR . . . .
H4B H 0.4332 0.3862 0.5361 0.041 Uiso 1 1 calc GR . . . .
H4C H 0.4429 0.2571 0.6111 0.041 Uiso 1 1 calc GR . . . .
C5 C 0.37973(10) 0.04139(16) 0.51346(15) 0.0219(4) Uani 1 1 d . . . . .
H5 H 0.3688 0.0869 0.5835 0.026 Uiso 1 1 calc R . . . .
C6 C 0.35831(10) -0.09370(17) 0.50495(15) 0.0216(4) Uani 1 1 d . . . . .
C7 C 0.37220(11) -0.16707(17) 0.40409(17) 0.0265(4) Uani 1 1 d . . . . .
C8 C 0.35332(12) -0.29651(19) 0.40225(19) 0.0343(5) Uani 1 1 d . . . . .
H8 H 0.3630 -0.3457 0.3340 0.041 Uiso 1 1 calc R . . . .
C9 C 0.32059(11) -0.35367(18) 0.49920(19) 0.0335(5) Uani 1 1 d . . . . .
H9 H 0.3092 -0.4428 0.4980 0.040 Uiso 1 1 calc R . . . .
C10 C 0.30404(12) -0.2832(2) 0.59843(18) 0.0325(5) Uani 1 1 d . . . . .
H10 H 0.2802 -0.3230 0.6644 0.039 Uiso 1 1 calc R . . . .
C11 C 0.32259(12) -0.15427(18) 0.60028(16) 0.0288(5) Uani 1 1 d . . . . .
H11 H 0.3108 -0.1056 0.6681 0.035 Uiso 1 1 calc R . . . .
H1 H 0.4177(17) -0.023(3) 0.327(2) 0.085(9) Uiso 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0587(10) 0.0283(8) 0.0350(8) -0.0086(6) 0.0225(7) -0.0123(7)
N1 0.0331(8) 0.0166(8) 0.0248(8) 0.0003(6) 0.0007(7) 0.0014(7)
N2 0.0320(9) 0.0147(8) 0.0227(8) -0.0022(6) 0.0052(7) -0.0008(6)
N3 0.0251(8) 0.0141(8) 0.0243(8) -0.0012(6) 0.0025(6) 0.0003(6)
C1 0.0220(9) 0.0182(9) 0.0202(9) 0.0008(7) -0.0016(7) -0.0008(7)
C2 0.0261(13) 0.0129(12) 0.0242(13) 0.000 0.0036(11) 0.000
C3 0.0383(15) 0.0114(12) 0.0266(14) 0.000 0.0019(12) 0.000
C4 0.0361(11) 0.0206(10) 0.0248(10) -0.0033(8) 0.0058(8) 0.0000(8)
C5 0.0239(9) 0.0212(10) 0.0208(9) -0.0013(7) 0.0020(7) 0.0002(7)
C6 0.0195(9) 0.0216(10) 0.0236(9) 0.0017(8) 0.0016(7) 0.0007(7)
C7 0.0258(9) 0.0218(10) 0.0325(11) 0.0004(8) 0.0077(8) 0.0010(8)
C8 0.0307(11) 0.0233(11) 0.0499(13) -0.0075(9) 0.0118(10) 0.0002(9)
C9 0.0234(10) 0.0183(10) 0.0585(14) 0.0070(9) 0.0003(9) -0.0013(8)
C10 0.0287(10) 0.0321(12) 0.0362(12) 0.0129(9) -0.0025(9) -0.0066(9)
C11 0.0293(10) 0.0277(11) 0.0294(11) 0.0040(8) 0.0009(8) -0.0049(8)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C7 1.362(2) . ?
O1 H1 0.99(3) . ?
N1 C1 1.349(2) . ?
N1 C3 1.3265(17) . ?
N2 N3 1.3652(19) . ?
N2 C1 1.384(2) . ?
N2 C4 1.455(2) . ?
N3 C5 1.290(2) . ?
C1 C2 1.389(2) . ?
C2 C1 1.389(2) 2_655 ?
C2 H2 0.9500 . ?
C3 N1 1.3265(17) 2_655 ?
C3 H3 0.9500 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5 0.9500 . ?
C5 C6 1.455(2) . ?
C6 C7 1.406(2) . ?
C6 C11 1.396(2) . ?
C7 C8 1.387(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.375(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.383(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.381(3) . ?
C11 H11 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 O1 H1 106.6(14) . . ?
C3 N1 C1 114.86(16) . . ?
N3 N2 C1 116.86(13) . . ?
N3 N2 C4 120.96(14) . . ?
C1 N2 C4 122.14(14) . . ?
C5 N3 N2 119.59(14) . . ?
N1 C1 N2 115.24(15) . . ?
N1 C1 C2 122.00(16) . . ?
N2 C1 C2 122.76(16) . . ?
C1 C2 C1 117.1(2) . 2_655 ?
C1 C2 H2 121.5 . . ?
C1 C2 H2 121.5 2_655 . ?
N1 C3 N1 129.2(2) 2_655 . ?
N1 C3 H3 115.4 2_655 . ?
N1 C3 H3 115.4 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 H5 119.5 . . ?
N3 C5 C6 120.92(16) . . ?
C6 C5 H5 119.5 . . ?
C7 C6 C5 122.73(15) . . ?
C11 C6 C5 119.30(16) . . ?
C11 C6 C7 117.97(17) . . ?
O1 C7 C6 121.24(16) . . ?
O1 C7 C8 118.44(17) . . ?
C8 C7 C6 120.31(17) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 C7 120.05(19) . . ?
C9 C8 H8 120.0 . . ?
C8 C9 H9 119.5 . . ?
C8 C9 C10 120.91(18) . . ?
C10 C9 H9 119.5 . . ?
C9 C10 H10 120.5 . . ?
C11 C10 C9 119.10(17) . . ?
C11 C10 H10 120.5 . . ?
C6 C11 H11 119.2 . . ?
C10 C11 C6 121.62(18) . . ?
C10 C11 H11 119.2 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 N3 0.99(3) 1.73(3) 2.6251(19) 148(2) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 N2 N3 167.62(14) . . . . ?
C1 N2 N3 C5 179.71(15) . . . . ?
C2 C1 N2 N3 -12.0(2) . . . . ?
C2 C1 N2 C4 165.98(14) . . . . ?
C4 N2 N3 C5 1.7(2) . . . . ?
C4 N2 C1 N1 -14.4(2) . . . . ?
C6 C5 N3 N2 177.81(15) . . . . ?
C7 C6 C5 N3 -0.3(3) . . . . ?
C11 C6 C5 N3 179.59(16) . . . . ?
_shelx_SHELXL_version_number 2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1 -1 5 0.0116 -0.9998 -1.0001 5.0002 0.0229 -0.2157 0.2365
-2 0 -5 0.0259 -2.0003 0.0002 -5.0002 -0.0259 0.3093 -0.1152
5 2 0 0.0489 5.0001 2.0000 0.0001 0.0249 -0.1582 -0.2126
-5 -2 0 0.0489 -5.0001 -2.0000 -0.0001 -0.0249 0.1582 0.2126
-5 0 2 0.0521 -5.0000 -0.0000 2.0000 0.1200 0.0444 0.2202
5 0 -2 0.0521 5.0000 0.0000 -2.0000 -0.1200 -0.0444 -0.2202
5 4 -4 0.0604 4.9999 4.0001 -4.0001 0.0934 0.0296 -0.4152
-5 -4 4 0.0604 -4.9999 -4.0001 4.0001 -0.0934 -0.0296 0.4152
_olex2_submission_special_instructions 'No special instructions were received'
_iucr_refine_instructions_details
;
TITL 16srv249 in I2/a
CELL 0.71073 15.502526 10.473413 11.353242 90 93.231 90
ZERR 4 0.001162 0.000846 0.000913 0 0.0069 0
LATT 2
SYMM -X,+Y,0.5-Z
SFAC C H N O
UNIT 80 80 24 8
L.S. 9
PLAN 5
SIZE 0.06 0.1 0.32
TEMP -153.15
HTAB O1 N3
CONF C7 C6 C5 N3
CONF C11 C6 C5 N3
CONF C6 C5 N3 N2
CONF C1 N2 N3 C5
CONF C4 N2 N3 C5
CONF N1 C1 N2 N3
CONF C2 C1 N2 N3
CONF C4 N2 C1 N1
CONF C2 C1 N2 C4
BOND $h
fmap 2 53
acta
OMIT -2 58
OMIT 2 0 0
WGHT 0.042 0.15
FVAR 2.37564
REM
REM
REM
O1 4 0.40564 -0.11401 0.30705 11.00000 0.05873 0.02833 0.03504 =
-0.00856 0.02245 -0.01228
N1 3 0.46655 0.41420 0.34259 11.00000 0.03313 0.01664 0.02476 =
0.00025 0.00074 0.00138
N2 3 0.43000 0.22788 0.43630 11.00000 0.03196 0.01465 0.02272 =
-0.00217 0.00517 -0.00084
N3 3 0.41328 0.10016 0.42730 11.00000 0.02515 0.01414 0.02434 =
-0.00120 0.00245 0.00029
C1 1 0.46638 0.28536 0.34119 11.00000 0.02198 0.01816 0.02017 =
0.00084 -0.00160 -0.00076
C2 1 0.50000 0.21615 0.25000 10.50000 0.02612 0.01286 0.02423 =
-0.00000 0.00360 0.00000
AFIX 43
H2 2 0.50000 0.12545 0.25000 10.50000 -1.20000
AFIX 0
C3 1 0.50000 0.46856 0.25000 10.50000 0.03828 0.01141 0.02661 =
-0.00000 0.00186 -0.00000
AFIX 43
H3 2 0.50000 0.55927 0.25000 10.50000 -1.20000
AFIX 0
C4 1 0.41273 0.29810 0.54299 11.00000 0.03608 0.02061 0.02480 =
-0.00331 0.00582 0.00005
AFIX 137
H4a 2 0.35044 0.29835 0.55368 11.00000 -1.50000
H4b 2 0.43321 0.38616 0.53607 11.00000 -1.50000
H4c 2 0.44290 0.25709 0.61110 11.00000 -1.50000
AFIX 0
C5 1 0.37973 0.04139 0.51346 11.00000 0.02390 0.02117 0.02077 =
-0.00128 0.00201 0.00024
AFIX 43
H5 2 0.36885 0.08693 0.58346 11.00000 -1.20000
AFIX 0
C6 1 0.35831 -0.09370 0.50495 11.00000 0.01949 0.02163 0.02361 =
0.00166 0.00164 0.00070
C7 1 0.37220 -0.16707 0.40409 11.00000 0.02579 0.02183 0.03253 =
0.00040 0.00774 0.00097
C8 1 0.35332 -0.29651 0.40225 11.00000 0.03073 0.02328 0.04986 =
-0.00751 0.01183 0.00024
AFIX 43
H8 2 0.36301 -0.34571 0.33395 11.00000 -1.20000
AFIX 0
C9 1 0.32059 -0.35367 0.49920 11.00000 0.02344 0.01829 0.05847 =
0.00703 0.00034 -0.00130
AFIX 43
H9 2 0.30919 -0.44279 0.49800 11.00000 -1.20000
AFIX 0
C10 1 0.30404 -0.28321 0.59843 11.00000 0.02871 0.03206 0.03616 =
0.01288 -0.00245 -0.00656
AFIX 43
H10 2 0.28022 -0.32298 0.66443 11.00000 -1.20000
AFIX 0
C11 1 0.32260 -0.15427 0.60028 11.00000 0.02929 0.02768 0.02941 =
0.00404 0.00091 -0.00489
AFIX 43
H11 2 0.31076 -0.10558 0.66810 11.00000 -1.20000
AFIX 0
H1 2 0.41774 -0.02313 0.32658 11.00000 0.08486
HKLF 4
END
;
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_Ir2dpyx2L6_16srv324
_database_code_depnum_ccdc_archive 'CCDC 2006848'
loop_
_audit_author_name
_audit_author_address
'Dmitry Yufit'
;Durham University
United Kingdom
;
_audit_update_record
;
2020-07-07 deposited with the CCDC. 2020-07-10 downloaded from the CCDC.
;
_audit_creation_date 2017-01-18
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety
'2(C64 H64 Ir2 N10 O2), 3(F6 P), C H4 O, 6(C2 H3 N)'
_chemical_formula_sum 'C141 H150 F18 Ir4 N26 O5 P3'
_chemical_formula_weight 3492.57
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 12.2674(11)
_cell_length_b 16.3422(15)
_cell_length_c 21.227(2)
_cell_angle_alpha 75.235(3)
_cell_angle_beta 76.582(3)
_cell_angle_gamma 87.493(3)
_cell_volume 4002.2(6)
_cell_formula_units_Z 1
_cell_measurement_reflns_used 9442
_cell_measurement_temperature 120.0
_cell_measurement_theta_max 31.46
_cell_measurement_theta_min 2.43
_shelx_estimated_absorpt_T_max 0.821
_shelx_estimated_absorpt_T_min 0.611
_exptl_absorpt_coefficient_mu 3.422
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.8352
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0667 before and 0.0509 after correction.
The Ratio of minimum to maximum transmission is 0.8352.
The \l/2 correction factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear orange'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_primary orange
_exptl_crystal_density_diffrn 1.449
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description prism
_exptl_crystal_F_000 1733
_exptl_crystal_size_max 0.16
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.06
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0351
_diffrn_reflns_av_unetI/netI 0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 83046
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.999
_diffrn_reflns_theta_min 2.120
_diffrn_ambient_temperature 120.0
_diffrn_detector 'Bruker PHOTON 100 CMOS'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type 'CMOS sensor'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device '3-circle diffractometer'
_diffrn_measurement_device_type 'Bruker D8 Venture'
_diffrn_measurement_method \w-scan
_diffrn_radiation_monochromator 'focusing mirrors'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_type 'Incoatec I\mS microsource'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 16817
_reflns_number_total 21245
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
Structure factors included contributions from the .fab file.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing.bruker_data_scaling 'SADABS V2012/1 (Bruker AXS Inc.)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection 'APEX2 v.2013.4_1 (Bruker, 2013)'
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'XS (Sheldrick, 2008)'
_refine_diff_density_max 4.907
_refine_diff_density_min -3.051
_refine_diff_density_rms 0.174
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.053
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 891
_refine_ls_number_reflns 21245
_refine_ls_number_restraints 64
_refine_ls_R_factor_all 0.0674
_refine_ls_R_factor_gt 0.0484
_refine_ls_restrained_S_all 1.054
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0230P)^2^+45.6800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1054
_refine_ls_wR_factor_ref 0.1166
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H) groups
2. Restrained distances
P2-F6A \\sim P2-F4 \\sim P2-F4A \\sim P2-F8 \\sim P2-F8A \\sim P2-F9 \\sim
P2-F9A \\sim P2-F6
with sigma of 0.005
N1S-C2S \\sim N2S-C4S \\sim N3S-C6S \\sim N4S-C8S
with sigma of 0.005
C3S-C2S \\sim C5S-C4S \\sim C7S-C6S \\sim C9S-C8S
with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C22) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.005
Uanis(C5S) \\sim Ueq, Uanis(C4S) \\sim Ueq, Uanis(N2S) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
4. Others
Fixed Sof: C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C17A(0.5) H17D(0.5)
H17E(0.5) H17F(0.5) C26(0.6) H26A(0.6) H26B(0.6) H26C(0.6) C26A(0.4) H26D(0.4)
H26E(0.4) H26F(0.4) C27(0.6) H27A(0.6) H27B(0.6) H27C(0.6) C27A(0.4) H27D(0.4)
H27E(0.4) H27F(0.4) C28(0.6) H28A(0.6) H28B(0.6) H28C(0.6) C28A(0.4) H28D(0.4)
H28E(0.4) H28F(0.4) F4(0.5) F4A(0.5) F6(0.5) F6A(0.5) F8(0.5) F8A(0.5) F9(0.5)
F9A(0.5) O1S(0.5) H1S(0.5) C10S(0.5) H10D(0.5) H10E(0.5) H10F(0.5) N1S(0.5)
C2S(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) H3SC(0.5) N4S(0.5) C8S(0.5) C9S(0.5)
H9SA(0.5) H9SB(0.5) H9SC(0.5)
5.a Riding coordinates:
C17(H17A,H17B,H17C), C17A(H17D,H17E,H17F), O1S(H1S), C10S(H10D,H10E,H10F),
C3S(H3SA,H3SB,H3SC), C5S(H5SA,H5SB,H5SC), C7S(H7SA,H7SB,H7SC), C9S(H9SA,H9SB,
H9SC)
5.b Aromatic/amide H refined with riding coordinates:
C3(H3), C5(H5), C6(H6), C11(H11), C14(H14), C16(H16), C18(H18), C21(H21),
C22(H22), C24(H24), C29(H29), C30(H30), C31(H31), C32(H32), C38(H38), C43(H43),
C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50),
C56(H56), C61(H61), C62(H62), C63(H63), C64(H64)
5.c Idealised Me refined as rotating group:
C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
C26(H26A,H26B,H26C), C26A(H26D,H26E,H26F), C27(H27A,H27B,H27C), C27A(H27D,H27E,
H27F), C28(H28A,H28B,H28C), C28A(H28D,H28E,H28F), C40(H40A,H40B,H40C),
C41(H41A,H41B,H41C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.28441(2) 0.60850(2) 0.13055(2) 0.01853(5) Uani 1 1 d . . . . .
Ir2 Ir 0.58523(2) 0.65642(2) 0.30615(2) 0.01874(5) Uani 1 1 d . . . . .
O1 O 0.2129(3) 0.5593(2) 0.0710(2) 0.0228(8) Uani 1 1 d . . . . .
O2 O 0.7011(3) 0.6382(3) 0.3626(2) 0.0255(8) Uani 1 1 d . . . . .
N1 N 0.2293(4) 0.7300(3) 0.0952(3) 0.0227(10) Uani 1 1 d . . . . .
N2 N 0.2548(4) 0.7873(3) 0.1281(3) 0.0259(10) Uani 1 1 d . . . . .
N3 N 0.3518(4) 0.6745(3) 0.1816(2) 0.0209(9) Uani 1 1 d . . . . .
N4 N 0.4722(4) 0.6933(3) 0.2486(2) 0.0199(9) Uani 1 1 d . . . . .
N5 N 0.5028(5) 0.8271(3) 0.2624(3) 0.0363(13) Uani 1 1 d . . . . .
N6 N 0.5770(4) 0.7857(3) 0.2993(3) 0.0258(10) Uani 1 1 d . . . . .
N7 N 0.4372(4) 0.6090(3) 0.0657(3) 0.0239(10) Uani 1 1 d . . . . .
N8 N 0.1488(4) 0.5683(3) 0.2081(2) 0.0222(9) Uani 1 1 d . . . . .
N9 N 0.7099(4) 0.6523(3) 0.2236(2) 0.0222(9) Uani 1 1 d . . . . .
N10 N 0.4633(4) 0.6169(3) 0.3923(2) 0.0212(9) Uani 1 1 d . . . . .
C1 C 0.1619(4) 0.6073(3) 0.0265(3) 0.0223(11) Uani 1 1 d . . . . .
C2 C 0.1396(4) 0.6957(4) 0.0156(3) 0.0237(11) Uani 1 1 d . . . . .
C3 C 0.0779(4) 0.7340(4) -0.0324(3) 0.0250(12) Uani 1 1 d . . . . .
H3 H 0.0639 0.7928 -0.0388 0.030 Uiso 1 1 calc R . . . .
C4 C 0.0364(5) 0.6913(4) -0.0708(3) 0.0243(11) Uani 1 1 d . . . . .
C5 C 0.0610(4) 0.6044(4) -0.0602(3) 0.0234(11) Uani 1 1 d . . . . .
H5 H 0.0350 0.5721 -0.0853 0.028 Uiso 1 1 calc R . . . .
C6 C 0.1215(4) 0.5653(4) -0.0143(3) 0.0243(12) Uani 1 1 d . . . . .
H6 H 0.1370 0.5069 -0.0098 0.029 Uiso 1 1 calc R . . . .
C7 C -0.0346(5) 0.7378(4) -0.1192(3) 0.0298(13) Uani 1 1 d . . . . .
C8 C -0.1372(6) 0.7737(5) -0.0790(4) 0.0407(17) Uani 1 1 d . . . . .
H8A H -0.1802 0.7274 -0.0445 0.061 Uiso 1 1 calc GR . . . .
H8B H -0.1845 0.8025 -0.1091 0.061 Uiso 1 1 calc GR . . . .
H8C H -0.1127 0.8140 -0.0578 0.061 Uiso 1 1 calc GR . . . .
C9 C 0.0346(6) 0.8101(4) -0.1715(4) 0.0412(17) Uani 1 1 d . . . . .
H9A H 0.0564 0.8504 -0.1493 0.062 Uiso 1 1 calc GR . . . .
H9B H -0.0101 0.8390 -0.2031 0.062 Uiso 1 1 calc GR . . . .
H9C H 0.1021 0.7874 -0.1957 0.062 Uiso 1 1 calc GR . . . .
C10 C -0.0748(5) 0.6792(4) -0.1552(3) 0.0332(14) Uani 1 1 d . . . . .
H10A H -0.0101 0.6598 -0.1842 0.050 Uiso 1 1 calc GR . . . .
H10B H -0.1254 0.7100 -0.1823 0.050 Uiso 1 1 calc GR . . . .
H10C H -0.1147 0.6303 -0.1221 0.050 Uiso 1 1 calc GR . . . .
C11 C 0.1710(5) 0.7521(4) 0.0507(3) 0.0251(12) Uani 1 1 d . . . . .
H11 H 0.1472 0.8091 0.0404 0.030 Uiso 1 1 calc R . . . .
C12 C 0.2139(6) 0.8742(4) 0.1131(4) 0.0351(15) Uani 1 1 d . . . . .
H12A H 0.2252 0.9022 0.1469 0.053 Uiso 1 1 calc GR . . . .
H12B H 0.1339 0.8730 0.1137 0.053 Uiso 1 1 calc GR . . . .
H12C H 0.2554 0.9054 0.0688 0.053 Uiso 1 1 calc GR . . . .
C13 C 0.3262(5) 0.7594(3) 0.1688(3) 0.0233(11) Uani 1 1 d . . . . .
C14 C 0.3727(5) 0.8119(4) 0.1974(3) 0.0295(13) Uani 1 1 d . . . . .
H14 H 0.3531 0.8698 0.1907 0.035 Uiso 1 1 calc R . . . .
C15 C 0.4484(5) 0.7786(3) 0.2362(3) 0.0258(12) Uani 1 1 d . . . . .
C16 C 0.4231(4) 0.6469(3) 0.2202(3) 0.0203(11) Uani 1 1 d . . . . .
H16 H 0.4404 0.5885 0.2283 0.024 Uiso 1 1 calc R . . . .
C17 C 0.4654(14) 0.9137(10) 0.2676(8) 0.040(3) Uiso 0.5 1 d . . . A 1
H17A H 0.4533 0.9460 0.2253 0.059 Uiso 0.5 1 d R . . A 1
H17B H 0.5221 0.9412 0.2798 0.059 Uiso 0.5 1 d R . . A 1
H17C H 0.3969 0.9096 0.3012 0.059 Uiso 0.5 1 d R . . A 1
C17A C 0.5036(12) 0.9218(8) 0.2421(7) 0.029(3) Uiso 0.5 1 d . . . A 2
H17D H 0.4686 0.9406 0.2049 0.044 Uiso 0.5 1 d R . . A 2
H17E H 0.4631 0.9429 0.2790 0.044 Uiso 0.5 1 d R . . A 2
H17F H 0.5795 0.9427 0.2292 0.044 Uiso 0.5 1 d R . . A 2
C18 C 0.6301(5) 0.8266(4) 0.3281(3) 0.0289(13) Uani 1 1 d . . . . .
H18 H 0.6182 0.8856 0.3221 0.035 Uiso 1 1 calc R . . . .
C19 C 0.7057(5) 0.7874(4) 0.3685(3) 0.0276(12) Uani 1 1 d . . . . .
C20 C 0.7362(5) 0.7004(4) 0.3832(3) 0.0240(11) Uani 1 1 d . . . . .
C21 C 0.8124(6) 0.6779(4) 0.4243(3) 0.0334(14) Uani 1 1 d . . . . .
H21 H 0.8371 0.6212 0.4352 0.040 Uiso 1 1 calc R . . . .
C22 C 0.8513(5) 0.7373(4) 0.4488(3) 0.0318(13) Uani 1 1 d . U . . .
H22 H 0.9019 0.7187 0.4771 0.038 Uiso 1 1 calc R . . . .
C23 C 0.8249(7) 0.8208(5) 0.4367(4) 0.0417(17) Uani 1 1 d . . . . .
C24 C 0.7508(6) 0.8444(4) 0.3960(3) 0.0354(15) Uani 1 1 d . . . . .
H24 H 0.7289 0.9018 0.3859 0.042 Uiso 1 1 calc R . . . .
C25 C 0.8700(8) 0.8863(5) 0.4657(4) 0.049(2) Uani 1 1 d . . . . .
C26 C 0.9327(12) 0.9524(9) 0.4090(7) 0.046(3) Uiso 0.6 1 d . . . B 1
H26A H 0.9909 0.9260 0.3808 0.069 Uiso 0.6 1 calc GR . . B 1
H26B H 0.9676 0.9922 0.4263 0.069 Uiso 0.6 1 calc GR . . B 1
H26C H 0.8811 0.9828 0.3825 0.069 Uiso 0.6 1 calc GR . . B 1
C26A C 0.839(3) 0.977(2) 0.4377(18) 0.101(10) Uiso 0.4 1 d . . . B 2
H26D H 0.8598 1.0136 0.4636 0.151 Uiso 0.4 1 calc GR . . B 2
H26E H 0.7579 0.9806 0.4409 0.151 Uiso 0.4 1 calc GR . . B 2
H26F H 0.8788 0.9969 0.3908 0.151 Uiso 0.4 1 calc GR . . B 2
C27 C 0.9471(12) 0.8434(9) 0.5114(7) 0.048(3) Uiso 0.6 1 d . . . B 1
H27A H 1.0121 0.8205 0.4852 0.072 Uiso 0.6 1 calc GR . . B 1
H27B H 0.9059 0.7974 0.5471 0.072 Uiso 0.6 1 calc GR . . B 1
H27C H 0.9726 0.8850 0.5311 0.072 Uiso 0.6 1 calc GR . . B 1
C27A C 0.998(2) 0.890(2) 0.4422(16) 0.082(8) Uiso 0.4 1 d . . . B 2
H27D H 1.0187 0.9102 0.3933 0.123 Uiso 0.4 1 calc GR . . B 2
H27E H 1.0278 0.8333 0.4559 0.123 Uiso 0.4 1 calc GR . . B 2
H27F H 1.0285 0.9288 0.4622 0.123 Uiso 0.4 1 calc GR . . B 2
C28 C 0.7701(13) 0.9218(10) 0.5079(8) 0.057(4) Uiso 0.6 1 d . . . B 1
H28A H 0.7970 0.9620 0.5284 0.086 Uiso 0.6 1 calc GR . . B 1
H28B H 0.7287 0.8754 0.5431 0.086 Uiso 0.6 1 calc GR . . B 1
H28C H 0.7206 0.9507 0.4794 0.086 Uiso 0.6 1 calc GR . . B 1
C28A C 0.847(3) 0.8604(19) 0.5388(14) 0.081(8) Uiso 0.4 1 d . . . B 2
H28D H 0.8820 0.8056 0.5529 0.121 Uiso 0.4 1 calc GR . . B 2
H28E H 0.7664 0.8555 0.5572 0.121 Uiso 0.4 1 calc GR . . B 2
H28F H 0.8790 0.9029 0.5551 0.121 Uiso 0.4 1 calc GR . . B 2
C29 C 0.4779(5) 0.6723(4) 0.0122(3) 0.0282(13) Uani 1 1 d . . . . .
H29 H 0.4356 0.7224 0.0041 0.034 Uiso 1 1 calc R . . . .
C30 C 0.5789(5) 0.6674(4) -0.0317(3) 0.0350(14) Uani 1 1 d . . . . .
H30 H 0.6067 0.7133 -0.0691 0.042 Uiso 1 1 calc R . . . .
C31 C 0.6388(5) 0.5928(4) -0.0194(4) 0.0348(15) Uani 1 1 d . . . . .
H31 H 0.7075 0.5866 -0.0494 0.042 Uiso 1 1 calc R . . . .
C32 C 0.5988(5) 0.5291(4) 0.0354(4) 0.0330(14) Uani 1 1 d . . . . .
H32 H 0.6410 0.4790 0.0439 0.040 Uiso 1 1 calc R . . . .
C33 C 0.4975(4) 0.5354(4) 0.0795(3) 0.0249(12) Uani 1 1 d . . . . .
C34 C 0.4417(5) 0.4717(3) 0.1395(3) 0.0245(12) Uani 1 1 d . . . . .
C35 C 0.3354(5) 0.4963(3) 0.1697(3) 0.0209(11) Uani 1 1 d . . . . .
C36 C 0.2635(5) 0.4460(4) 0.2259(3) 0.0247(11) Uani 1 1 d . . . . .
C37 C 0.3032(6) 0.3666(4) 0.2556(3) 0.0350(14) Uani 1 1 d . . . . .
C38 C 0.4096(6) 0.3434(4) 0.2264(4) 0.0398(16) Uani 1 1 d . . . . .
H38 H 0.4360 0.2900 0.2469 0.048 Uiso 1 1 calc R . . . .
C39 C 0.4806(5) 0.3925(4) 0.1694(4) 0.0321(14) Uani 1 1 d . . . . .
C40 C 0.5938(6) 0.3570(5) 0.1443(4) 0.0462(19) Uani 1 1 d . . . . .
H40A H 0.5953 0.3431 0.1019 0.069 Uiso 1 1 calc GR . . . .
H40B H 0.6069 0.3058 0.1774 0.069 Uiso 1 1 calc GR . . . .
H40C H 0.6526 0.3993 0.1374 0.069 Uiso 1 1 calc GR . . . .
C41 C 0.2384(8) 0.3074(5) 0.3195(4) 0.057(2) Uani 1 1 d . . . . .
H41A H 0.2236 0.3363 0.3558 0.085 Uiso 1 1 calc GR . . . .
H41B H 0.2826 0.2568 0.3315 0.085 Uiso 1 1 calc GR . . . .
H41C H 0.1672 0.2909 0.3125 0.085 Uiso 1 1 calc GR . . . .
C42 C 0.1557(5) 0.4867(4) 0.2454(3) 0.0241(11) Uani 1 1 d . . . . .
C43 C 0.0650(6) 0.4527(5) 0.2974(3) 0.0359(15) Uani 1 1 d . . . . .
H43 H 0.0679 0.3963 0.3234 0.043 Uiso 1 1 calc R . . . .
C44 C -0.0298(5) 0.5003(5) 0.3116(3) 0.0382(16) Uani 1 1 d . . . . .
H44 H -0.0921 0.4762 0.3465 0.046 Uiso 1 1 calc R . . . .
C45 C -0.0330(5) 0.5822(5) 0.2752(3) 0.0358(15) Uani 1 1 d . . . . .
H45 H -0.0959 0.6164 0.2858 0.043 Uiso 1 1 calc R . . . .
C46 C 0.0566(5) 0.6143(4) 0.2229(3) 0.0274(12) Uani 1 1 d . . . . .
H46 H 0.0533 0.6704 0.1965 0.033 Uiso 1 1 calc R . . . .
C47 C 0.7623(5) 0.7196(4) 0.1782(3) 0.0280(12) Uani 1 1 d . . . . .
H47 H 0.7466 0.7743 0.1855 0.034 Uiso 1 1 calc R . . . .
C48 C 0.8393(5) 0.7118(4) 0.1206(3) 0.0357(15) Uani 1 1 d . . . . .
H48 H 0.8752 0.7606 0.0889 0.043 Uiso 1 1 calc R . . . .
C49 C 0.8624(5) 0.6328(4) 0.1105(3) 0.0356(15) Uani 1 1 d . . . . .
H49 H 0.9143 0.6261 0.0713 0.043 Uiso 1 1 calc R . . . .
C50 C 0.8094(5) 0.5629(4) 0.1579(3) 0.0263(12) Uani 1 1 d . . . . .
H50 H 0.8245 0.5080 0.1508 0.032 Uiso 1 1 calc R . . . .
C51 C 0.7348(4) 0.5719(3) 0.2155(3) 0.0201(10) Uani 1 1 d . . . . .
C52 C 0.6715(4) 0.5035(3) 0.2695(3) 0.0194(10) Uani 1 1 d . . . . .
C53 C 0.5883(4) 0.5350(3) 0.3145(3) 0.0174(10) Uani 1 1 d . . . . .
C54 C 0.5157(4) 0.4825(4) 0.3697(3) 0.0211(11) Uani 1 1 d . . . . .
C55 C 0.5206(5) 0.3947(4) 0.3768(3) 0.0249(12) Uani 1 1 d . . . . .
C56 C 0.6072(5) 0.3644(3) 0.3338(3) 0.0283(13) Uani 1 1 d . . . . .
H56 H 0.6134 0.3048 0.3405 0.034 Uiso 1 1 calc R . . . .
C57 C 0.6861(5) 0.4156(4) 0.2811(3) 0.0247(11) Uani 1 1 d . . . . .
C58 C 0.7836(5) 0.3734(4) 0.2456(3) 0.0304(13) Uani 1 1 d . . . . .
H58A H 0.7786 0.3803 0.1991 0.046 Uiso 1 1 calc GR . . . .
H58B H 0.7821 0.3130 0.2681 0.046 Uiso 1 1 calc GR . . . .
H58C H 0.8536 0.3993 0.2463 0.046 Uiso 1 1 calc GR . . . .
C59 C 0.4397(6) 0.3303(4) 0.4287(4) 0.0374(15) Uani 1 1 d . . . . .
H59A H 0.4533 0.3260 0.4731 0.056 Uiso 1 1 calc GR . . . .
H59B H 0.4510 0.2750 0.4184 0.056 Uiso 1 1 calc GR . . . .
H59C H 0.3626 0.3482 0.4282 0.056 Uiso 1 1 calc GR . . . .
C60 C 0.4475(4) 0.5311(4) 0.4146(3) 0.0216(11) Uani 1 1 d . . . . .
C61 C 0.3752(5) 0.4978(4) 0.4761(3) 0.0273(12) Uani 1 1 d . . . . .
H61 H 0.3635 0.4383 0.4918 0.033 Uiso 1 1 calc R . . . .
C62 C 0.3200(5) 0.5503(5) 0.5147(3) 0.0338(14) Uani 1 1 d . . . . .
H62 H 0.2737 0.5271 0.5578 0.041 Uiso 1 1 calc R . . . .
C63 C 0.3334(5) 0.6372(5) 0.4895(3) 0.0365(15) Uani 1 1 d . . . . .
H63 H 0.2928 0.6747 0.5138 0.044 Uiso 1 1 calc R . . . .
C64 C 0.4064(5) 0.6679(4) 0.4289(3) 0.0297(13) Uani 1 1 d . . . . .
H64 H 0.4172 0.7274 0.4121 0.036 Uiso 1 1 calc R . . . .
P1 P 1.0000 1.0000 0.0000 0.0319(5) Uani 1 2 d S T P . .
F1 F 1.0545(5) 1.0254(3) 0.0537(3) 0.0617(14) Uani 1 1 d . . . . .
F2 F 0.8860(4) 1.0425(3) 0.0277(3) 0.0563(13) Uani 1 1 d . . . . .
F3 F 0.9600(4) 0.9115(3) 0.0521(2) 0.0516(11) Uani 1 1 d . . . . .
P2 P 0.5972(2) 1.10286(12) 0.31922(11) 0.0517(5) Uani 1 1 d D . . . .
F4 F 0.6870(9) 1.1768(6) 0.2809(6) 0.068(3) Uiso 0.5 1 d D . . C 1
F4A F 0.6447(9) 1.1859(5) 0.2626(4) 0.056(3) Uiso 0.5 1 d D . . C 2
F5 F 0.5135(6) 1.1591(4) 0.3578(4) 0.098(2) Uani 1 1 d . . . . .
F6 F 0.6619(13) 1.0655(11) 0.3769(6) 0.113(5) Uiso 0.5 1 d D . . C 1
F6A F 0.6849(11) 1.1222(11) 0.3584(8) 0.105(5) Uiso 0.5 1 d D . . C 2
F7 F 0.6798(5) 1.0433(3) 0.2808(3) 0.0733(16) Uani 1 1 d . . . . .
F8 F 0.5353(14) 1.1341(12) 0.2591(6) 0.108(6) Uiso 0.5 1 d D . . C 1
F8A F 0.5080(10) 1.0933(10) 0.2773(7) 0.087(4) Uiso 0.5 1 d D . . C 2
F9 F 0.5070(9) 1.0279(6) 0.3525(6) 0.080(4) Uiso 0.5 1 d D . . C 1
F9A F 0.5570(12) 1.0179(6) 0.3755(5) 0.084(4) Uiso 0.5 1 d D . . C 2
O1S O 0.0140(17) 0.5387(12) 0.5107(10) 0.112(6) Uiso 0.5 1 d . . . D -1
H1S H 0.0607 0.5329 0.4776 0.167 Uiso 0.5 1 d R . . D -1
C10S C 0.0476(14) 0.6117(11) 0.5280(9) 0.050(4) Uiso 0.5 1 d . . . D -1
H10D H -0.0100 0.6191 0.5653 0.075 Uiso 0.5 1 d R . . D -1
H10E H 0.1175 0.6008 0.5414 0.075 Uiso 0.5 1 d R . . D -1
H10F H 0.0549 0.6621 0.4921 0.075 Uiso 0.5 1 d R . . D -1
N1S N 0.3025(13) 0.8738(11) 0.4153(8) 0.067(4) Uiso 0.5 1 d D . . . .
C2S C 0.3579(11) 0.8776(9) 0.4480(7) 0.038(3) Uiso 0.5 1 d D . . . .
C3S C 0.4387(13) 0.8842(11) 0.4848(8) 0.054(4) Uiso 0.5 1 d D . . . .
H3SA H 0.4287 0.8428 0.5269 0.081 Uiso 0.5 1 d R . . . .
H3SB H 0.5092 0.8757 0.4564 0.081 Uiso 0.5 1 d R . . . .
H3SC H 0.4377 0.9399 0.4920 0.081 Uiso 0.5 1 d R . . . .
N2S N 0.2154(8) 0.6035(6) 0.3478(5) 0.080(3) Uani 1 1 d D U . . .
C4S C 0.1835(9) 0.6672(6) 0.3480(6) 0.072(3) Uani 1 1 d D U . . .
C5S C 0.1382(13) 0.7482(8) 0.3503(8) 0.117(5) Uani 1 1 d D U . . .
H5SA H 0.1492 0.7624 0.3897 0.176 Uiso 1 1 d R . . . .
H5SB H 0.0595 0.7477 0.3516 0.176 Uiso 1 1 d R . . . .
H5SC H 0.1759 0.7895 0.3112 0.176 Uiso 1 1 d R . . . .
N3S N 0.9623(8) 0.8003(5) 0.2355(5) 0.082(3) Uani 1 1 d D . . . .
C6S C 0.9436(8) 0.8679(5) 0.2289(5) 0.058(2) Uani 1 1 d D . . . .
C7S C 0.9187(9) 0.9556(5) 0.2184(6) 0.075(3) Uani 1 1 d D . . . .
H7SA H 0.8389 0.9623 0.2271 0.112 Uiso 1 1 d R . . . .
H7SB H 0.9487 0.9790 0.2480 0.112 Uiso 1 1 d R . . . .
H7SC H 0.9514 0.9845 0.1729 0.112 Uiso 1 1 d R . . . .
N4S N 0.5772(17) 0.7835(11) 0.0839(9) 0.091(6) Uiso 0.5 1 d D . . . .
C8S C 0.6110(15) 0.8374(10) 0.0419(8) 0.059(4) Uiso 0.5 1 d D . . E 1
C9S C 0.6694(12) 0.9115(8) -0.0013(7) 0.038(3) Uiso 0.5 1 d D . . E 1
H9SA H 0.6236 0.9600 0.0022 0.058 Uiso 0.5 1 d R . . E 1
H9SB H 0.7382 0.9180 0.0113 0.058 Uiso 0.5 1 d R . . E 1
H9SC H 0.6856 0.9063 -0.0466 0.058 Uiso 0.5 1 d R . . E 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ir1 0.01442(9) 0.01218(9) 0.02866(11) -0.00762(8) -0.00180(8) 0.00156(7)
Ir2 0.01696(10) 0.01608(10) 0.02362(11) -0.00893(8) -0.00069(8) -0.00227(7)
O1 0.0208(18) 0.0168(18) 0.033(2) -0.0113(16) -0.0057(16) 0.0001(14)
O2 0.026(2) 0.028(2) 0.024(2) -0.0095(17) -0.0029(16) -0.0057(16)
N1 0.018(2) 0.015(2) 0.035(3) -0.0088(19) -0.0027(19) 0.0018(17)
N2 0.025(2) 0.015(2) 0.040(3) -0.011(2) -0.008(2) 0.0065(18)
N3 0.016(2) 0.015(2) 0.031(2) -0.0083(18) -0.0023(18) 0.0021(16)
N4 0.016(2) 0.016(2) 0.028(2) -0.0084(18) -0.0021(18) 0.0005(16)
N5 0.037(3) 0.018(2) 0.066(4) -0.022(3) -0.025(3) 0.006(2)
N6 0.025(2) 0.022(2) 0.033(3) -0.013(2) -0.003(2) -0.0044(19)
N7 0.017(2) 0.020(2) 0.035(3) -0.013(2) 0.0005(19) 0.0019(17)
N8 0.017(2) 0.022(2) 0.027(2) -0.0077(19) -0.0025(18) -0.0031(17)
N9 0.019(2) 0.020(2) 0.026(2) -0.0066(19) -0.0004(18) 0.0003(17)
N10 0.019(2) 0.024(2) 0.022(2) -0.0114(19) -0.0011(18) 0.0001(18)
C1 0.014(2) 0.018(2) 0.030(3) -0.005(2) 0.005(2) -0.0010(19)
C2 0.015(2) 0.021(3) 0.034(3) -0.010(2) 0.002(2) -0.001(2)
C3 0.016(2) 0.020(3) 0.035(3) -0.008(2) 0.002(2) 0.002(2)
C4 0.017(2) 0.026(3) 0.025(3) -0.004(2) 0.004(2) 0.000(2)
C5 0.012(2) 0.030(3) 0.027(3) -0.009(2) 0.000(2) -0.006(2)
C6 0.018(2) 0.021(3) 0.030(3) -0.007(2) 0.005(2) -0.002(2)
C7 0.022(3) 0.033(3) 0.033(3) -0.010(3) 0.000(2) 0.002(2)
C8 0.026(3) 0.052(4) 0.054(4) -0.029(4) -0.013(3) 0.013(3)
C9 0.034(4) 0.033(4) 0.051(4) 0.001(3) -0.011(3) 0.003(3)
C10 0.027(3) 0.040(4) 0.034(3) -0.013(3) -0.005(3) 0.002(3)
C11 0.019(3) 0.017(3) 0.037(3) -0.009(2) 0.001(2) 0.003(2)
C12 0.043(4) 0.017(3) 0.050(4) -0.013(3) -0.016(3) 0.011(3)
C13 0.020(3) 0.015(2) 0.034(3) -0.008(2) -0.002(2) 0.003(2)
C14 0.031(3) 0.014(2) 0.045(4) -0.010(2) -0.010(3) 0.005(2)
C15 0.025(3) 0.016(3) 0.039(3) -0.013(2) -0.006(2) 0.000(2)
C16 0.019(2) 0.012(2) 0.030(3) -0.009(2) -0.001(2) -0.0011(19)
C18 0.030(3) 0.027(3) 0.031(3) -0.015(3) -0.001(3) -0.008(2)
C19 0.029(3) 0.029(3) 0.026(3) -0.012(2) -0.001(2) -0.009(2)
C20 0.029(3) 0.025(3) 0.018(3) -0.007(2) -0.003(2) -0.006(2)
C21 0.037(3) 0.035(3) 0.030(3) -0.006(3) -0.010(3) -0.010(3)
C22 0.033(2) 0.034(2) 0.0286(19) 0.0001(15) -0.0175(16) 0.0028(16)
C23 0.056(5) 0.037(4) 0.035(4) -0.009(3) -0.012(3) -0.021(3)
C24 0.053(4) 0.029(3) 0.030(3) -0.011(3) -0.015(3) -0.011(3)
C25 0.068(5) 0.044(4) 0.045(4) -0.015(3) -0.024(4) -0.010(4)
C29 0.020(3) 0.022(3) 0.041(3) -0.008(2) -0.003(2) 0.001(2)
C30 0.028(3) 0.034(3) 0.037(4) -0.010(3) 0.005(3) -0.007(3)
C31 0.017(3) 0.042(4) 0.048(4) -0.025(3) 0.002(3) -0.003(2)
C32 0.018(3) 0.031(3) 0.053(4) -0.022(3) -0.003(3) 0.002(2)
C33 0.016(2) 0.022(3) 0.042(3) -0.017(2) -0.007(2) 0.004(2)
C34 0.024(3) 0.018(3) 0.035(3) -0.013(2) -0.008(2) 0.003(2)
C35 0.023(3) 0.013(2) 0.031(3) -0.009(2) -0.013(2) 0.0014(19)
C36 0.027(3) 0.019(3) 0.029(3) -0.006(2) -0.009(2) 0.000(2)
C37 0.046(4) 0.022(3) 0.036(3) 0.000(3) -0.017(3) -0.002(3)
C38 0.053(4) 0.016(3) 0.055(4) -0.007(3) -0.025(4) 0.009(3)
C39 0.034(3) 0.023(3) 0.049(4) -0.018(3) -0.020(3) 0.010(2)
C40 0.040(4) 0.038(4) 0.066(5) -0.018(4) -0.021(4) 0.026(3)
C41 0.072(6) 0.035(4) 0.052(5) 0.013(4) -0.016(4) -0.001(4)
C42 0.023(3) 0.025(3) 0.024(3) -0.005(2) -0.005(2) -0.005(2)
C43 0.036(3) 0.042(4) 0.027(3) -0.001(3) -0.007(3) -0.014(3)
C44 0.021(3) 0.060(5) 0.030(3) -0.009(3) 0.001(3) -0.014(3)
C45 0.019(3) 0.053(4) 0.035(3) -0.018(3) 0.000(3) 0.004(3)
C46 0.020(3) 0.031(3) 0.034(3) -0.013(3) -0.007(2) 0.001(2)
C47 0.024(3) 0.022(3) 0.032(3) -0.005(2) 0.004(2) -0.004(2)
C48 0.028(3) 0.033(3) 0.038(4) -0.004(3) 0.004(3) -0.005(3)
C49 0.028(3) 0.039(4) 0.033(3) -0.011(3) 0.010(3) -0.004(3)
C50 0.020(3) 0.029(3) 0.028(3) -0.010(2) 0.001(2) 0.001(2)
C51 0.016(2) 0.020(3) 0.024(3) -0.008(2) -0.003(2) -0.0004(19)
C52 0.015(2) 0.021(3) 0.023(3) -0.009(2) -0.002(2) 0.0002(19)
C53 0.015(2) 0.018(2) 0.023(3) -0.010(2) -0.007(2) -0.0007(18)
C54 0.016(2) 0.024(3) 0.025(3) -0.010(2) -0.004(2) -0.001(2)
C55 0.026(3) 0.020(3) 0.029(3) -0.005(2) -0.006(2) -0.004(2)
C56 0.032(3) 0.012(2) 0.040(3) -0.007(2) -0.006(3) 0.002(2)
C57 0.025(3) 0.025(3) 0.028(3) -0.010(2) -0.010(2) 0.004(2)
C58 0.030(3) 0.026(3) 0.035(3) -0.010(3) -0.003(3) 0.010(2)
C59 0.034(3) 0.025(3) 0.045(4) -0.004(3) 0.003(3) -0.005(3)
C60 0.017(2) 0.023(3) 0.025(3) -0.006(2) -0.006(2) 0.001(2)
C61 0.023(3) 0.030(3) 0.027(3) -0.005(2) -0.002(2) -0.002(2)
C62 0.024(3) 0.049(4) 0.027(3) -0.013(3) 0.002(2) -0.003(3)
C63 0.028(3) 0.046(4) 0.038(4) -0.025(3) 0.004(3) -0.001(3)
C64 0.026(3) 0.028(3) 0.035(3) -0.017(3) 0.003(3) -0.002(2)
P1 0.0402(13) 0.0212(10) 0.0353(12) -0.0041(9) -0.0155(10) 0.0101(9)
F1 0.085(4) 0.053(3) 0.062(3) -0.019(2) -0.044(3) 0.008(3)
F2 0.048(3) 0.039(2) 0.071(3) -0.005(2) -0.004(2) 0.018(2)
F3 0.058(3) 0.027(2) 0.059(3) 0.0057(19) -0.012(2) 0.0042(19)
P2 0.0745(15) 0.0296(9) 0.0512(12) -0.0143(9) -0.0094(11) -0.0034(10)
F5 0.117(6) 0.058(4) 0.106(5) -0.046(4) 0.028(4) -0.007(4)
F7 0.087(4) 0.046(3) 0.084(4) -0.021(3) -0.012(3) 0.018(3)
N2S 0.079(3) 0.084(3) 0.080(3) -0.0216(19) -0.0221(19) -0.0029(19)
C4S 0.072(3) 0.073(3) 0.072(3) -0.0184(12) -0.0168(12) 0.0001(10)
C5S 0.116(5) 0.118(5) 0.117(5) -0.029(2) -0.026(2) 0.000(2)
N3S 0.082(6) 0.051(5) 0.101(7) -0.025(5) 0.006(5) 0.003(4)
C6S 0.057(5) 0.042(5) 0.063(6) -0.015(4) 0.008(4) -0.002(4)
C7S 0.080(7) 0.052(6) 0.081(7) -0.017(5) 0.000(6) 0.023(5)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 O1 2.026(4) . ?
Ir1 N1 2.079(5) . ?
Ir1 N3 2.027(5) . ?
Ir1 N7 2.051(5) . ?
Ir1 N8 2.045(5) . ?
Ir1 C35 1.952(5) . ?
Ir2 O2 2.029(4) . ?
Ir2 N4 2.029(5) . ?
Ir2 N6 2.079(5) . ?
Ir2 N9 2.055(5) . ?
Ir2 N10 2.053(5) . ?
Ir2 C53 1.947(5) . ?
O1 C1 1.325(7) . ?
O2 C20 1.327(7) . ?
N1 N2 1.387(7) . ?
N1 C11 1.285(8) . ?
N2 C12 1.467(7) . ?
N2 C13 1.354(8) . ?
N3 C13 1.381(7) . ?
N3 C16 1.324(7) . ?
N4 C15 1.383(7) . ?
N4 C16 1.319(7) . ?
N5 N6 1.381(7) . ?
N5 C15 1.351(7) . ?
N5 C17 1.492(16) . ?
N5 C17A 1.497(14) . ?
N6 C18 1.294(7) . ?
N7 C29 1.339(8) . ?
N7 C33 1.387(7) . ?
N8 C42 1.376(7) . ?
N8 C46 1.351(7) . ?
N9 C47 1.336(7) . ?
N9 C51 1.379(7) . ?
N10 C60 1.367(7) . ?
N10 C64 1.347(7) . ?
C1 C2 1.428(7) . ?
C1 C6 1.414(8) . ?
C2 C3 1.412(8) . ?
C2 C11 1.439(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.386(8) . ?
C4 C5 1.411(8) . ?
C4 C7 1.532(9) . ?
C5 H5 0.9500 . ?
C5 C6 1.371(8) . ?
C6 H6 0.9500 . ?
C7 C8 1.532(8) . ?
C7 C9 1.527(9) . ?
C7 C10 1.528(9) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.377(8) . ?
C14 H14 0.9500 . ?
C14 C15 1.385(9) . ?
C16 H16 0.9500 . ?
C17 H17A 0.9601 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C17A H17D 0.9598 . ?
C17A H17E 0.9601 . ?
C17A H17F 0.9601 . ?
C18 H18 0.9500 . ?
C18 C19 1.429(9) . ?
C19 C20 1.428(8) . ?
C19 C24 1.410(8) . ?
C20 C21 1.399(9) . ?
C21 H21 0.9500 . ?
C21 C22 1.361(9) . ?
C22 H22 0.9500 . ?
C22 C23 1.361(10) . ?
C23 C24 1.374(10) . ?
C23 C25 1.541(10) . ?
C24 H24 0.9500 . ?
C25 C26 1.478(15) . ?
C25 C26A 1.52(3) . ?
C25 C27 1.532(16) . ?
C25 C27A 1.53(3) . ?
C25 C28 1.528(17) . ?
C25 C28A 1.46(3) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C26A H26D 0.9800 . ?
C26A H26E 0.9800 . ?
C26A H26F 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C27A H27D 0.9800 . ?
C27A H27E 0.9800 . ?
C27A H27F 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C28A H28D 0.9800 . ?
C28A H28E 0.9800 . ?
C28A H28F 0.9800 . ?
C29 H29 0.9500 . ?
C29 C30 1.380(8) . ?
C30 H30 0.9500 . ?
C30 C31 1.393(10) . ?
C31 H31 0.9500 . ?
C31 C32 1.358(10) . ?
C32 H32 0.9500 . ?
C32 C33 1.388(8) . ?
C33 C34 1.469(9) . ?
C34 C35 1.404(8) . ?
C34 C39 1.404(8) . ?
C35 C36 1.398(8) . ?
C36 C37 1.410(8) . ?
C36 C42 1.473(8) . ?
C37 C38 1.391(10) . ?
C37 C41 1.519(10) . ?
C38 H38 0.9500 . ?
C38 C39 1.394(10) . ?
C39 C40 1.515(9) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.392(8) . ?
C43 H43 0.9500 . ?
C43 C44 1.388(10) . ?
C44 H44 0.9500 . ?
C44 C45 1.368(10) . ?
C45 H45 0.9500 . ?
C45 C46 1.380(9) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C47 C48 1.391(9) . ?
C48 H48 0.9500 . ?
C48 C49 1.369(9) . ?
C49 H49 0.9500 . ?
C49 C50 1.385(9) . ?
C50 H50 0.9500 . ?
C50 C51 1.384(8) . ?
C51 C52 1.475(7) . ?
C52 C53 1.404(7) . ?
C52 C57 1.405(8) . ?
C53 C54 1.404(7) . ?
C54 C55 1.405(8) . ?
C54 C60 1.482(7) . ?
C55 C56 1.393(8) . ?
C55 C59 1.516(8) . ?
C56 H56 0.9500 . ?
C56 C57 1.406(8) . ?
C57 C58 1.499(8) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 C61 1.389(8) . ?
C61 H61 0.9500 . ?
C61 C62 1.384(9) . ?
C62 H62 0.9500 . ?
C62 C63 1.387(10) . ?
C63 H63 0.9500 . ?
C63 C64 1.373(9) . ?
C64 H64 0.9500 . ?
P1 F1 1.593(5) 2_775 ?
P1 F1 1.593(5) . ?
P1 F2 1.589(4) 2_775 ?
P1 F2 1.589(4) . ?
P1 F3 1.597(4) . ?
P1 F3 1.597(4) 2_775 ?
P2 F4 1.592(5) . ?
P2 F4A 1.593(5) . ?
P2 F5 1.576(6) . ?
P2 F6 1.591(5) . ?
P2 F6A 1.590(5) . ?
P2 F7 1.605(6) . ?
P2 F8 1.597(5) . ?
P2 F8A 1.597(5) . ?
P2 F9 1.593(5) . ?
P2 F9A 1.593(5) . ?
O1S H1S 0.8202 . ?
O1S C10S 1.44(2) . ?
C10S H10D 0.9602 . ?
C10S H10E 0.9600 . ?
C10S H10F 0.9601 . ?
N1S C2S 1.092(8) . ?
C2S C3S 1.420(9) . ?
C3S H3SA 0.9601 . ?
C3S H3SB 0.9599 . ?
C3S H3SC 0.9599 . ?
N2S C4S 1.095(8) . ?
C4S C5S 1.422(9) . ?
C5S H5SA 0.9598 . ?
C5S H5SB 0.9600 . ?
C5S H5SC 0.9601 . ?
N3S C6S 1.098(8) . ?
C6S C7S 1.424(9) . ?
C7S H7SA 0.9598 . ?
C7S H7SB 0.9600 . ?
C7S H7SC 0.9600 . ?
N4S C8S 1.096(8) . ?
C8S C9S 1.423(9) . ?
C9S H9SA 0.9601 . ?
C9S H9SB 0.9601 . ?
C9S H9SC 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ir1 N1 93.31(17) . . ?
O1 Ir1 N3 171.58(17) . . ?
O1 Ir1 N7 89.55(18) . . ?
O1 Ir1 N8 89.76(17) . . ?
N3 Ir1 N1 78.51(19) . . ?
N3 Ir1 N7 90.17(18) . . ?
N3 Ir1 N8 93.25(18) . . ?
N7 Ir1 N1 101.68(19) . . ?
N8 Ir1 N1 97.45(19) . . ?
N8 Ir1 N7 160.87(19) . . ?
C35 Ir1 O1 90.10(19) . . ?
C35 Ir1 N1 176.0(2) . . ?
C35 Ir1 N3 98.1(2) . . ?
C35 Ir1 N7 80.4(2) . . ?
C35 Ir1 N8 80.5(2) . . ?
O2 Ir2 N6 93.17(18) . . ?
O2 Ir2 N9 89.62(18) . . ?
O2 Ir2 N10 88.76(17) . . ?
N4 Ir2 O2 171.44(17) . . ?
N4 Ir2 N6 78.31(19) . . ?
N4 Ir2 N9 91.27(19) . . ?
N4 Ir2 N10 93.22(18) . . ?
N9 Ir2 N6 101.53(19) . . ?
N10 Ir2 N6 98.04(19) . . ?
N10 Ir2 N9 160.42(18) . . ?
C53 Ir2 O2 87.39(19) . . ?
C53 Ir2 N4 101.15(19) . . ?
C53 Ir2 N6 178.2(2) . . ?
C53 Ir2 N9 80.2(2) . . ?
C53 Ir2 N10 80.2(2) . . ?
C1 O1 Ir1 122.0(3) . . ?
C20 O2 Ir2 122.2(4) . . ?
N2 N1 Ir1 113.1(4) . . ?
C11 N1 Ir1 125.8(4) . . ?
C11 N1 N2 121.0(5) . . ?
N1 N2 C12 120.1(5) . . ?
C13 N2 N1 115.6(4) . . ?
C13 N2 C12 124.1(5) . . ?
C13 N3 Ir1 114.4(4) . . ?
C16 N3 Ir1 127.4(4) . . ?
C16 N3 C13 117.9(5) . . ?
C15 N4 Ir2 114.6(4) . . ?
C16 N4 Ir2 128.1(4) . . ?
C16 N4 C15 117.2(5) . . ?
N6 N5 C17 119.5(7) . . ?
N6 N5 C17A 119.6(7) . . ?
C15 N5 N6 116.1(5) . . ?
C15 N5 C17 122.5(8) . . ?
C15 N5 C17A 123.1(7) . . ?
N5 N6 Ir2 113.6(3) . . ?
C18 N6 Ir2 126.0(5) . . ?
C18 N6 N5 120.3(5) . . ?
C29 N7 Ir1 125.0(4) . . ?
C29 N7 C33 120.2(5) . . ?
C33 N7 Ir1 114.7(4) . . ?
C42 N8 Ir1 114.5(4) . . ?
C46 N8 Ir1 125.2(4) . . ?
C46 N8 C42 120.3(5) . . ?
C47 N9 Ir2 125.4(4) . . ?
C47 N9 C51 120.1(5) . . ?
C51 N9 Ir2 114.4(4) . . ?
C60 N10 Ir2 114.9(3) . . ?
C64 N10 Ir2 125.0(4) . . ?
C64 N10 C60 120.0(5) . . ?
O1 C1 C2 128.3(5) . . ?
O1 C1 C6 116.0(5) . . ?
C6 C1 C2 115.6(5) . . ?
C1 C2 C11 126.4(6) . . ?
C3 C2 C1 119.3(5) . . ?
C3 C2 C11 114.3(5) . . ?
C2 C3 H3 117.9 . . ?
C4 C3 C2 124.3(5) . . ?
C4 C3 H3 117.9 . . ?
C3 C4 C5 115.6(5) . . ?
C3 C4 C7 120.2(5) . . ?
C5 C4 C7 124.1(5) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 C4 121.6(5) . . ?
C6 C5 H5 119.2 . . ?
C1 C6 H6 118.2 . . ?
C5 C6 C1 123.5(5) . . ?
C5 C6 H6 118.2 . . ?
C8 C7 C4 108.5(5) . . ?
C9 C7 C4 109.5(5) . . ?
C9 C7 C8 109.6(6) . . ?
C9 C7 C10 108.6(6) . . ?
C10 C7 C4 112.1(5) . . ?
C10 C7 C8 108.6(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C2 123.9(5) . . ?
N1 C11 H11 118.0 . . ?
C2 C11 H11 118.0 . . ?
N2 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
N2 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 N3 117.4(5) . . ?
N2 C13 C14 122.8(5) . . ?
C14 C13 N3 119.8(5) . . ?
C13 C14 H14 120.6 . . ?
C13 C14 C15 118.9(5) . . ?
C15 C14 H14 120.6 . . ?
N4 C15 C14 120.3(5) . . ?
N5 C15 N4 117.4(5) . . ?
N5 C15 C14 122.3(5) . . ?
N3 C16 H16 117.1 . . ?
N4 C16 N3 125.8(5) . . ?
N4 C16 H16 117.1 . . ?
N5 C17 H17A 109.5 . . ?
N5 C17 H17B 109.5 . . ?
N5 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N5 C17A H17D 109.5 . . ?
N5 C17A H17E 109.5 . . ?
N5 C17A H17F 109.5 . . ?
H17D C17A H17E 109.5 . . ?
H17D C17A H17F 109.5 . . ?
H17E C17A H17F 109.5 . . ?
N6 C18 H18 118.3 . . ?
N6 C18 C19 123.3(6) . . ?
C19 C18 H18 118.3 . . ?
C20 C19 C18 127.3(5) . . ?
C24 C19 C18 112.9(6) . . ?
C24 C19 C20 119.8(6) . . ?
O2 C20 C19 127.9(5) . . ?
O2 C20 C21 116.0(5) . . ?
C21 C20 C19 116.1(5) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 C20 120.0(6) . . ?
C22 C21 H21 120.0 . . ?
C21 C22 H22 116.8 . . ?
C21 C22 C23 126.5(6) . . ?
C23 C22 H22 116.8 . . ?
C22 C23 C24 114.5(6) . . ?
C22 C23 C25 125.1(7) . . ?
C24 C23 C25 120.4(7) . . ?
C19 C24 H24 118.4 . . ?
C23 C24 C19 123.2(7) . . ?
C23 C24 H24 118.4 . . ?
C26 C25 C23 108.0(8) . . ?
C26 C25 C27 110.2(9) . . ?
C26 C25 C28 112.4(10) . . ?
C26A C25 C23 114.6(15) . . ?
C26A C25 C27A 102.0(19) . . ?
C27 C25 C23 110.1(8) . . ?
C27A C25 C23 108.1(13) . . ?
C28 C25 C23 108.0(9) . . ?
C28 C25 C27 108.1(9) . . ?
C28A C25 C23 111.9(13) . . ?
C28A C25 C26A 113.8(19) . . ?
C28A C25 C27A 105.3(18) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C26A H26D 109.5 . . ?
C25 C26A H26E 109.5 . . ?
C25 C26A H26F 109.5 . . ?
H26D C26A H26E 109.5 . . ?
H26D C26A H26F 109.5 . . ?
H26E C26A H26F 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C27A H27D 109.5 . . ?
C25 C27A H27E 109.5 . . ?
C25 C27A H27F 109.5 . . ?
H27D C27A H27E 109.5 . . ?
H27D C27A H27F 109.5 . . ?
H27E C27A H27F 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C25 C28A H28D 109.5 . . ?
C25 C28A H28E 109.5 . . ?
C25 C28A H28F 109.5 . . ?
H28D C28A H28E 109.5 . . ?
H28D C28A H28F 109.5 . . ?
H28E C28A H28F 109.5 . . ?
N7 C29 H29 118.7 . . ?
N7 C29 C30 122.5(6) . . ?
C30 C29 H29 118.7 . . ?
C29 C30 H30 121.1 . . ?
C29 C30 C31 117.8(6) . . ?
C31 C30 H30 121.1 . . ?
C30 C31 H31 120.0 . . ?
C32 C31 C30 119.9(6) . . ?
C32 C31 H31 120.0 . . ?
C31 C32 H32 119.2 . . ?
C31 C32 C33 121.6(6) . . ?
C33 C32 H32 119.2 . . ?
N7 C33 C32 118.0(6) . . ?
N7 C33 C34 113.9(5) . . ?
C32 C33 C34 128.1(5) . . ?
C35 C34 C33 113.1(5) . . ?
C39 C34 C33 129.0(6) . . ?
C39 C34 C35 117.8(6) . . ?
C34 C35 Ir1 117.8(4) . . ?
C36 C35 Ir1 117.7(4) . . ?
C36 C35 C34 124.5(5) . . ?
C35 C36 C37 117.2(6) . . ?
C35 C36 C42 112.9(5) . . ?
C37 C36 C42 130.0(6) . . ?
C36 C37 C41 123.5(7) . . ?
C38 C37 C36 118.0(6) . . ?
C38 C37 C41 118.5(6) . . ?
C37 C38 H38 117.5 . . ?
C37 C38 C39 125.0(6) . . ?
C39 C38 H38 117.5 . . ?
C34 C39 C40 124.7(7) . . ?
C38 C39 C34 117.4(6) . . ?
C38 C39 C40 117.9(6) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C37 C41 H41A 109.5 . . ?
C37 C41 H41B 109.5 . . ?
C37 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N8 C42 C36 114.3(5) . . ?
N8 C42 C43 118.5(6) . . ?
C43 C42 C36 127.3(6) . . ?
C42 C43 H43 119.6 . . ?
C44 C43 C42 120.7(6) . . ?
C44 C43 H43 119.6 . . ?
C43 C44 H44 120.2 . . ?
C45 C44 C43 119.7(6) . . ?
C45 C44 H44 120.2 . . ?
C44 C45 H45 120.6 . . ?
C44 C45 C46 118.8(6) . . ?
C46 C45 H45 120.6 . . ?
N8 C46 C45 122.0(6) . . ?
N8 C46 H46 119.0 . . ?
C45 C46 H46 119.0 . . ?
N9 C47 H47 119.0 . . ?
N9 C47 C48 121.9(6) . . ?
C48 C47 H47 119.0 . . ?
C47 C48 H48 120.5 . . ?
C49 C48 C47 118.9(6) . . ?
C49 C48 H48 120.5 . . ?
C48 C49 H49 120.4 . . ?
C48 C49 C50 119.3(6) . . ?
C50 C49 H49 120.4 . . ?
C49 C50 H50 119.6 . . ?
C51 C50 C49 120.8(6) . . ?
C51 C50 H50 119.6 . . ?
N9 C51 C50 118.9(5) . . ?
N9 C51 C52 114.5(5) . . ?
C50 C51 C52 126.6(5) . . ?
C53 C52 C51 112.1(5) . . ?
C53 C52 C57 118.9(5) . . ?
C57 C52 C51 129.0(5) . . ?
C52 C53 Ir2 118.3(4) . . ?
C54 C53 Ir2 118.2(4) . . ?
C54 C53 C52 123.1(5) . . ?
C53 C54 C55 118.2(5) . . ?
C53 C54 C60 112.2(5) . . ?
C55 C54 C60 129.6(5) . . ?
C54 C55 C59 124.8(5) . . ?
C56 C55 C54 117.6(5) . . ?
C56 C55 C59 117.6(5) . . ?
C55 C56 H56 117.6 . . ?
C55 C56 C57 124.8(5) . . ?
C57 C56 H56 117.6 . . ?
C52 C57 C56 116.7(5) . . ?
C52 C57 C58 124.9(5) . . ?
C56 C57 C58 118.1(5) . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C55 C59 H59A 109.5 . . ?
C55 C59 H59B 109.5 . . ?
C55 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
N10 C60 C54 114.3(5) . . ?
N10 C60 C61 119.1(5) . . ?
C61 C60 C54 126.5(5) . . ?
C60 C61 H61 119.6 . . ?
C62 C61 C60 120.8(6) . . ?
C62 C61 H61 119.6 . . ?
C61 C62 H62 120.5 . . ?
C61 C62 C63 118.9(6) . . ?
C63 C62 H62 120.5 . . ?
C62 C63 H63 120.7 . . ?
C64 C63 C62 118.6(6) . . ?
C64 C63 H63 120.7 . . ?
N10 C64 C63 122.5(6) . . ?
N10 C64 H64 118.8 . . ?
C63 C64 H64 118.8 . . ?
F1 P1 F1 180.0 2_775 . ?
F1 P1 F3 89.6(3) . . ?
F1 P1 F3 89.6(3) 2_775 2_775 ?
F1 P1 F3 90.4(3) . 2_775 ?
F1 P1 F3 90.4(3) 2_775 . ?
F2 P1 F1 89.9(3) . . ?
F2 P1 F1 89.9(3) 2_775 2_775 ?
F2 P1 F1 90.1(3) . 2_775 ?
F2 P1 F1 90.1(3) 2_775 . ?
F2 P1 F2 180.0 . 2_775 ?
F2 P1 F3 90.9(2) . . ?
F2 P1 F3 89.1(2) 2_775 . ?
F2 P1 F3 89.1(2) . 2_775 ?
F2 P1 F3 90.9(2) 2_775 2_775 ?
F3 P1 F3 180.0 2_775 . ?
F4 P2 F7 86.4(5) . . ?
F4 P2 F8 87.3(8) . . ?
F4 P2 F9 175.9(7) . . ?
F4A P2 F7 92.1(5) . . ?
F4A P2 F8A 88.3(7) . . ?
F4A P2 F9A 176.7(7) . . ?
F5 P2 F4 95.3(5) . . ?
F5 P2 F4A 89.4(5) . . ?
F5 P2 F6 96.8(7) . . ?
F5 P2 F6A 86.2(7) . . ?
F5 P2 F7 178.3(4) . . ?
F5 P2 F8 87.4(7) . . ?
F5 P2 F8A 90.6(6) . . ?
F5 P2 F9 87.0(5) . . ?
F5 P2 F9A 93.1(6) . . ?
F6 P2 F4 94.1(8) . . ?
F6 P2 F7 83.3(7) . . ?
F6 P2 F8 175.5(9) . . ?
F6 P2 F9 89.0(8) . . ?
F6A P2 F4A 87.0(8) . . ?
F6A P2 F7 94.7(7) . . ?
F6A P2 F8A 174.3(9) . . ?
F6A P2 F9A 91.0(8) . . ?
F8 P2 F7 92.6(7) . . ?
F8A P2 F7 88.6(6) . . ?
F9 P2 F7 91.3(5) . . ?
F9 P2 F8 89.4(9) . . ?
F9A P2 F7 85.4(5) . . ?
F9A P2 F8A 93.9(8) . . ?
C10S O1S H1S 107.1 . . ?
O1S C10S H10D 105.9 . . ?
O1S C10S H10E 109.4 . . ?
O1S C10S H10F 113.1 . . ?
H10D C10S H10E 109.5 . . ?
H10D C10S H10F 109.5 . . ?
H10E C10S H10F 109.5 . . ?
N1S C2S C3S 174.4(18) . . ?
C2S C3S H3SA 113.7 . . ?
C2S C3S H3SB 104.6 . . ?
C2S C3S H3SC 109.9 . . ?
H3SA C3S H3SB 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?
N2S C4S C5S 177.6(15) . . ?
C4S C5S H5SA 109.4 . . ?
C4S C5S H5SB 109.9 . . ?
C4S C5S H5SC 109.1 . . ?
H5SA C5S H5SB 109.5 . . ?
H5SA C5S H5SC 109.5 . . ?
H5SB C5S H5SC 109.5 . . ?
N3S C6S C7S 178.3(13) . . ?
C6S C7S H7SA 109.4 . . ?
C6S C7S H7SB 109.5 . . ?
C6S C7S H7SC 109.5 . . ?
H7SA C7S H7SB 109.5 . . ?
H7SA C7S H7SC 109.5 . . ?
H7SB C7S H7SC 109.5 . . ?
N4S C8S C9S 166(2) . . ?
C8S C9S H9SA 109.4 . . ?
C8S C9S H9SB 109.7 . . ?
C8S C9S H9SC 109.3 . . ?
H9SA C9S H9SB 109.5 . . ?
H9SA C9S H9SC 109.5 . . ?
H9SB C9S H9SC 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 C13 N2 N1 -9.9(8) . . . . ?
N4 C15 N5 N6 -0.2(9) . . . . ?
C1 C2 C11 N1 3.6(9) . . . . ?
C2 C11 N1 Ir1 -3.4(8) . . . . ?
C2 C11 N1 N2 -178.7(5) . . . . ?
C3 C2 C11 N1 -178.4(5) . . . . ?
C3 C4 C7 C8 -58.5(7) . . . . ?
C3 C4 C7 C9 61.1(7) . . . . ?
C3 C4 C7 C10 -178.3(5) . . . . ?
C5 C4 C7 C8 119.3(6) . . . . ?
C5 C4 C7 C9 -121.2(6) . . . . ?
C5 C4 C7 C10 -0.6(8) . . . . ?
C11 N1 N2 C12 0.9(8) . . . . ?
C11 N1 N2 C13 -173.5(5) . . . . ?
C12 N2 N1 Ir1 -175.0(4) . . . . ?
C12 N2 C13 N3 176.0(5) . . . . ?
C13 N2 N1 Ir1 10.7(6) . . . . ?
C14 C13 N2 N1 170.3(5) . . . . ?
C14 C13 N2 C12 -3.8(9) . . . . ?
C14 C15 N5 N6 -179.3(6) . . . . ?
C14 C15 N5 C17 16.6(12) . . . . ?
C14 C15 N5 C17A -11.9(12) . . . . ?
C15 N5 N6 Ir2 -0.6(7) . . . . ?
C15 N5 N6 C18 -177.8(6) . . . . ?
C17 N5 N6 Ir2 164.1(8) . . . . ?
C17 N5 N6 C18 -13.1(11) . . . . ?
C17 N5 C15 N4 -164.3(9) . . . . ?
C17A N5 N6 Ir2 -168.4(7) . . . . ?
C17A N5 N6 C18 14.4(10) . . . . ?
C17A N5 C15 N4 167.2(8) . . . . ?
C19 C18 N6 Ir2 1.5(9) . . . . ?
C19 C18 N6 N5 178.3(6) . . . . ?
C20 C19 C18 N6 0.7(10) . . . . ?
C22 C23 C25 C26 119.2(10) . . . . ?
C22 C23 C25 C26A 172.9(17) . . . . ?
C22 C23 C25 C27 -1.2(12) . . . . ?
C22 C23 C25 C27A 60.0(16) . . . . ?
C22 C23 C25 C28 -119.1(10) . . . . ?
C22 C23 C25 C28A -55.5(17) . . . . ?
C24 C19 C18 N6 -178.3(6) . . . . ?
C24 C23 C25 C26 -61.8(11) . . . . ?
C24 C23 C25 C26A -8.1(19) . . . . ?
C24 C23 C25 C27 177.8(8) . . . . ?
C24 C23 C25 C27A -121.0(14) . . . . ?
C24 C23 C25 C28 59.9(11) . . . . ?
C24 C23 C25 C28A 123.5(15) . . . . ?
C32 C33 C34 C35 -175.1(6) . . . . ?
C32 C33 C34 C39 5.4(10) . . . . ?
C35 C34 C33 N7 2.7(7) . . . . ?
C35 C36 C42 N8 -4.4(7) . . . . ?
C35 C36 C42 C43 177.7(6) . . . . ?
C37 C36 C42 N8 174.6(6) . . . . ?
C37 C36 C42 C43 -3.3(11) . . . . ?
C39 C34 C33 N7 -176.8(6) . . . . ?
C50 C51 C52 C53 -169.0(5) . . . . ?
C50 C51 C52 C57 12.6(10) . . . . ?
C53 C52 C51 N9 7.2(7) . . . . ?
C53 C54 C60 N10 3.4(7) . . . . ?
C53 C54 C60 C61 -174.1(5) . . . . ?
C55 C54 C60 N10 -179.9(6) . . . . ?
C55 C54 C60 C61 2.6(10) . . . . ?
C57 C52 C51 N9 -171.2(5) . . . . ?
_smtbx_masks_special_details ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.000 0.000 620.6 140.1 ?
_iucr_refine_instructions_details
;
TITL 16srv324 in P-1 #2
REM reset to P-1 #2
CELL 0.71073 12.2674 16.3422 21.2271 75.235 76.5822 87.4928
ZERR 1 0.0011 0.0015 0.002 0.0034 0.0034 0.0032
LATT 1
SFAC C H F Ir N O P
UNIT 141 150 18 4 26 5 3
SADI 0.005 P2 F6A P2 F4 P2 F4A P2 F8 P2 F8A P2 F9 P2 F9A P2 F6
SADI 0.005 N1S C2S N2S C4S N3S C6S N4S C8S
SADI 0.005 C3S C2S C5S C4S C7S C6S C9S C8S
ISOR 0.002 0.005 C22
ISOR 0.001 0.002 C5S C4S N2S
L.S. 9
PLAN 9
SIZE 0.06 0.15 0.16
TEMP -153.15
CONF C3 C4 C7 C8
CONF C5 C4 C7 C8
CONF C3 C4 C7 C9
CONF C5 C4 C7 C9
CONF C3 C4 C7 C10
CONF C5 C4 C7 C10
CONF C1 C2 C11 N1
CONF C3 C2 C11 N1
CONF C2 C11 N1 Ir1
CONF C2 C11 N1 N2
CONF C12 N2 N1 Ir1
CONF C11 N1 N2 C12
CONF C13 N2 N1 Ir1
CONF C11 N1 N2 C13
CONF N3 C13 N2 N1
CONF C14 C13 N2 N1
CONF C12 N2 C13 N3
CONF C14 C13 N2 C12
CONF N4 C15 N5 N6
CONF C14 C15 N5 N6
CONF C17 N5 C15 N4
CONF C14 C15 N5 C17
CONF C17A N5 C15 N4
CONF C14 C15 N5 C17A
CONF C15 N5 N6 Ir2
CONF C17 N5 N6 Ir2
CONF C17A N5 N6 Ir2
CONF C15 N5 N6 C18
CONF C17 N5 N6 C18
CONF C17A N5 N6 C18
CONF C19 C18 N6 Ir2
CONF C19 C18 N6 N5
CONF C20 C19 C18 N6
CONF C24 C19 C18 N6
CONF C22 C23 C25 C26
CONF C24 C23 C25 C26
CONF C22 C23 C25 C26A
CONF C24 C23 C25 C26A
CONF C22 C23 C25 C27
CONF C24 C23 C25 C27
CONF C22 C23 C25 C27A
CONF C24 C23 C25 C27A
CONF C22 C23 C25 C28
CONF C24 C23 C25 C28
CONF C22 C23 C25 C28A
CONF C24 C23 C25 C28A
CONF C35 C36 C42 N8
CONF C37 C36 C42 N8
CONF C35 C36 C42 C43
CONF C37 C36 C42 C43
CONF C35 C34 C33 N7
CONF C32 C33 C34 C35
CONF C39 C34 C33 N7
CONF C32 C33 C34 C39
CONF C53 C54 C60 N10
CONF C55 C54 C60 N10
CONF C53 C54 C60 C61
CONF C55 C54 C60 C61
CONF C53 C52 C51 N9
CONF C50 C51 C52 C53
CONF C57 C52 C51 N9
CONF C50 C51 C52 C57
BOND $h
ABIN
fmap 2
acta
OMIT -2 58
OMIT 1 1 1
OMIT 1 1 0
OMIT 0 0 2
OMIT -1 1 2
OMIT -1 1 0
OMIT -1 -1 2
WGHT 0.023 45.68
FVAR 0.25487
REM
REM
REM
Ir1 4 0.28441 0.60850 0.13055 11.00000 0.01442 0.01218 0.02866 =
-0.00762 -0.00180 0.00156
Ir2 4 0.58523 0.65642 0.30615 11.00000 0.01696 0.01608 0.02362 =
-0.00893 -0.00069 -0.00227
O1 6 0.21293 0.55931 0.07104 11.00000 0.02077 0.01681 0.03344 =
-0.01130 -0.00571 0.00008
O2 6 0.70105 0.63822 0.36264 11.00000 0.02623 0.02765 0.02364 =
-0.00952 -0.00294 -0.00573
N1 5 0.22930 0.73004 0.09520 11.00000 0.01796 0.01489 0.03494 =
-0.00883 -0.00273 0.00184
N2 5 0.25484 0.78729 0.12815 11.00000 0.02472 0.01486 0.04010 =
-0.01072 -0.00799 0.00650
N3 5 0.35180 0.67452 0.18155 11.00000 0.01607 0.01494 0.03134 =
-0.00829 -0.00233 0.00212
N4 5 0.47223 0.69329 0.24857 11.00000 0.01605 0.01603 0.02764 =
-0.00839 -0.00209 0.00051
N5 5 0.50279 0.82708 0.26238 11.00000 0.03726 0.01810 0.06639 =
-0.02232 -0.02527 0.00567
N6 5 0.57695 0.78566 0.29933 11.00000 0.02503 0.02176 0.03263 =
-0.01304 -0.00296 -0.00445
N7 5 0.43718 0.60903 0.06570 11.00000 0.01665 0.02019 0.03474 =
-0.01277 0.00048 0.00191
N8 5 0.14884 0.56827 0.20810 11.00000 0.01722 0.02248 0.02678 =
-0.00773 -0.00250 -0.00312
N9 5 0.70991 0.65227 0.22358 11.00000 0.01856 0.01988 0.02625 =
-0.00657 -0.00044 0.00030
N10 5 0.46329 0.61688 0.39233 11.00000 0.01879 0.02427 0.02185 =
-0.01139 -0.00105 0.00011
C1 1 0.16189 0.60729 0.02649 11.00000 0.01353 0.01846 0.02963 =
-0.00546 0.00491 -0.00105
C2 1 0.13955 0.69567 0.01558 11.00000 0.01474 0.02087 0.03389 =
-0.01035 0.00177 -0.00057
C3 1 0.07787 0.73397 -0.03242 11.00000 0.01644 0.01983 0.03517 =
-0.00787 0.00206 0.00244
AFIX 43
H3 2 0.06386 0.79281 -0.03882 11.00000 -1.20000
AFIX 0
C4 1 0.03642 0.69130 -0.07082 11.00000 0.01709 0.02554 0.02457 =
-0.00389 0.00392 -0.00005
C5 1 0.06100 0.60440 -0.06015 11.00000 0.01163 0.03015 0.02743 =
-0.00879 0.00013 -0.00559
AFIX 43
H5 2 0.03501 0.57213 -0.08532 11.00000 -1.20000
AFIX 0
C6 1 0.12146 0.56533 -0.01435 11.00000 0.01754 0.02078 0.02983 =
-0.00711 0.00542 -0.00239
AFIX 43
H6 2 0.13704 0.50692 -0.00980 11.00000 -1.20000
AFIX 0
C7 1 -0.03456 0.73782 -0.11916 11.00000 0.02168 0.03316 0.03271 =
-0.01031 -0.00041 0.00157
C8 1 -0.13723 0.77367 -0.07901 11.00000 0.02551 0.05220 0.05429 =
-0.02934 -0.01343 0.01267
AFIX 137
H8a 2 -0.18021 0.72738 -0.04449 11.00000 -1.50000
H8b 2 -0.18447 0.80254 -0.10909 11.00000 -1.50000
H8c 2 -0.11266 0.81401 -0.05779 11.00000 -1.50000
AFIX 0
C9 1 0.03463 0.81012 -0.17149 11.00000 0.03402 0.03338 0.05056 =
0.00058 -0.01104 0.00257
AFIX 137
H9a 2 0.05638 0.85044 -0.14926 11.00000 -1.50000
H9b 2 -0.01013 0.83896 -0.20307 11.00000 -1.50000
H9c 2 0.10206 0.78735 -0.19572 11.00000 -1.50000
AFIX 0
C10 1 -0.07480 0.67923 -0.15516 11.00000 0.02694 0.03959 0.03397 =
-0.01339 -0.00471 0.00203
AFIX 137
H10a 2 -0.01014 0.65980 -0.18418 11.00000 -1.50000
H10b 2 -0.12535 0.70999 -0.18231 11.00000 -1.50000
H10c 2 -0.11471 0.63031 -0.12208 11.00000 -1.50000
AFIX 0
C11 1 0.17101 0.75211 0.05072 11.00000 0.01858 0.01735 0.03653 =
-0.00872 0.00115 0.00345
AFIX 43
H11 2 0.14724 0.80910 0.04040 11.00000 -1.20000
AFIX 0
C12 1 0.21391 0.87417 0.11313 11.00000 0.04330 0.01690 0.04979 =
-0.01343 -0.01637 0.01114
AFIX 137
H12a 2 0.22516 0.90218 0.14688 11.00000 -1.50000
H12b 2 0.13389 0.87303 0.11368 11.00000 -1.50000
H12c 2 0.25535 0.90536 0.06878 11.00000 -1.50000
AFIX 0
C13 1 0.32615 0.75944 0.16883 11.00000 0.02016 0.01458 0.03427 =
-0.00822 -0.00243 0.00278
C14 1 0.37266 0.81186 0.19741 11.00000 0.03146 0.01403 0.04463 =
-0.00990 -0.01006 0.00525
AFIX 43
H14 2 0.35311 0.86984 0.19067 11.00000 -1.20000
AFIX 0
C15 1 0.44843 0.77863 0.23616 11.00000 0.02503 0.01648 0.03910 =
-0.01342 -0.00620 -0.00031
C16 1 0.42311 0.64691 0.22024 11.00000 0.01906 0.01249 0.02956 =
-0.00929 -0.00105 -0.00112
AFIX 43
H16 2 0.44044 0.58846 0.22831 11.00000 -1.20000
AFIX 0
PART 1
C17 1 0.46543 0.91370 0.26764 10.50000 0.03953
AFIX 3
H17a 2 0.45326 0.94598 0.22531 10.50000 -1.50000
H17b 2 0.52209 0.94122 0.27979 10.50000 -1.50000
H17c 2 0.39690 0.90962 0.30121 10.50000 -1.50000
AFIX 0
PART 0
PART 2
C17A 1 0.50356 0.92181 0.24206 10.50000 0.02910
AFIX 3
H17d 2 0.46857 0.94062 0.20495 10.50000 -1.50000
H17e 2 0.46310 0.94286 0.27901 10.50000 -1.50000
H17f 2 0.57953 0.94270 0.22921 10.50000 -1.50000
AFIX 0
PART 0
C18 1 0.63007 0.82656 0.32811 11.00000 0.03043 0.02727 0.03106 =
-0.01505 -0.00103 -0.00837
AFIX 43
H18 2 0.61817 0.88561 0.32209 11.00000 -1.20000
AFIX 0
C19 1 0.70571 0.78738 0.36847 11.00000 0.02908 0.02909 0.02561 =
-0.01162 -0.00143 -0.00871
C20 1 0.73619 0.70039 0.38322 11.00000 0.02949 0.02453 0.01840 =
-0.00719 -0.00285 -0.00621
C21 1 0.81244 0.67791 0.42435 11.00000 0.03656 0.03477 0.02950 =
-0.00587 -0.00959 -0.00996
AFIX 43
H21 2 0.83707 0.62119 0.43520 11.00000 -1.20000
AFIX 0
C22 1 0.85129 0.73733 0.44880 11.00000 0.03331 0.03416 0.02858 =
0.00007 -0.01748 0.00285
AFIX 43
H22 2 0.90186 0.71870 0.47714 11.00000 -1.20000
AFIX 0
C23 1 0.82494 0.82078 0.43672 11.00000 0.05569 0.03735 0.03505 =
-0.00933 -0.01189 -0.02053
C24 1 0.75084 0.84435 0.39599 11.00000 0.05283 0.02941 0.02983 =
-0.01060 -0.01542 -0.01087
AFIX 43
H24 2 0.72894 0.90183 0.38588 11.00000 -1.20000
AFIX 0
C25 1 0.87002 0.88629 0.46566 11.00000 0.06772 0.04353 0.04476 =
-0.01472 -0.02387 -0.01003
PART 1
C26 1 0.93269 0.95239 0.40905 10.60000 0.04630
AFIX 137
H26a 2 0.99088 0.92598 0.38085 10.60000 -1.50000
H26b 2 0.96764 0.99225 0.42627 10.60000 -1.50000
H26c 2 0.88110 0.98276 0.38248 10.60000 -1.50000
AFIX 0
PART 0
PART 2
C26A 1 0.83883 0.97749 0.43774 10.40000 0.10059
AFIX 137
H26d 2 0.85979 1.01361 0.46362 10.40000 -1.50000
H26e 2 0.75785 0.98055 0.44088 10.40000 -1.50000
H26f 2 0.87879 0.99694 0.39078 10.40000 -1.50000
AFIX 0
PART 0
PART 1
C27 1 0.94710 0.84344 0.51139 10.60000 0.04796
AFIX 137
H27a 2 1.01209 0.82047 0.48518 10.60000 -1.50000
H27b 2 0.90594 0.79740 0.54709 10.60000 -1.50000
H27c 2 0.97257 0.88504 0.53115 10.60000 -1.50000
AFIX 0
PART 0
PART 2
C27A 1 0.99772 0.88996 0.44216 10.40000 0.08232
AFIX 137
H27d 2 1.01872 0.91017 0.39329 10.40000 -1.50000
H27e 2 1.02776 0.83331 0.45589 10.40000 -1.50000
H27f 2 1.02854 0.92877 0.46224 10.40000 -1.50000
AFIX 0
PART 0
PART 1
C28 1 0.77013 0.92179 0.50791 10.60000 0.05740
AFIX 137
H28a 2 0.79702 0.96202 0.52836 10.60000 -1.50000
H28b 2 0.72873 0.87538 0.54311 10.60000 -1.50000
H28c 2 0.72059 0.95074 0.47935 10.60000 -1.50000
AFIX 0
PART 0
PART 2
C28A 1 0.84749 0.86044 0.53876 10.40000 0.08054
AFIX 137
H28d 2 0.88198 0.80563 0.55293 10.40000 -1.50000
H28e 2 0.76636 0.85549 0.55718 10.40000 -1.50000
H28f 2 0.87905 0.90287 0.55514 10.40000 -1.50000
AFIX 0
PART 0
C29 1 0.47789 0.67228 0.01218 11.00000 0.01997 0.02208 0.04056 =
-0.00814 -0.00305 0.00065
AFIX 43
H29 2 0.43564 0.72244 0.00413 11.00000 -1.20000
AFIX 0
C30 1 0.57893 0.66739 -0.03174 11.00000 0.02790 0.03444 0.03729 =
-0.00985 0.00537 -0.00668
AFIX 43
H30 2 0.60671 0.71332 -0.06912 11.00000 -1.20000
AFIX 0
C31 1 0.63877 0.59285 -0.01942 11.00000 0.01724 0.04187 0.04840 =
-0.02508 0.00249 -0.00333
AFIX 43
H31 2 0.70752 0.58661 -0.04936 11.00000 -1.20000
AFIX 0
C32 1 0.59875 0.52912 0.03544 11.00000 0.01838 0.03076 0.05326 =
-0.02191 -0.00259 0.00218
AFIX 43
H32 2 0.64105 0.47904 0.04387 11.00000 -1.20000
AFIX 0
C33 1 0.49751 0.53539 0.07950 11.00000 0.01616 0.02194 0.04151 =
-0.01689 -0.00736 0.00419
C34 1 0.44172 0.47166 0.13950 11.00000 0.02447 0.01794 0.03524 =
-0.01320 -0.00828 0.00302
C35 1 0.33536 0.49626 0.16970 11.00000 0.02307 0.01307 0.03133 =
-0.00857 -0.01262 0.00137
C36 1 0.26345 0.44598 0.22594 11.00000 0.02698 0.01938 0.02914 =
-0.00594 -0.00946 0.00036
C37 1 0.30322 0.36665 0.25565 11.00000 0.04636 0.02194 0.03612 =
0.00037 -0.01661 -0.00181
C38 1 0.40963 0.34341 0.22642 11.00000 0.05272 0.01600 0.05532 =
-0.00680 -0.02514 0.00853
AFIX 43
H38 2 0.43598 0.28998 0.24686 11.00000 -1.20000
AFIX 0
C39 1 0.48057 0.39252 0.16943 11.00000 0.03357 0.02340 0.04891 =
-0.01763 -0.02041 0.01019
C40 1 0.59384 0.35704 0.14430 11.00000 0.03951 0.03750 0.06639 =
-0.01804 -0.02102 0.02589
AFIX 137
H40a 2 0.59533 0.34311 0.10186 11.00000 -1.50000
H40b 2 0.60687 0.30579 0.17738 11.00000 -1.50000
H40c 2 0.65262 0.39926 0.13741 11.00000 -1.50000
AFIX 0
C41 1 0.23840 0.30739 0.31952 11.00000 0.07206 0.03463 0.05171 =
0.01345 -0.01641 -0.00128
AFIX 137
H41a 2 0.22362 0.33625 0.35578 11.00000 -1.50000
H41b 2 0.28259 0.25677 0.33153 11.00000 -1.50000
H41c 2 0.16716 0.29090 0.31249 11.00000 -1.50000
AFIX 0
C42 1 0.15574 0.48672 0.24543 11.00000 0.02324 0.02457 0.02401 =
-0.00506 -0.00478 -0.00515
C43 1 0.06498 0.45274 0.29740 11.00000 0.03595 0.04238 0.02653 =
-0.00071 -0.00736 -0.01403
AFIX 43
H43 2 0.06793 0.39634 0.32340 11.00000 -1.20000
AFIX 0
C44 1 -0.02977 0.50035 0.31164 11.00000 0.02096 0.06030 0.03005 =
-0.00945 0.00118 -0.01449
AFIX 43
H44 2 -0.09207 0.47619 0.34649 11.00000 -1.20000
AFIX 0
C45 1 -0.03305 0.58223 0.27525 11.00000 0.01917 0.05328 0.03506 =
-0.01776 0.00010 0.00409
AFIX 43
H45 2 -0.09590 0.61640 0.28582 11.00000 -1.20000
AFIX 0
C46 1 0.05659 0.61431 0.22290 11.00000 0.01997 0.03084 0.03399 =
-0.01275 -0.00655 0.00107
AFIX 43
H46 2 0.05334 0.67044 0.19649 11.00000 -1.20000
AFIX 0
C47 1 0.76232 0.71955 0.17824 11.00000 0.02430 0.02177 0.03217 =
-0.00506 0.00381 -0.00405
AFIX 43
H47 2 0.74659 0.77427 0.18554 11.00000 -1.20000
AFIX 0
C48 1 0.83929 0.71182 0.12063 11.00000 0.02826 0.03300 0.03778 =
-0.00409 0.00377 -0.00467
AFIX 43
H48 2 0.87522 0.76055 0.08886 11.00000 -1.20000
AFIX 0
C49 1 0.86242 0.63284 0.11048 11.00000 0.02757 0.03856 0.03346 =
-0.01078 0.00975 -0.00366
AFIX 43
H49 2 0.91426 0.62611 0.07132 11.00000 -1.20000
AFIX 0
C50 1 0.80943 0.56288 0.15789 11.00000 0.02034 0.02897 0.02756 =
-0.00980 0.00115 0.00095
AFIX 43
H50 2 0.82447 0.50800 0.15079 11.00000 -1.20000
AFIX 0
C51 1 0.73482 0.57192 0.21551 11.00000 0.01638 0.02040 0.02400 =
-0.00796 -0.00310 -0.00040
C52 1 0.67154 0.50350 0.26946 11.00000 0.01485 0.02124 0.02288 =
-0.00871 -0.00243 0.00018
C53 1 0.58826 0.53498 0.31447 11.00000 0.01470 0.01849 0.02304 =
-0.00956 -0.00712 -0.00070
C54 1 0.51572 0.48252 0.36971 11.00000 0.01612 0.02387 0.02517 =
-0.01016 -0.00365 -0.00064
C55 1 0.52056 0.39465 0.37680 11.00000 0.02555 0.01988 0.02942 =
-0.00548 -0.00626 -0.00409
C56 1 0.60718 0.36440 0.33378 11.00000 0.03172 0.01245 0.03953 =
-0.00720 -0.00558 0.00220
AFIX 43
H56 2 0.61339 0.30480 0.34051 11.00000 -1.20000
AFIX 0
C57 1 0.68609 0.41557 0.28113 11.00000 0.02468 0.02519 0.02797 =
-0.01039 -0.00991 0.00399
C58 1 0.78355 0.37338 0.24559 11.00000 0.02962 0.02570 0.03456 =
-0.01035 -0.00334 0.00976
AFIX 137
H58a 2 0.77860 0.38031 0.19911 11.00000 -1.50000
H58b 2 0.78213 0.31297 0.26809 11.00000 -1.50000
H58c 2 0.85364 0.39929 0.24634 11.00000 -1.50000
AFIX 0
C59 1 0.43973 0.33027 0.42872 11.00000 0.03423 0.02498 0.04487 =
-0.00425 0.00307 -0.00530
AFIX 137
H59a 2 0.45332 0.32604 0.47314 11.00000 -1.50000
H59b 2 0.45103 0.27496 0.41837 11.00000 -1.50000
H59c 2 0.36257 0.34817 0.42821 11.00000 -1.50000
AFIX 0
C60 1 0.44754 0.53109 0.41463 11.00000 0.01687 0.02349 0.02472 =
-0.00609 -0.00555 0.00067
C61 1 0.37521 0.49781 0.47609 11.00000 0.02274 0.02951 0.02703 =
-0.00523 -0.00205 -0.00189
AFIX 43
H61 2 0.36347 0.43829 0.49182 11.00000 -1.20000
AFIX 0
C62 1 0.32000 0.55026 0.51470 11.00000 0.02384 0.04854 0.02742 =
-0.01313 0.00198 -0.00341
AFIX 43
H62 2 0.27370 0.52709 0.55775 11.00000 -1.20000
AFIX 0
C63 1 0.33336 0.63722 0.48955 11.00000 0.02770 0.04647 0.03765 =
-0.02473 0.00385 -0.00117
AFIX 43
H63 2 0.29284 0.67474 0.51376 11.00000 -1.20000
AFIX 0
C64 1 0.40640 0.66792 0.42891 11.00000 0.02641 0.02791 0.03527 =
-0.01729 0.00268 -0.00150
AFIX 43
H64 2 0.41719 0.72741 0.41214 11.00000 -1.20000
AFIX 0
P1 7 1.00000 1.00000 0.00000 10.50000 0.04016 0.02117 0.03527 =
-0.00413 -0.01546 0.01011
F1 3 1.05451 1.02543 0.05369 11.00000 0.08518 0.05289 0.06234 =
-0.01858 -0.04389 0.00834
F2 3 0.88598 1.04248 0.02769 11.00000 0.04795 0.03859 0.07140 =
-0.00535 -0.00435 0.01818
F3 3 0.95999 0.91148 0.05206 11.00000 0.05806 0.02738 0.05880 =
0.00569 -0.01159 0.00415
P2 7 0.59721 1.10286 0.31922 11.00000 0.07447 0.02959 0.05119 =
-0.01429 -0.00939 -0.00336
PART 1
F4 3 0.68697 1.17678 0.28093 10.50000 0.06840
PART 0
PART 2
F4A 3 0.64468 1.18588 0.26264 10.50000 0.05616
PART 0
F5 3 0.51353 1.15914 0.35784 11.00000 0.11692 0.05792 0.10649 =
-0.04577 0.02840 -0.00716
PART 1
F6 3 0.66194 1.06547 0.37692 10.50000 0.11303
PART 0
PART 2
F6A 3 0.68491 1.12218 0.35843 10.50000 0.10500
PART 0
F7 3 0.67977 1.04326 0.28079 11.00000 0.08668 0.04637 0.08395 =
-0.02088 -0.01194 0.01757
PART 1
F8 3 0.53531 1.13406 0.25909 10.50000 0.10847
PART 0
PART 2
F8A 3 0.50804 1.09333 0.27729 10.50000 0.08658
PART 0
PART 1
F9 3 0.50696 1.02794 0.35248 10.50000 0.08012
PART 0
PART 2
F9A 3 0.55703 1.01789 0.37548 10.50000 0.08362
PART 0
PART -1
O1S 6 0.01396 0.53870 0.51070 10.50000 0.11160
AFIX 3
H1S 2 0.06068 0.53290 0.47763 10.50000 -1.50000
AFIX 0
C10S 1 0.04756 0.61170 0.52799 10.50000 0.04983
AFIX 3
H10d 2 -0.00997 0.61911 0.56530 10.50000 -1.50000
H10e 2 0.11745 0.60083 0.54139 10.50000 -1.50000
H10f 2 0.05486 0.66213 0.49213 10.50000 -1.50000
AFIX 0
PART 0
N1S 5 0.30248 0.87380 0.41526 10.50000 0.06686
C2S 1 0.35791 0.87759 0.44795 10.50000 0.03792
C3S 1 0.43869 0.88417 0.48477 10.50000 0.05429
AFIX 3
H3Sa 2 0.42871 0.84276 0.52694 10.50000 -1.50000
H3Sb 2 0.50925 0.87570 0.45639 10.50000 -1.50000
H3Sc 2 0.43769 0.93986 0.49201 10.50000 -1.50000
AFIX 0
N2S 5 0.21541 0.60354 0.34784 11.00000 0.07877 0.08448 0.07954 =
-0.02157 -0.02212 -0.00294
C4S 1 0.18352 0.66716 0.34799 11.00000 0.07164 0.07337 0.07202 =
-0.01842 -0.01684 0.00010
C5S 1 0.13819 0.74822 0.35034 11.00000 0.11584 0.11815 0.11699 =
-0.02931 -0.02608 0.00047
AFIX 3
H5Sa 2 0.14918 0.76237 0.38965 11.00000 -1.50000
H5Sb 2 0.05950 0.74770 0.35155 11.00000 -1.50000
H5Sc 2 0.17588 0.78952 0.31124 11.00000 -1.50000
AFIX 0
N3S 5 0.96235 0.80034 0.23553 11.00000 0.08223 0.05150 0.10116 =
-0.02462 0.00585 0.00280
C6S 1 0.94363 0.86790 0.22887 11.00000 0.05734 0.04245 0.06322 =
-0.01464 0.00833 -0.00199
C7S 1 0.91866 0.95557 0.21835 11.00000 0.08035 0.05228 0.08071 =
-0.01747 0.00016 0.02261
AFIX 3
H7Sa 2 0.83888 0.96233 0.22712 11.00000 -1.50000
H7Sb 2 0.94873 0.97895 0.24802 11.00000 -1.50000
H7Sc 2 0.95142 0.98451 0.17285 11.00000 -1.50000
AFIX 0
N4S 5 0.57725 0.78350 0.08392 10.50000 0.09060
PART 1
C8S 1 0.61096 0.83737 0.04194 10.50000 0.05853
C9S 1 0.66938 0.91146 -0.00130 10.50000 0.03834
AFIX 3
H9Sa 2 0.62356 0.95998 0.00218 10.50000 -1.50000
H9Sb 2 0.73818 0.91804 0.01125 10.50000 -1.50000
H9Sc 2 0.68560 0.90634 -0.04659 10.50000 -1.50000
AFIX 0
HKLF 4
END
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# start Validation Reply Form
_vrf_PLAT016_Ir2dpyx2L6_16srv324
;
PROBLEM: No _shelx_fab_file Record in SHELXL20xy CIF .... Please Supply
RESPONSE: The authors will be happy to provide FAB file on request
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# end Validation Reply Form