# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2019
#######################################################################
#
# 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_7-16s488
_database_code_depnum_ccdc_archive 'CCDC 1884007'
loop_
_audit_author_name
_audit_author_address
'Andrei S. Batsanov'
;Durham University
United Kingdom
;
_audit_update_record
;
2018-12-10 deposited with the CCDC. 2019-05-29 downloaded from the CCDC.
;
_ccdc_polymorph 'room-temperature phase'
_audit_creation_date 2016-03-14
_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 'C42 H34 N2 O2 S3'
_chemical_formula_sum 'C42 H34 N2 O2 S3'
_chemical_formula_weight 694.89
_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'
S S 0.1246 0.1234 '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 12.9638(8)
_cell_length_b 14.1725(10)
_cell_length_c 9.5622(6)
_cell_angle_alpha 77.138(2)
_cell_angle_beta 84.451(2)
_cell_angle_gamma 83.336(3)
_cell_volume 1696.65(19)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 5163
_cell_measurement_temperature 190
_cell_measurement_theta_max 24.31
_cell_measurement_theta_min 2.67
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.260
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.8989
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1396 before and 0.0544 after correction.
The Ratio of minimum to maximum transmission is 0.8989.
The \l/2 correction factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.360
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description lathe
_exptl_crystal_F_000 728
_exptl_crystal_size_max 0.319
_exptl_crystal_size_mid 0.067
_exptl_crystal_size_min 0.058
_exptl_special_details
; Data were collected in shutterless mode. Full sphere of reciprocal
space was nominally covered by 4 runs of narrow-frame \w-scans (scan
width 0.5\%, 10s exposure), every run at a different \f angle.
Crystal to detector distance 3.50 cm.
;
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 1.00 0.0030
0.00 0.00 -1.00 0.0270
1.00 0.00 0.00 0.0300
-1.00 0.00 0.00 0.0320
0.00 1.00 0.00 0.1410
0.00 -1.00 0.00 0.1450
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0641
_diffrn_reflns_av_unetI/netI 0.0701
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 23900
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full 25.126
_diffrn_reflns_theta_max 25.126
_diffrn_reflns_theta_min 2.273
_diffrn_ambient_temperature 190
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type 'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device '3-circle area detector 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 'Incoatec I\mS microsource'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 3903
_reflns_number_total 6043
_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 v8.34A (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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution 'ShelXS 2013/1 (Sheldrick, 2008)'
_refine_diff_density_max 0.399
_refine_diff_density_min -0.336
_refine_diff_density_rms 0.052
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.018
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 451
_refine_ls_number_reflns 6043
_refine_ls_number_restraints 6
_refine_ls_R_factor_all 0.0947
_refine_ls_R_factor_gt 0.0489
_refine_ls_restrained_S_all 1.105
_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^)+(0.0440P)^2^+0.7120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0981
_refine_ls_wR_factor_ref 0.1128
_refine_special_details
; High-temperature phase of 16srv065.
The iso-propyl group H~3~C(41)C(40)HC(42)H~3~ is disordered
between two positions with occupancies refined to 0.620(6) (A)
and 0.380(6) (B). Ordered methyl groups were refined as rigid bodies
rotating around C---C bonds. Other H atoms: riding model.
;
_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
C41B-C40A \\sim C40A-C41A \\sim C42B-C40A \\sim C40A-C42A
with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(C40B) = Uiso(C40A)
4. Others
Sof(C40B)=Sof(H40B)=Sof(C41B)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C42B)=
Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(1)
Sof(C40A)=Sof(H40A)=Sof(C41A)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42A)=
Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
C37(H37), C40A(H40A), C40B(H40B)
5.b Me refined with riding coordinates:
C41A(H41A,H41B,H41C), C42A(H42A,H42B,H42C), C41B(H41D,H41E,H41F), C42B(H42D,
H42E,H42F)
5.c Aromatic/amide H refined with riding coordinates:
C2(H2), C5(H5), C8(H8), C11(H11), C14(H14), C15(H15), C16(H16), C17(H17),
C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C27(H27), C28(H28), C29(H29),
C32(H32), C33(H33), C34(H34), C35(H35)
5.d Idealised Me refined as rotating group:
C38(H38A,H38B,H38C), C39(H39A,H39B,H39C)
;
_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
S1 S -0.01328(5) 0.54881(5) 0.23310(8) 0.02908(19) Uani 1 1 d . . . . .
S2 S 0.55482(6) 0.75933(6) 0.45426(10) 0.0483(3) Uani 1 1 d . . . . .
S3 S 0.33780(7) -0.03847(5) 0.50830(9) 0.0420(2) Uani 1 1 d . . . . .
O1 O -0.09594(14) 0.56173(15) 0.3400(2) 0.0420(5) Uani 1 1 d . . . . .
O2 O -0.03477(15) 0.58410(14) 0.0856(2) 0.0422(5) Uani 1 1 d . . . . .
N1 N 0.37976(17) 0.65809(16) 0.3919(2) 0.0312(6) Uani 1 1 d . . . . .
N2 N 0.20916(16) 0.15565(15) 0.3978(2) 0.0270(5) Uani 1 1 d . . . . .
C1 C 0.10101(19) 0.59354(19) 0.2703(3) 0.0244(6) Uani 1 1 d . . . . .
C2 C 0.1179(2) 0.68949(19) 0.2544(3) 0.0267(6) Uani 1 1 d . . . . .
H2 H 0.0658 0.7396 0.2186 0.032 Uiso 1 1 calc R . . . .
C3 C 0.2117(2) 0.71296(19) 0.2908(3) 0.0267(6) Uani 1 1 d . . . . .
C4 C 0.2842(2) 0.6358(2) 0.3464(3) 0.0277(7) Uani 1 1 d . . . . .
C5 C 0.2664(2) 0.5394(2) 0.3629(3) 0.0299(7) Uani 1 1 d . . . . .
H5 H 0.3168 0.4888 0.4026 0.036 Uiso 1 1 calc R . . . .
C6 C 0.1741(2) 0.51727(19) 0.3207(3) 0.0252(6) Uani 1 1 d . . . . .
C7 C 0.14136(19) 0.42140(19) 0.3202(3) 0.0237(6) Uani 1 1 d . . . . .
C8 C 0.1955(2) 0.33111(19) 0.3600(3) 0.0268(6) Uani 1 1 d . . . . .
H8 H 0.2624 0.3253 0.3955 0.032 Uiso 1 1 calc R . . . .
C9 C 0.15169(19) 0.24889(19) 0.3479(3) 0.0254(6) Uani 1 1 d . . . . .
C10 C 0.0552(2) 0.2533(2) 0.2926(3) 0.0299(7) Uani 1 1 d . . . . .
C11 C 0.0007(2) 0.3457(2) 0.2542(3) 0.0303(7) Uani 1 1 d . . . . .
H11 H -0.0658 0.3522 0.2173 0.036 Uiso 1 1 calc R . . . .
C12 C 0.04324(19) 0.42637(19) 0.2700(3) 0.0250(6) Uani 1 1 d . . . . .
C13 C 0.3783(2) 0.6664(2) 0.5374(3) 0.0342(7) Uani 1 1 d . . . . .
C14 C 0.2986(2) 0.6333(2) 0.6387(3) 0.0443(8) Uani 1 1 d . . . . .
H14 H 0.2445 0.6026 0.6118 0.053 Uiso 1 1 calc R . . . .
C15 C 0.2983(3) 0.6453(3) 0.7795(4) 0.0531(9) Uani 1 1 d . . . . .
H15 H 0.2435 0.6231 0.8481 0.064 Uiso 1 1 calc R . . . .
C16 C 0.3765(3) 0.6888(3) 0.8201(4) 0.0573(10) Uani 1 1 d . . . . .
H16 H 0.3749 0.6980 0.9157 0.069 Uiso 1 1 calc R . . . .
C17 C 0.4570(3) 0.7190(2) 0.7224(4) 0.0518(10) Uani 1 1 d . . . . .
H17 H 0.5122 0.7470 0.7516 0.062 Uiso 1 1 calc R . . . .
C18 C 0.4583(2) 0.7089(2) 0.5811(3) 0.0398(8) Uani 1 1 d . . . . .
C19 C 0.4741(2) 0.6400(2) 0.3111(3) 0.0330(7) Uani 1 1 d . . . . .
C20 C 0.4824(2) 0.5903(2) 0.2004(3) 0.0405(8) Uani 1 1 d . . . . .
H20 H 0.4224 0.5659 0.1773 0.049 Uiso 1 1 calc R . . . .
C21 C 0.5763(2) 0.5755(2) 0.1229(4) 0.0500(9) Uani 1 1 d . . . . .
H21 H 0.5794 0.5434 0.0451 0.060 Uiso 1 1 calc R . . . .
C22 C 0.6654(2) 0.6069(2) 0.1576(4) 0.0549(10) Uani 1 1 d . . . . .
H22 H 0.7306 0.5939 0.1075 0.066 Uiso 1 1 calc R . . . .
C23 C 0.6581(2) 0.6572(2) 0.2659(4) 0.0479(9) Uani 1 1 d . . . . .
H23 H 0.7191 0.6787 0.2909 0.058 Uiso 1 1 calc R . . . .
C24 C 0.5642(2) 0.6770(2) 0.3391(3) 0.0377(8) Uani 1 1 d . . . . .
C25 C 0.2106(2) 0.12488(19) 0.5502(3) 0.0270(7) Uani 1 1 d . . . . .
C26 C 0.1528(2) 0.1778(2) 0.6412(3) 0.0338(7) Uani 1 1 d . . . . .
H26 H 0.1116 0.2358 0.6015 0.041 Uiso 1 1 calc R . . . .
C27 C 0.1540(2) 0.1479(2) 0.7887(3) 0.0419(8) Uani 1 1 d . . . . .
H27 H 0.1134 0.1852 0.8490 0.050 Uiso 1 1 calc R . . . .
C28 C 0.2133(2) 0.0646(2) 0.8492(3) 0.0422(8) Uani 1 1 d . . . . .
H28 H 0.2147 0.0444 0.9507 0.051 Uiso 1 1 calc R . . . .
C29 C 0.2707(2) 0.0111(2) 0.7601(3) 0.0359(7) Uani 1 1 d . . . . .
H29 H 0.3120 -0.0465 0.8008 0.043 Uiso 1 1 calc R . . . .
C30 C 0.2692(2) 0.0397(2) 0.6122(3) 0.0293(7) Uani 1 1 d . . . . .
C31 C 0.2939(2) 0.12914(19) 0.3037(3) 0.0255(6) Uani 1 1 d . . . . .
C32 C 0.3106(2) 0.1844(2) 0.1653(3) 0.0332(7) Uani 1 1 d . . . . .
H32 H 0.2647 0.2406 0.1326 0.040 Uiso 1 1 calc R . . . .
C33 C 0.3938(2) 0.1581(2) 0.0744(3) 0.0385(8) Uani 1 1 d . . . . .
H33 H 0.4030 0.1957 -0.0207 0.046 Uiso 1 1 calc R . . . .
C34 C 0.4617(2) 0.0798(2) 0.1192(3) 0.0385(8) Uani 1 1 d . . . . .
H34 H 0.5195 0.0638 0.0570 0.046 Uiso 1 1 calc R . . . .
C35 C 0.4469(2) 0.0233(2) 0.2558(3) 0.0366(8) Uani 1 1 d . . . . .
H35 H 0.4955 -0.0310 0.2878 0.044 Uiso 1 1 calc R . . . .
C36 C 0.3614(2) 0.0452(2) 0.3468(3) 0.0299(7) Uani 1 1 d . . . . .
C37 C 0.2365(2) 0.8177(2) 0.2660(3) 0.0321(7) Uani 1 1 d . . . . .
H37 H 0.2712 0.8248 0.3516 0.039 Uiso 1 1 calc R . . . .
C38 C 0.3131(2) 0.8414(2) 0.1346(3) 0.0417(8) Uani 1 1 d . . . . .
H38A H 0.3779 0.7987 0.1503 0.063 Uiso 1 1 calc GR . . . .
H38B H 0.3280 0.9093 0.1194 0.063 Uiso 1 1 calc GR . . . .
H38C H 0.2827 0.8314 0.0497 0.063 Uiso 1 1 calc GR . . . .
C39 C 0.1407(2) 0.8919(2) 0.2490(4) 0.0450(8) Uani 1 1 d . . . . .
H39A H 0.1112 0.8937 0.1578 0.068 Uiso 1 1 calc GR . . . .
H39B H 0.1609 0.9564 0.2495 0.068 Uiso 1 1 calc GR . . . .
H39C H 0.0887 0.8733 0.3289 0.068 Uiso 1 1 calc GR . . . .
C40A C 0.0163(5) 0.1630(5) 0.2573(5) 0.0310(10) Uiso 0.620(6) 1 d D . P A 1
H40A H 0.0800 0.1195 0.2380 0.037 Uiso 0.620(6) 1 calc R . P A 1
C41A C -0.0440(5) 0.1812(4) 0.1263(5) 0.0506(18) Uani 0.620(6) 1 d D . P A 1
H41A H -0.0035 0.2171 0.0437 0.076 Uiso 0.620(6) 1 calc R . P A 1
H41B H -0.0576 0.1189 0.1068 0.076 Uiso 0.620(6) 1 calc R . P A 1
H41C H -0.1102 0.2195 0.1427 0.076 Uiso 0.620(6) 1 calc R . P A 1
C42A C -0.0409(6) 0.1087(5) 0.3866(6) 0.076(3) Uani 0.620(6) 1 d D . P A 1
H42A H 0.0011 0.0984 0.4695 0.114 Uiso 0.620(6) 1 calc R . P A 1
H42B H -0.1071 0.1462 0.4058 0.114 Uiso 0.620(6) 1 calc R . P A 1
H42C H -0.0545 0.0456 0.3699 0.114 Uiso 0.620(6) 1 calc R . P A 1
C40B C 0.0066(8) 0.1624(8) 0.2983(11) 0.0310(10) Uiso 0.380(6) 1 d . . P A 2
H40B H 0.0418 0.1073 0.3674 0.037 Uiso 0.380(6) 1 calc R . P A 2
C41B C 0.0320(7) 0.1467(6) 0.1364(8) 0.038(2) Uiso 0.380(6) 1 d D . P A 2
H41D H 0.1074 0.1441 0.1126 0.058 Uiso 0.380(6) 1 calc R . P A 2
H41E H 0.0070 0.0856 0.1286 0.058 Uiso 0.380(6) 1 calc R . P A 2
H41F H -0.0029 0.2009 0.0695 0.058 Uiso 0.380(6) 1 calc R . P A 2
C42B C -0.1075(6) 0.1659(7) 0.3294(10) 0.044(3) Uiso 0.380(6) 1 d D . P A 2
H42D H -0.1305 0.1022 0.3305 0.066 Uiso 0.380(6) 1 calc R . P A 2
H42E H -0.1261 0.1824 0.4235 0.066 Uiso 0.380(6) 1 calc R . P A 2
H42F H -0.1417 0.2153 0.2550 0.066 Uiso 0.380(6) 1 calc R . P A 2
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
S1 0.0259(4) 0.0218(4) 0.0403(5) -0.0053(3) -0.0126(3) 0.0002(3)
S2 0.0459(5) 0.0298(5) 0.0743(6) -0.0090(4) -0.0269(5) -0.0103(4)
S3 0.0593(5) 0.0200(4) 0.0446(5) -0.0054(4) -0.0092(4) 0.0070(4)
O1 0.0243(11) 0.0427(13) 0.0588(14) -0.0154(11) 0.0027(10) 0.0023(9)
O2 0.0531(13) 0.0309(12) 0.0428(13) 0.0002(10) -0.0281(11) 0.0003(10)
N1 0.0283(13) 0.0267(14) 0.0410(15) -0.0072(12) -0.0138(11) -0.0037(10)
N2 0.0262(12) 0.0196(13) 0.0330(14) -0.0013(11) -0.0043(11) 0.0005(10)
C1 0.0234(14) 0.0231(16) 0.0273(16) -0.0057(13) -0.0047(12) -0.0022(12)
C2 0.0270(15) 0.0217(16) 0.0308(16) -0.0042(13) -0.0074(13) 0.0016(12)
C3 0.0304(15) 0.0238(16) 0.0272(16) -0.0072(13) -0.0053(13) -0.0019(12)
C4 0.0257(15) 0.0275(17) 0.0313(16) -0.0054(14) -0.0093(13) -0.0035(12)
C5 0.0264(15) 0.0255(17) 0.0364(17) -0.0017(14) -0.0117(13) 0.0019(12)
C6 0.0273(15) 0.0204(15) 0.0278(16) -0.0034(13) -0.0056(12) -0.0021(12)
C7 0.0239(14) 0.0228(16) 0.0242(15) -0.0025(12) -0.0046(12) -0.0037(12)
C8 0.0231(14) 0.0260(16) 0.0296(16) -0.0006(13) -0.0080(12) -0.0005(12)
C9 0.0255(15) 0.0201(15) 0.0277(16) 0.0014(13) -0.0039(12) -0.0014(12)
C10 0.0285(15) 0.0239(16) 0.0367(17) -0.0011(14) -0.0085(13) -0.0062(12)
C11 0.0254(15) 0.0266(17) 0.0395(18) -0.0040(14) -0.0108(13) -0.0042(13)
C12 0.0255(15) 0.0219(16) 0.0265(15) -0.0013(13) -0.0083(12) -0.0001(12)
C13 0.0373(17) 0.0257(17) 0.0423(19) -0.0103(15) -0.0196(15) 0.0058(13)
C14 0.0417(19) 0.048(2) 0.048(2) -0.0164(17) -0.0162(17) -0.0019(16)
C15 0.056(2) 0.060(2) 0.045(2) -0.0176(19) -0.0134(18) 0.0072(18)
C16 0.075(3) 0.053(2) 0.051(2) -0.026(2) -0.031(2) 0.014(2)
C17 0.059(2) 0.039(2) 0.066(3) -0.0210(19) -0.035(2) 0.0015(18)
C18 0.0473(19) 0.0212(17) 0.054(2) -0.0079(15) -0.0256(16) 0.0029(14)
C19 0.0280(16) 0.0231(16) 0.0468(19) -0.0019(15) -0.0149(14) 0.0018(13)
C20 0.0311(17) 0.0362(19) 0.056(2) -0.0099(17) -0.0095(16) -0.0036(14)
C21 0.041(2) 0.041(2) 0.070(2) -0.0187(19) -0.0079(18) 0.0023(16)
C22 0.0307(19) 0.046(2) 0.082(3) -0.007(2) -0.0004(18) 0.0030(16)
C23 0.0301(19) 0.035(2) 0.074(2) 0.0031(19) -0.0181(17) 0.0004(15)
C24 0.0310(17) 0.0253(17) 0.054(2) 0.0026(15) -0.0181(15) -0.0002(13)
C25 0.0236(15) 0.0231(16) 0.0328(17) 0.0009(13) -0.0059(13) -0.0061(12)
C26 0.0287(16) 0.0276(17) 0.0397(19) -0.0001(15) 0.0004(14) 0.0032(13)
C27 0.0374(18) 0.047(2) 0.038(2) -0.0071(16) 0.0055(15) 0.0008(15)
C28 0.0439(19) 0.045(2) 0.0324(18) 0.0032(16) -0.0086(15) -0.0021(16)
C29 0.0384(18) 0.0284(18) 0.0373(19) 0.0003(15) -0.0078(15) 0.0017(14)
C30 0.0291(15) 0.0205(15) 0.0382(18) -0.0027(13) -0.0082(13) -0.0034(12)
C31 0.0268(15) 0.0188(15) 0.0330(17) -0.0078(13) -0.0065(13) -0.0030(12)
C32 0.0371(17) 0.0255(17) 0.0362(18) -0.0056(14) -0.0035(14) -0.0014(13)
C33 0.0405(18) 0.042(2) 0.0354(18) -0.0128(16) 0.0002(15) -0.0091(15)
C34 0.0371(18) 0.036(2) 0.048(2) -0.0212(17) 0.0006(15) -0.0059(15)
C35 0.0338(17) 0.0292(18) 0.049(2) -0.0147(16) -0.0115(15) 0.0048(14)
C36 0.0331(16) 0.0229(16) 0.0383(17) -0.0125(14) -0.0096(14) -0.0043(13)
C37 0.0371(17) 0.0225(16) 0.0395(18) -0.0091(14) -0.0128(14) -0.0008(13)
C38 0.0443(19) 0.0258(18) 0.053(2) -0.0019(16) -0.0045(16) -0.0070(14)
C39 0.0428(19) 0.0235(17) 0.071(2) -0.0153(17) -0.0081(17) 0.0006(14)
C41A 0.063(4) 0.047(4) 0.049(4) -0.019(3) -0.004(3) -0.021(3)
C42A 0.113(6) 0.071(5) 0.052(4) 0.000(4) -0.013(4) -0.068(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
S1 O1 1.432(2) . ?
S1 O2 1.431(2) . ?
S1 C1 1.773(3) . ?
S1 C12 1.776(3) . ?
S2 C18 1.754(3) . ?
S2 C24 1.761(3) . ?
S3 C30 1.759(3) . ?
S3 C36 1.750(3) . ?
N1 C4 1.443(3) . ?
N1 C13 1.420(4) . ?
N1 C19 1.412(3) . ?
N2 C9 1.445(3) . ?
N2 C25 1.426(3) . ?
N2 C31 1.422(3) . ?
C1 C2 1.375(4) . ?
C1 C6 1.384(3) . ?
C2 C3 1.391(4) . ?
C3 C4 1.401(4) . ?
C3 C37 1.518(4) . ?
C4 C5 1.383(4) . ?
C5 C6 1.389(4) . ?
C6 C7 1.471(4) . ?
C7 C8 1.379(4) . ?
C7 C12 1.391(3) . ?
C8 C9 1.385(4) . ?
C9 C10 1.394(4) . ?
C10 C11 1.403(4) . ?
C10 C40A 1.544(7) . ?
C10 C40B 1.487(11) . ?
C11 C12 1.369(4) . ?
C13 C14 1.394(4) . ?
C13 C18 1.398(4) . ?
C14 C15 1.393(4) . ?
C15 C16 1.374(5) . ?
C16 C17 1.371(5) . ?
C17 C18 1.388(4) . ?
C19 C20 1.386(4) . ?
C19 C24 1.405(4) . ?
C20 C21 1.381(4) . ?
C21 C22 1.380(4) . ?
C22 C23 1.372(5) . ?
C23 C24 1.376(4) . ?
C25 C26 1.384(4) . ?
C25 C30 1.393(4) . ?
C26 C27 1.380(4) . ?
C27 C28 1.375(4) . ?
C28 C29 1.374(4) . ?
C29 C30 1.384(4) . ?
C31 C32 1.391(4) . ?
C31 C36 1.401(4) . ?
C32 C33 1.387(4) . ?
C33 C34 1.351(4) . ?
C34 C35 1.380(4) . ?
C35 C36 1.392(4) . ?
C37 C38 1.525(4) . ?
C37 C39 1.528(4) . ?
C40A C41A 1.499(7) . ?
C40A C42A 1.484(8) . ?
C40B C41B 1.610(12) . ?
C40B C42B 1.478(12) . ?
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 S1 C1 110.44(12) . . ?
O1 S1 C12 109.66(12) . . ?
O2 S1 O1 117.44(12) . . ?
O2 S1 C1 110.86(12) . . ?
O2 S1 C12 113.06(12) . . ?
C1 S1 C12 92.65(12) . . ?
C18 S2 C24 99.08(14) . . ?
C36 S3 C30 99.94(13) . . ?
C13 N1 C4 116.4(2) . . ?
C19 N1 C4 119.0(2) . . ?
C19 N1 C13 121.4(2) . . ?
C25 N2 C9 115.2(2) . . ?
C31 N2 C9 115.8(2) . . ?
C31 N2 C25 121.7(2) . . ?
C2 C1 S1 126.6(2) . . ?
C2 C1 C6 122.9(2) . . ?
C6 C1 S1 110.5(2) . . ?
C1 C2 C3 119.8(2) . . ?
C2 C3 C4 117.3(2) . . ?
C2 C3 C37 121.6(2) . . ?
C4 C3 C37 121.1(2) . . ?
C3 C4 N1 118.4(2) . . ?
C5 C4 N1 118.9(2) . . ?
C5 C4 C3 122.6(2) . . ?
C4 C5 C6 119.3(2) . . ?
C1 C6 C5 118.0(2) . . ?
C1 C6 C7 113.2(2) . . ?
C5 C6 C7 128.8(2) . . ?
C8 C7 C6 128.5(2) . . ?
C8 C7 C12 118.2(2) . . ?
C12 C7 C6 113.3(2) . . ?
C7 C8 C9 119.6(2) . . ?
C8 C9 N2 117.5(2) . . ?
C8 C9 C10 122.6(2) . . ?
C10 C9 N2 119.9(2) . . ?
C9 C10 C11 117.0(2) . . ?
C9 C10 C40A 121.5(3) . . ?
C9 C10 C40B 120.1(5) . . ?
C11 C10 C40A 121.1(3) . . ?
C11 C10 C40B 122.2(5) . . ?
C12 C11 C10 120.1(2) . . ?
C7 C12 S1 110.1(2) . . ?
C11 C12 S1 127.5(2) . . ?
C11 C12 C7 122.4(2) . . ?
C14 C13 N1 121.7(3) . . ?
C14 C13 C18 118.7(3) . . ?
C18 C13 N1 119.7(3) . . ?
C15 C14 C13 120.0(3) . . ?
C16 C15 C14 120.6(4) . . ?
C17 C16 C15 119.9(3) . . ?
C16 C17 C18 120.5(3) . . ?
C13 C18 S2 120.0(2) . . ?
C17 C18 S2 119.4(3) . . ?
C17 C18 C13 120.3(3) . . ?
C20 C19 N1 123.3(3) . . ?
C20 C19 C24 117.5(3) . . ?
C24 C19 N1 119.1(3) . . ?
C21 C20 C19 121.3(3) . . ?
C22 C21 C20 120.6(3) . . ?
C23 C22 C21 118.7(3) . . ?
C22 C23 C24 121.4(3) . . ?
C19 C24 S2 119.9(2) . . ?
C23 C24 S2 119.4(2) . . ?
C23 C24 C19 120.3(3) . . ?
C26 C25 N2 121.1(2) . . ?
C26 C25 C30 117.9(3) . . ?
C30 C25 N2 120.9(3) . . ?
C27 C26 C25 121.1(3) . . ?
C28 C27 C26 120.7(3) . . ?
C29 C28 C27 118.7(3) . . ?
C28 C29 C30 121.1(3) . . ?
C25 C30 S3 122.1(2) . . ?
C29 C30 S3 117.5(2) . . ?
C29 C30 C25 120.4(3) . . ?
C32 C31 N2 121.1(2) . . ?
C32 C31 C36 118.1(3) . . ?
C36 C31 N2 120.8(2) . . ?
C33 C32 C31 120.7(3) . . ?
C34 C33 C32 120.9(3) . . ?
C33 C34 C35 119.8(3) . . ?
C34 C35 C36 120.5(3) . . ?
C31 C36 S3 122.1(2) . . ?
C35 C36 S3 118.0(2) . . ?
C35 C36 C31 119.8(3) . . ?
C3 C37 C38 110.3(2) . . ?
C3 C37 C39 113.9(2) . . ?
C38 C37 C39 109.4(2) . . ?
C41A C40A C10 115.9(5) . . ?
C42A C40A C10 109.6(4) . . ?
C42A C40A C41A 112.2(5) . . ?
C10 C40B C41B 102.0(7) . . ?
C42B C40B C10 116.9(8) . . ?
C42B C40B C41B 107.6(7) . . ?
_shelx_SHELXL_version_number 2014/7
_iucr_refine_instructions_details
;
16srv065a.res created by SHELXL-2014/7
TITL 16srv065a in P-1 #2
CELL 0.71073 12.9638 14.1725 9.5622 77.1382 84.4509 83.3363
ZERR 2 0.0008 0.001 0.0006 0.0023 0.0023 0.0025
LATT 1
SFAC C H N O S
UNIT 84 68 4 4 6
SADI C41B C40A C40A C41A C42B C40A C40A C42A
EADP C40B C40A
L.S. 7
PLAN 10
TEMP -83.15
fmap 2 53
ACTA
REM
REM
REM
WGHT 0.044000 0.712000
FVAR 0.19353 0.61964
S1 5 -0.013277 0.548808 0.233105 11.00000 0.02594 0.02183 =
0.04026 -0.00530 -0.01258 0.00024
S2 5 0.554817 0.759327 0.454263 11.00000 0.04595 0.02977 =
0.07431 -0.00897 -0.02694 -0.01034
S3 5 0.337804 -0.038470 0.508305 11.00000 0.05928 0.02001 =
0.04459 -0.00543 -0.00924 0.00697
O1 4 -0.095941 0.561728 0.339965 11.00000 0.02430 0.04266 =
0.05879 -0.01543 0.00270 0.00234
O2 4 -0.034770 0.584097 0.085563 11.00000 0.05308 0.03089 =
0.04277 0.00016 -0.02811 0.00030
N1 3 0.379760 0.658087 0.391909 11.00000 0.02827 0.02666 =
0.04100 -0.00717 -0.01376 -0.00372
N2 3 0.209157 0.155654 0.397834 11.00000 0.02621 0.01956 =
0.03300 -0.00125 -0.00434 0.00046
C1 1 0.101010 0.593537 0.270328 11.00000 0.02336 0.02312 =
0.02727 -0.00566 -0.00465 -0.00217
C2 1 0.117937 0.689491 0.254394 11.00000 0.02697 0.02174 =
0.03079 -0.00422 -0.00740 0.00164
AFIX 43
H2 2 0.065816 0.739570 0.218646 11.00000 -1.20000
AFIX 0
C3 1 0.211659 0.712961 0.290812 11.00000 0.03044 0.02380 =
0.02724 -0.00723 -0.00535 -0.00193
C4 1 0.284159 0.635760 0.346421 11.00000 0.02568 0.02750 =
0.03125 -0.00540 -0.00930 -0.00352
C5 1 0.266397 0.539381 0.362861 11.00000 0.02640 0.02548 =
0.03642 -0.00174 -0.01172 0.00192
AFIX 43
H5 2 0.316814 0.488848 0.402558 11.00000 -1.20000
AFIX 0
C6 1 0.174084 0.517271 0.320724 11.00000 0.02735 0.02038 =
0.02782 -0.00335 -0.00562 -0.00210
C7 1 0.141365 0.421397 0.320180 11.00000 0.02391 0.02276 =
0.02416 -0.00254 -0.00459 -0.00372
C8 1 0.195468 0.331108 0.359997 11.00000 0.02308 0.02599 =
0.02963 -0.00058 -0.00804 -0.00049
AFIX 43
H8 2 0.262375 0.325305 0.395524 11.00000 -1.20000
AFIX 0
C9 1 0.151692 0.248891 0.347897 11.00000 0.02546 0.02011 =
0.02770 0.00145 -0.00386 -0.00144
C10 1 0.055245 0.253337 0.292580 11.00000 0.02848 0.02391 =
0.03674 -0.00110 -0.00851 -0.00622
C11 1 0.000738 0.345666 0.254223 11.00000 0.02545 0.02655 =
0.03953 -0.00401 -0.01083 -0.00415
AFIX 43
H11 2 -0.065766 0.352183 0.217280 11.00000 -1.20000
AFIX 0
C12 1 0.043238 0.426368 0.269950 11.00000 0.02552 0.02189 =
0.02649 -0.00135 -0.00831 -0.00011
C13 1 0.378301 0.666419 0.537360 11.00000 0.03726 0.02566 =
0.04232 -0.01028 -0.01960 0.00585
C14 1 0.298609 0.633312 0.638743 11.00000 0.04174 0.04802 =
0.04813 -0.01637 -0.01621 -0.00188
AFIX 43
H14 2 0.244537 0.602601 0.611843 11.00000 -1.20000
AFIX 0
C15 1 0.298282 0.645276 0.779536 11.00000 0.05608 0.05952 =
0.04543 -0.01760 -0.01338 0.00722
AFIX 43
H15 2 0.243489 0.623148 0.848065 11.00000 -1.20000
AFIX 0
C16 1 0.376526 0.688803 0.820097 11.00000 0.07500 0.05324 =
0.05101 -0.02590 -0.03103 0.01394
AFIX 43
H16 2 0.374898 0.697991 0.915742 11.00000 -1.20000
AFIX 0
C17 1 0.456966 0.718971 0.722400 11.00000 0.05936 0.03893 =
0.06631 -0.02098 -0.03514 0.00152
AFIX 43
H17 2 0.512207 0.746972 0.751630 11.00000 -1.20000
AFIX 0
C18 1 0.458283 0.708901 0.581120 11.00000 0.04732 0.02120 =
0.05377 -0.00790 -0.02557 0.00293
C19 1 0.474146 0.640007 0.311052 11.00000 0.02800 0.02315 =
0.04677 -0.00194 -0.01493 0.00179
C20 1 0.482432 0.590266 0.200357 11.00000 0.03109 0.03623 =
0.05562 -0.00986 -0.00954 -0.00362
AFIX 43
H20 2 0.422422 0.565882 0.177331 11.00000 -1.20000
AFIX 0
C21 1 0.576258 0.575471 0.122890 11.00000 0.04104 0.04141 =
0.07000 -0.01871 -0.00790 0.00231
AFIX 43
H21 2 0.579421 0.543401 0.045060 11.00000 -1.20000
AFIX 0
C22 1 0.665422 0.606874 0.157584 11.00000 0.03072 0.04613 =
0.08242 -0.00713 -0.00044 0.00297
AFIX 43
H22 2 0.730624 0.593938 0.107474 11.00000 -1.20000
AFIX 0
C23 1 0.658090 0.657160 0.265888 11.00000 0.03007 0.03527 =
0.07359 0.00307 -0.01812 0.00036
AFIX 43
H23 2 0.719149 0.678735 0.290886 11.00000 -1.20000
AFIX 0
C24 1 0.564200 0.677006 0.339061 11.00000 0.03098 0.02526 =
0.05403 0.00260 -0.01806 -0.00022
C25 1 0.210602 0.124880 0.550215 11.00000 0.02362 0.02315 =
0.03280 0.00089 -0.00590 -0.00609
C26 1 0.152791 0.177840 0.641198 11.00000 0.02873 0.02760 =
0.03971 -0.00012 0.00037 0.00319
AFIX 43
H26 2 0.111599 0.235788 0.601474 11.00000 -1.20000
AFIX 0
C27 1 0.153986 0.147877 0.788660 11.00000 0.03737 0.04702 =
0.03763 -0.00711 0.00546 0.00081
AFIX 43
H27 2 0.113362 0.185194 0.849006 11.00000 -1.20000
AFIX 0
C28 1 0.213343 0.064582 0.849213 11.00000 0.04388 0.04548 =
0.03239 0.00321 -0.00858 -0.00213
AFIX 43
H28 2 0.214668 0.044431 0.950711 11.00000 -1.20000
AFIX 0
C29 1 0.270663 0.011098 0.760138 11.00000 0.03842 0.02841 =
0.03728 0.00035 -0.00776 0.00174
AFIX 43
H29 2 0.311984 -0.046525 0.800810 11.00000 -1.20000
AFIX 0
C30 1 0.269247 0.039720 0.612171 11.00000 0.02908 0.02046 =
0.03822 -0.00274 -0.00824 -0.00339
C31 1 0.293871 0.129138 0.303719 11.00000 0.02679 0.01883 =
0.03299 -0.00783 -0.00654 -0.00298
C32 1 0.310637 0.184360 0.165272 11.00000 0.03711 0.02546 =
0.03624 -0.00558 -0.00352 -0.00143
AFIX 43
H32 2 0.264708 0.240612 0.132637 11.00000 -1.20000
AFIX 0
C33 1 0.393753 0.158120 0.074365 11.00000 0.04052 0.04245 =
0.03536 -0.01284 0.00016 -0.00910
AFIX 43
H33 2 0.403013 0.195693 -0.020698 11.00000 -1.20000
AFIX 0
C34 1 0.461689 0.079849 0.119238 11.00000 0.03711 0.03646 =
0.04758 -0.02123 0.00058 -0.00586
AFIX 43
H34 2 0.519502 0.063775 0.056980 11.00000 -1.20000
AFIX 0
C35 1 0.446903 0.023290 0.255753 11.00000 0.03379 0.02923 =
0.04946 -0.01473 -0.01155 0.00477
AFIX 43
H35 2 0.495458 -0.031024 0.287801 11.00000 -1.20000
AFIX 0
C36 1 0.361424 0.045197 0.346830 11.00000 0.03308 0.02291 =
0.03830 -0.01246 -0.00960 -0.00432
C37 1 0.236534 0.817727 0.266028 11.00000 0.03712 0.02247 =
0.03951 -0.00913 -0.01283 -0.00084
AFIX 13
H37 2 0.271203 0.824753 0.351644 11.00000 -1.20000
AFIX 0
C38 1 0.313129 0.841403 0.134637 11.00000 0.04426 0.02585 =
0.05295 -0.00195 -0.00453 -0.00698
AFIX 137
H38A 2 0.377899 0.798654 0.150302 11.00000 -1.50000
H38B 2 0.328006 0.909327 0.119433 11.00000 -1.50000
H38C 2 0.282705 0.831443 0.049738 11.00000 -1.50000
AFIX 0
C39 1 0.140731 0.891926 0.249018 11.00000 0.04285 0.02349 =
0.07109 -0.01534 -0.00810 0.00055
AFIX 137
H39A 2 0.111205 0.893705 0.157806 11.00000 -1.50000
H39B 2 0.160883 0.956392 0.249474 11.00000 -1.50000
H39C 2 0.088659 0.873271 0.328863 11.00000 -1.50000
AFIX 0
PART 1
C40A 1 0.016302 0.162982 0.257315 21.00000 0.03105
AFIX 13
H40A 2 0.080020 0.119454 0.237990 21.00000 -1.20000
AFIX 0
C41A 1 -0.043973 0.181187 0.126282 21.00000 0.06303 0.04726 =
0.04935 -0.01869 -0.00447 -0.02091
AFIX 33
H41A 2 -0.003528 0.217087 0.043693 21.00000 -1.50000
H41B 2 -0.057573 0.118924 0.106764 21.00000 -1.50000
H41C 2 -0.110235 0.219457 0.142699 21.00000 -1.50000
AFIX 0
C42A 1 -0.040899 0.108679 0.386629 21.00000 0.11331 0.07130 =
0.05170 0.00041 -0.01323 -0.06806
AFIX 33
H42A 2 0.001138 0.098373 0.469540 21.00000 -1.50000
H42B 2 -0.107134 0.146170 0.405836 21.00000 -1.50000
H42C 2 -0.054473 0.045636 0.369901 21.00000 -1.50000
AFIX 0
PART 0
PART 2
C40B 1 0.006603 0.162447 0.298348 -21.00000 0.03105
AFIX 13
H40B 2 0.041754 0.107311 0.367391 -21.00000 -1.20000
AFIX 0
C41B 1 0.032003 0.146719 0.136427 -21.00000 0.03839
AFIX 33
H41D 2 0.107379 0.144144 0.112616 -21.00000 -1.50000
H41E 2 0.007020 0.085562 0.128612 -21.00000 -1.50000
H41F 2 -0.002933 0.200881 0.069517 -21.00000 -1.50000
AFIX 0
C42B 1 -0.107530 0.165867 0.329440 -21.00000 0.04424
AFIX 33
H42D 2 -0.130467 0.102201 0.330474 -21.00000 -1.50000
H42E 2 -0.126094 0.182406 0.423482 -21.00000 -1.50000
H42F 2 -0.141704 0.215261 0.254980 -21.00000 -1.50000
AFIX 0
HKLF 4
REM 16srv065a in P-1 #2
REM R1 = 0.0489 for 3903 Fo > 4sig(Fo) and 0.0947 for all 6043 data
REM 451 parameters refined using 6 restraints
END
WGHT 0.0446 0.7124
REM Highest difference peak 0.399, deepest hole -0.336, 1-sigma level 0.052
Q1 1 0.0327 0.1596 0.2210 11.00000 0.05 0.40
Q2 1 -0.1455 0.1937 0.3088 11.00000 0.05 0.29
Q3 1 -0.1435 0.1957 0.3521 11.00000 0.05 0.28
Q4 1 0.0571 0.5790 0.2461 11.00000 0.05 0.27
Q5 1 0.0053 0.4776 0.2740 11.00000 0.05 0.27
Q6 1 0.3450 0.0146 0.4246 11.00000 0.05 0.25
Q7 1 -0.0443 0.5202 0.3691 11.00000 0.05 0.25
Q8 1 0.0793 0.4187 0.3390 11.00000 0.05 0.21
Q9 1 0.5286 0.7015 0.5254 11.00000 0.05 0.21
Q10 1 0.5996 0.5794 -0.0095 11.00000 0.05 0.20
REM The information below was added by Olex2.
REM
REM R1 = 0.0489 for 3903 Fo > 4sig(Fo) and 0.0947 for all 23900 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.40, deepest hole -0.34
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0947
REM R1_gt = 0.0489
REM wR_ref = 0.1128
REM GOOF = 1.018
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 23900
REM Reflections_gt = 3903
REM Parameters = n/a
REM Hole = -0.34
REM Peak = 0.40
REM Flack = n/a
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
#===END
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/hexane'
_exptl_crystal_preparation Luminescent
#######################################################################
#
# 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_6-15s293
_database_code_depnum_ccdc_archive 'CCDC 1884010'
loop_
_audit_author_name
_audit_author_address
'Andrei S. Batsanov'
;Durham University
United Kingdom
;
_audit_update_record
;
2018-12-10 deposited with the CCDC. 2019-05-29 downloaded from the CCDC.
;
_audit_creation_date 2018-12-06
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C38 H26 N2 O2 S3'
_chemical_formula_sum 'C38 H26 N2 O2 S3'
_chemical_formula_weight 638.79
_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'
S S 0.1246 0.1234 '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 8.7268(8)
_cell_length_b 13.2586(11)
_cell_length_c 13.8335(12)
_cell_angle_alpha 79.822(3)
_cell_angle_beta 75.146(3)
_cell_angle_gamma 73.305(3)
_cell_volume 1472.7(2)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 3261
_cell_measurement_temperature 120
_cell_measurement_theta_max 23.98
_cell_measurement_theta_min 2.35
_shelx_estimated_absorpt_T_max 0.996
_shelx_estimated_absorpt_T_min 0.969
_exptl_absorpt_coefficient_mu 0.292
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.9294
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker, 2014) was used for absorption correction.
wR2(int) was 0.0711 before and 0.0570 after correction.
The Ratio of minimum to maximum transmission is 0.9294.
The \l/2 correction factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'light yellow'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier light
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.441
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description stick
_exptl_crystal_F_000 664
_exptl_crystal_size_max 0.11
_exptl_crystal_size_mid 0.03
_exptl_crystal_size_min 0.015
_exptl_special_details
; Data were collected in shutterless mode. Full sphere of reciprocal
space was nominally covered by 4 runs of 170 narrow-frame \w-scans (scan
width 1.0\%, 40s exposure), every run at a different \f angle.
Crystal to detector distance 3.49 cm.
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0862
_diffrn_reflns_av_unetI/netI 0.0837
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 23441
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 24.999
_diffrn_reflns_theta_max 24.999
_diffrn_reflns_theta_min 2.346
_diffrn_ambient_temperature 120.0
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type 'Bruker PHOTON 100 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 scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'Incoatec I\mS microsource'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 3435
_reflns_number_total 5185
_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 'SAINT v8.34A (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution 'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max 0.329
_refine_diff_density_min -0.306
_refine_diff_density_rms 0.066
_refine_ls_extinction_coef 0.0047(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref 1.014
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 409
_refine_ls_number_reflns 5185
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0931
_refine_ls_R_factor_gt 0.0460
_refine_ls_restrained_S_all 1.014
_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^)+(0.0368P)^2^+0.5979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0839
_refine_ls_wR_factor_ref 0.0981
_refine_special_details
; Methyl group C(37)H~3~ was treated as ideally disordered, C(38)~3~ as a rigid
body rotating around the C---C bond, with a common refined U(iso) for three H
atoms. Other H atoms - riding (constr).
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H,H,H,H,H) groups
2. Others
Uiso(H38A)=Uiso(H38B)=Uiso(H38C)=FVAR(1)
Fixed Sof: H37A(0.5) H37B(0.5) H37C(0.5) H37D(0.5) H37E(0.5) H37F(0.5)
3.a Aromatic/amide H refined with riding coordinates:
C2(H2), C5(H5), C8(H8), C11(H11), C14(H14), C15(H15), C16(H16), C17(H17),
C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C27(H27), C28(H28), C29(H29),
C32(H32), C33(H33), C34(H34), C35(H35)
3.b Disordered Me refined with riding coordinates:
C37(H37A,H37B,H37C,H37D,H37E,H37F)
3.c Idealised Me refined as rotating group:
C38(H38A,H38B,H38C)
;
_atom_sites_solution_hydrogens geom
_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
S1 S 0.25198(9) 0.04485(6) 0.44584(5) 0.01319(19) Uani 1 1 d . . . . .
S2 S 0.20216(10) 0.21549(6) 1.05430(6) 0.0223(2) Uani 1 1 d . . . . .
S3 S 0.59950(9) 0.62616(6) 0.22688(6) 0.0190(2) Uani 1 1 d . . . . .
O1 O 0.3776(2) -0.05037(14) 0.42325(14) 0.0201(5) Uani 1 1 d . . . . .
O2 O 0.1007(2) 0.06025(15) 0.41520(14) 0.0198(5) Uani 1 1 d . . . . .
N1 N 0.1955(3) 0.14201(17) 0.85667(16) 0.0139(6) Uani 1 1 d . . . . .
N2 N 0.4850(3) 0.43574(17) 0.33935(17) 0.0146(6) Uani 1 1 d . . . . .
C1 C 0.2214(3) 0.0634(2) 0.5734(2) 0.0112(6) Uani 1 1 d . . . . .
C2 C 0.1739(3) -0.0042(2) 0.6564(2) 0.0139(7) Uani 1 1 d . . . . .
H2 H 0.147372 -0.066527 0.648632 0.017 Uiso 1 1 calc R . . . .
C3 C 0.1652(3) 0.0203(2) 0.7523(2) 0.0151(7) Uani 1 1 d . . . . .
C4 C 0.1993(3) 0.1147(2) 0.7595(2) 0.0134(7) Uani 1 1 d . . . . .
C5 C 0.2468(3) 0.1821(2) 0.6751(2) 0.0147(7) Uani 1 1 d . . . . .
H5 H 0.268878 0.246055 0.682565 0.018 Uiso 1 1 calc R . . . .
C6 C 0.2616(3) 0.1558(2) 0.5809(2) 0.0120(6) Uani 1 1 d . . . . .
C7 C 0.3234(3) 0.2103(2) 0.4823(2) 0.0130(6) Uani 1 1 d . . . . .
C8 C 0.3781(3) 0.3019(2) 0.4619(2) 0.0148(7) Uani 1 1 d . . . . .
H8 H 0.382306 0.336681 0.515267 0.018 Uiso 1 1 calc R . . . .
C9 C 0.4266(3) 0.3420(2) 0.3627(2) 0.0133(7) Uani 1 1 d . . . . .
C10 C 0.4259(3) 0.2920(2) 0.2817(2) 0.0136(7) Uani 1 1 d . . . . .
C11 C 0.3759(3) 0.1981(2) 0.3031(2) 0.0139(7) Uani 1 1 d . . . . .
H11 H 0.376247 0.161162 0.250043 0.017 Uiso 1 1 calc R . . . .
C12 C 0.3259(3) 0.1594(2) 0.4020(2) 0.0112(6) Uani 1 1 d . . . . .
C13 C 0.3524(3) 0.1229(2) 0.8787(2) 0.0137(7) Uani 1 1 d . . . . .
C14 C 0.4922(4) 0.0688(2) 0.8161(2) 0.0160(7) Uani 1 1 d . . . . .
H14 H 0.481606 0.043627 0.758572 0.019 Uiso 1 1 calc R . . . .
C15 C 0.6463(4) 0.0504(2) 0.8352(2) 0.0196(7) Uani 1 1 d . . . . .
H15 H 0.739899 0.012843 0.791292 0.024 Uiso 1 1 calc R . . . .
C16 C 0.6636(4) 0.0868(2) 0.9182(2) 0.0207(7) Uani 1 1 d . . . . .
H16 H 0.769088 0.075384 0.931644 0.025 Uiso 1 1 calc R . . . .
C17 C 0.5261(4) 0.1398(2) 0.9814(2) 0.0196(7) Uani 1 1 d . . . . .
H17 H 0.537868 0.165426 1.038345 0.023 Uiso 1 1 calc R . . . .
C18 C 0.3717(3) 0.1565(2) 0.9640(2) 0.0148(7) Uani 1 1 d . . . . .
C19 C 0.0630(3) 0.2272(2) 0.8928(2) 0.0162(7) Uani 1 1 d . . . . .
C20 C -0.0684(4) 0.2676(2) 0.8455(2) 0.0189(7) Uani 1 1 d . . . . .
H20 H -0.068605 0.237993 0.787887 0.023 Uiso 1 1 calc R . . . .
C21 C -0.1991(4) 0.3503(2) 0.8810(2) 0.0223(7) Uani 1 1 d . . . . .
H21 H -0.288984 0.375171 0.848679 0.027 Uiso 1 1 calc R . . . .
C22 C -0.1991(4) 0.3966(2) 0.9628(2) 0.0229(8) Uani 1 1 d . . . . .
H22 H -0.286169 0.455090 0.985455 0.027 Uiso 1 1 calc R . . . .
C23 C -0.0702(4) 0.3563(2) 1.0115(2) 0.0213(7) Uani 1 1 d . . . . .
H23 H -0.069501 0.387475 1.068097 0.026 Uiso 1 1 calc R . . . .
C24 C 0.0575(3) 0.2714(2) 0.9787(2) 0.0169(7) Uani 1 1 d . . . . .
C25 C 0.6575(3) 0.4208(2) 0.3139(2) 0.0145(7) Uani 1 1 d . . . . .
C26 C 0.7626(4) 0.3223(2) 0.3336(2) 0.0194(7) Uani 1 1 d . . . . .
H26 H 0.718387 0.264249 0.365959 0.023 Uiso 1 1 calc R . . . .
C27 C 0.9307(4) 0.3081(2) 0.3067(2) 0.0225(7) Uani 1 1 d . . . . .
H27 H 1.000969 0.239897 0.318977 0.027 Uiso 1 1 calc R . . . .
C28 C 0.9971(4) 0.3920(2) 0.2622(2) 0.0238(8) Uani 1 1 d . . . . .
H28 H 1.112650 0.382108 0.244566 0.029 Uiso 1 1 calc R . . . .
C29 C 0.8943(4) 0.4906(2) 0.2435(2) 0.0200(7) Uani 1 1 d . . . . .
H29 H 0.939362 0.549257 0.214790 0.024 Uiso 1 1 calc R . . . .
C30 C 0.7259(3) 0.5046(2) 0.2664(2) 0.0159(7) Uani 1 1 d . . . . .
C31 C 0.3768(3) 0.5342(2) 0.3661(2) 0.0136(7) Uani 1 1 d . . . . .
C32 C 0.2221(4) 0.5432(2) 0.4286(2) 0.0213(7) Uani 1 1 d . . . . .
H32 H 0.184166 0.481354 0.454839 0.026 Uiso 1 1 calc R . . . .
C33 C 0.1231(4) 0.6408(2) 0.4528(2) 0.0247(8) Uani 1 1 d . . . . .
H33 H 0.016864 0.645243 0.494508 0.030 Uiso 1 1 calc R . . . .
C34 C 0.1747(4) 0.7318(2) 0.4180(2) 0.0247(8) Uani 1 1 d . . . . .
H34 H 0.107326 0.798301 0.437804 0.030 Uiso 1 1 calc R . . . .
C35 C 0.3258(4) 0.7248(2) 0.3541(2) 0.0201(7) Uani 1 1 d . . . . .
H35 H 0.362869 0.787185 0.329255 0.024 Uiso 1 1 calc R . . . .
C36 C 0.4243(3) 0.6281(2) 0.3255(2) 0.0151(7) Uani 1 1 d . . . . .
C37 C 0.1257(4) -0.0565(2) 0.8440(2) 0.0185(7) Uani 1 1 d . . . . .
H37A H 0.105470 -0.117696 0.823278 0.022 Uiso 0.5 1 calc R . P . .
H37B H 0.218324 -0.080493 0.877387 0.022 Uiso 0.5 1 calc R . P . .
H37C H 0.027728 -0.021260 0.890604 0.022 Uiso 0.5 1 calc R . P . .
H37D H 0.128878 -0.028603 0.904235 0.022 Uiso 0.5 1 calc R . P . .
H37E H 0.016024 -0.065806 0.850126 0.022 Uiso 0.5 1 calc R . P . .
H37F H 0.206620 -0.125039 0.836908 0.022 Uiso 0.5 1 calc R . P . .
C38 C 0.4785(4) 0.3373(2) 0.1748(2) 0.0205(7) Uani 1 1 d . . . . .
H38A H 0.597409 0.310934 0.152184 0.040(6) Uiso 1 1 calc GR . . . .
H38B H 0.449537 0.414771 0.170783 0.040(6) Uiso 1 1 calc GR . . . .
H38C H 0.422971 0.315716 0.131700 0.040(6) 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
S1 0.0171(4) 0.0120(4) 0.0122(4) -0.0004(3) -0.0035(3) -0.0067(3)
S2 0.0219(5) 0.0290(5) 0.0147(4) -0.0064(4) -0.0056(4) -0.0009(4)
S3 0.0198(5) 0.0148(4) 0.0209(4) 0.0023(3) -0.0020(3) -0.0070(3)
O1 0.0260(13) 0.0108(11) 0.0210(12) -0.0049(9) -0.0017(10) -0.0021(9)
O2 0.0202(12) 0.0251(12) 0.0202(12) 0.0027(9) -0.0099(9) -0.0132(10)
N1 0.0135(14) 0.0162(14) 0.0130(13) -0.0038(11) -0.0034(11) -0.0033(11)
N2 0.0132(14) 0.0106(13) 0.0202(14) -0.0006(10) -0.0022(11) -0.0054(11)
C1 0.0086(15) 0.0143(16) 0.0111(15) -0.0033(12) -0.0039(12) -0.0009(13)
C2 0.0133(16) 0.0126(16) 0.0174(16) -0.0007(13) -0.0044(13) -0.0054(13)
C3 0.0132(16) 0.0155(16) 0.0153(16) 0.0010(13) -0.0050(13) -0.0015(13)
C4 0.0135(17) 0.0151(16) 0.0121(16) -0.0034(13) -0.0019(13) -0.0039(13)
C5 0.0165(17) 0.0121(16) 0.0167(16) -0.0025(13) -0.0053(13) -0.0033(13)
C6 0.0109(16) 0.0084(15) 0.0158(16) -0.0004(12) -0.0042(13) -0.0003(12)
C7 0.0100(16) 0.0139(16) 0.0128(16) 0.0009(12) -0.0035(12) -0.0001(13)
C8 0.0132(16) 0.0149(16) 0.0187(17) -0.0040(13) -0.0034(13) -0.0058(13)
C9 0.0108(16) 0.0088(15) 0.0203(17) -0.0001(13) -0.0022(13) -0.0044(13)
C10 0.0110(16) 0.0128(16) 0.0151(16) 0.0002(12) -0.0026(13) -0.0015(13)
C11 0.0123(16) 0.0138(16) 0.0163(16) -0.0051(13) -0.0033(13) -0.0023(13)
C12 0.0090(15) 0.0104(15) 0.0137(16) -0.0015(12) -0.0012(12) -0.0024(12)
C13 0.0184(17) 0.0093(15) 0.0141(16) 0.0029(12) -0.0054(13) -0.0058(13)
C14 0.0224(18) 0.0147(17) 0.0119(16) 0.0005(13) -0.0057(13) -0.0056(14)
C15 0.0174(17) 0.0192(17) 0.0183(17) 0.0025(13) -0.0002(14) -0.0044(14)
C16 0.0148(17) 0.0216(18) 0.0266(18) -0.0009(15) -0.0096(14) -0.0024(14)
C17 0.0231(19) 0.0191(17) 0.0184(17) -0.0026(13) -0.0078(14) -0.0050(14)
C18 0.0171(17) 0.0130(16) 0.0142(16) 0.0011(12) -0.0034(13) -0.0051(13)
C19 0.0164(17) 0.0181(17) 0.0148(16) -0.0018(13) -0.0001(13) -0.0086(14)
C20 0.0171(18) 0.0232(18) 0.0181(17) -0.0019(14) -0.0032(14) -0.0085(15)
C21 0.0155(18) 0.0272(19) 0.0238(18) 0.0010(15) -0.0048(14) -0.0067(15)
C22 0.0181(18) 0.0237(19) 0.0214(18) -0.0041(15) 0.0015(14) -0.0008(15)
C23 0.0213(18) 0.0286(19) 0.0146(17) -0.0076(14) -0.0003(14) -0.0074(16)
C24 0.0175(17) 0.0193(17) 0.0140(16) 0.0021(13) -0.0040(13) -0.0068(14)
C25 0.0150(17) 0.0149(16) 0.0149(16) -0.0015(13) -0.0033(13) -0.0056(14)
C26 0.0221(19) 0.0133(17) 0.0233(18) 0.0017(13) -0.0051(14) -0.0073(14)
C27 0.0161(18) 0.0205(18) 0.0287(19) 0.0009(14) -0.0074(14) -0.0009(14)
C28 0.0136(18) 0.029(2) 0.0275(19) -0.0051(15) -0.0037(14) -0.0037(15)
C29 0.0197(18) 0.0205(18) 0.0209(17) -0.0028(14) -0.0004(14) -0.0105(15)
C30 0.0178(17) 0.0144(16) 0.0153(16) -0.0031(13) -0.0022(13) -0.0040(14)
C31 0.0155(17) 0.0130(16) 0.0144(16) -0.0019(12) -0.0065(13) -0.0037(13)
C32 0.0208(18) 0.0148(17) 0.0280(19) -0.0005(14) -0.0021(15) -0.0077(14)
C33 0.0115(17) 0.0231(19) 0.034(2) -0.0068(15) 0.0032(15) -0.0002(15)
C34 0.0216(19) 0.0184(18) 0.033(2) -0.0058(15) -0.0074(16) -0.0008(15)
C35 0.0241(19) 0.0141(17) 0.0256(18) 0.0003(14) -0.0109(15) -0.0071(14)
C36 0.0154(17) 0.0148(17) 0.0165(16) -0.0002(13) -0.0068(13) -0.0038(13)
C37 0.0259(18) 0.0178(17) 0.0156(16) 0.0016(13) -0.0063(14) -0.0120(14)
C38 0.0272(19) 0.0186(17) 0.0157(17) -0.0014(13) -0.0024(14) -0.0081(15)
_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
S1 O1 1.4358(19) . ?
S1 O2 1.4368(19) . ?
S1 C1 1.767(3) . ?
S1 C12 1.768(3) . ?
S2 C18 1.759(3) . ?
S2 C24 1.761(3) . ?
S3 C30 1.757(3) . ?
S3 C36 1.766(3) . ?
N1 C4 1.442(3) . ?
N1 C13 1.421(3) . ?
N1 C19 1.420(3) . ?
N2 C9 1.430(3) . ?
N2 C25 1.418(3) . ?
N2 C31 1.420(3) . ?
C1 C2 1.378(4) . ?
C1 C6 1.394(4) . ?
C2 C3 1.399(4) . ?
C3 C4 1.392(4) . ?
C3 C37 1.512(4) . ?
C4 C5 1.389(4) . ?
C5 C6 1.373(4) . ?
C6 C7 1.474(4) . ?
C7 C8 1.388(4) . ?
C7 C12 1.391(4) . ?
C8 C9 1.385(4) . ?
C9 C10 1.402(4) . ?
C10 C11 1.394(4) . ?
C10 C38 1.501(4) . ?
C11 C12 1.379(4) . ?
C13 C14 1.389(4) . ?
C13 C18 1.397(4) . ?
C14 C15 1.381(4) . ?
C15 C16 1.379(4) . ?
C16 C17 1.376(4) . ?
C17 C18 1.378(4) . ?
C19 C20 1.392(4) . ?
C19 C24 1.399(4) . ?
C20 C21 1.389(4) . ?
C21 C22 1.379(4) . ?
C22 C23 1.385(4) . ?
C23 C24 1.384(4) . ?
C25 C26 1.391(4) . ?
C25 C30 1.395(4) . ?
C26 C27 1.383(4) . ?
C27 C28 1.378(4) . ?
C28 C29 1.381(4) . ?
C29 C30 1.386(4) . ?
C31 C32 1.390(4) . ?
C31 C36 1.402(4) . ?
C32 C33 1.376(4) . ?
C33 C34 1.374(4) . ?
C34 C35 1.375(4) . ?
C35 C36 1.383(4) . ?
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 S1 O2 117.70(12) . . ?
O1 S1 C1 110.06(12) . . ?
O1 S1 C12 111.90(12) . . ?
O2 S1 C1 112.66(12) . . ?
O2 S1 C12 108.89(12) . . ?
C1 S1 C12 92.92(13) . . ?
C18 S2 C24 100.29(14) . . ?
C30 S3 C36 98.90(13) . . ?
C13 N1 C4 114.3(2) . . ?
C19 N1 C4 115.7(2) . . ?
C19 N1 C13 121.8(2) . . ?
C25 N2 C9 116.5(2) . . ?
C25 N2 C31 121.7(2) . . ?
C31 N2 C9 119.8(2) . . ?
C2 C1 S1 126.8(2) . . ?
C2 C1 C6 122.6(2) . . ?
C6 C1 S1 110.4(2) . . ?
C1 C2 C3 119.1(2) . . ?
C2 C3 C37 120.1(2) . . ?
C4 C3 C2 118.0(2) . . ?
C4 C3 C37 121.9(2) . . ?
C3 C4 N1 120.0(2) . . ?
C5 C4 N1 117.8(2) . . ?
C5 C4 C3 122.1(3) . . ?
C6 C5 C4 119.7(3) . . ?
C1 C6 C7 113.0(2) . . ?
C5 C6 C1 118.3(2) . . ?
C5 C6 C7 128.6(2) . . ?
C8 C7 C6 128.5(3) . . ?
C8 C7 C12 118.6(3) . . ?
C12 C7 C6 113.0(2) . . ?
C9 C8 C7 119.1(3) . . ?
C8 C9 N2 120.4(3) . . ?
C8 C9 C10 122.3(3) . . ?
C10 C9 N2 117.3(2) . . ?
C9 C10 C38 121.2(2) . . ?
C11 C10 C9 118.1(3) . . ?
C11 C10 C38 120.7(3) . . ?
C12 C11 C10 119.3(3) . . ?
C7 C12 S1 110.6(2) . . ?
C11 C12 S1 126.8(2) . . ?
C11 C12 C7 122.6(3) . . ?
C14 C13 N1 120.8(2) . . ?
C14 C13 C18 117.7(3) . . ?
C18 C13 N1 121.6(2) . . ?
C15 C14 C13 121.9(3) . . ?
C16 C15 C14 119.7(3) . . ?
C17 C16 C15 119.1(3) . . ?
C16 C17 C18 121.5(3) . . ?
C13 C18 S2 121.7(2) . . ?
C17 C18 S2 118.2(2) . . ?
C17 C18 C13 120.1(3) . . ?
C20 C19 N1 121.0(2) . . ?
C20 C19 C24 117.7(3) . . ?
C24 C19 N1 121.3(3) . . ?
C21 C20 C19 121.3(3) . . ?
C22 C21 C20 120.3(3) . . ?
C21 C22 C23 119.0(3) . . ?
C24 C23 C22 120.9(3) . . ?
C19 C24 S2 121.7(2) . . ?
C23 C24 S2 117.5(2) . . ?
C23 C24 C19 120.6(3) . . ?
C26 C25 N2 121.2(2) . . ?
C26 C25 C30 118.4(3) . . ?
C30 C25 N2 120.5(3) . . ?
C27 C26 C25 120.7(3) . . ?
C28 C27 C26 120.5(3) . . ?
C27 C28 C29 119.5(3) . . ?
C28 C29 C30 120.4(3) . . ?
C25 C30 S3 119.9(2) . . ?
C29 C30 S3 119.4(2) . . ?
C29 C30 C25 120.5(3) . . ?
C32 C31 N2 123.2(2) . . ?
C32 C31 C36 117.6(3) . . ?
C36 C31 N2 119.2(2) . . ?
C33 C32 C31 120.7(3) . . ?
C34 C33 C32 121.4(3) . . ?
C33 C34 C35 118.7(3) . . ?
C34 C35 C36 120.7(3) . . ?
C31 C36 S3 120.3(2) . . ?
C35 C36 S3 118.7(2) . . ?
C35 C36 C31 120.6(3) . . ?
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 C13 C18 S2 4.9(4) . . . . ?
N1 C19 C24 S2 -6.8(4) . . . . ?
N2 C25 C30 S3 -6.1(4) . . . . ?
N2 C31 C36 S3 10.4(4) . . . . ?
C3 C4 N1 C13 101.3(3) . . . . ?
C3 C4 N1 C19 -109.4(3) . . . . ?
C5 C4 N1 C13 -75.1(3) . . . . ?
C5 C4 N1 C19 74.2(3) . . . . ?
C8 C9 N2 C25 98.5(3) . . . . ?
C8 C9 N2 C31 -65.8(4) . . . . ?
C10 C9 N2 C25 -79.6(3) . . . . ?
C10 C9 N2 C31 116.1(3) . . . . ?
C13 C18 S2 C24 -27.5(3) . . . . ?
C14 C13 N1 C4 -8.5(4) . . . . ?
C14 C13 N1 C19 -155.7(3) . . . . ?
C14 C13 C18 S2 -174.4(2) . . . . ?
C14 C13 C18 C17 2.8(4) . . . . ?
C17 C18 S2 C24 155.3(2) . . . . ?
C17 C18 C13 N1 -177.9(2) . . . . ?
C18 C13 N1 C4 172.3(2) . . . . ?
C18 C13 N1 C19 25.1(4) . . . . ?
C19 C24 S2 C18 28.4(3) . . . . ?
C20 C19 N1 C4 11.1(4) . . . . ?
C20 C19 N1 C13 157.9(2) . . . . ?
C20 C19 C24 S2 171.3(2) . . . . ?
C23 C24 S2 C18 -156.5(2) . . . . ?
C23 C24 C19 N1 178.3(3) . . . . ?
C23 C24 C19 C20 -3.6(4) . . . . ?
C24 C19 N1 C4 -170.8(2) . . . . ?
C24 C19 N1 C13 -24.0(4) . . . . ?
C25 C30 S3 C36 35.2(2) . . . . ?
C26 C25 N2 C9 -14.7(4) . . . . ?
C26 C25 N2 C31 149.3(3) . . . . ?
C26 C25 C30 S3 172.6(2) . . . . ?
C29 C30 S3 C36 -149.4(2) . . . . ?
C29 C30 C25 N2 178.6(3) . . . . ?
C29 C30 C25 C26 -2.7(4) . . . . ?
C30 C25 N2 C9 163.9(3) . . . . ?
C30 C25 N2 C31 -32.1(4) . . . . ?
C31 C36 S3 C30 -37.6(3) . . . . ?
C32 C31 N2 C9 10.7(4) . . . . ?
C32 C31 N2 C25 -152.8(3) . . . . ?
C32 C31 C36 S3 -167.4(2) . . . . ?
C32 C31 C36 C35 5.6(4) . . . . ?
C35 C36 S3 C30 149.3(2) . . . . ?
C35 C36 C31 N2 -176.6(2) . . . . ?
C36 C31 N2 C9 -167.1(2) . . . . ?
C36 C31 N2 C25 29.4(4) . . . . ?
_shelx_res_file
;
TITL 15srv293
15srv293.res
created by SHELXL-2018/3 at 14:00:09 on 06-Dec-2018
CELL 0.71073 8.7268 13.2586 13.8335 79.8215 75.146 73.3054
ZERR 2 0.0008 0.0011 0.0012 0.0028 0.0027 0.0027
LATT 1
SFAC C H N O S
UNIT 76 52 4 4 6
L.S. 7
PLAN 10
SIZE 0.015 0.03 0.11
TEMP -153.15
CONF C3 C4 N1 C13
CONF C5 C4 N1 C13
CONF C3 C4 N1 C19
CONF C5 C4 N1 C19
CONF C14 C13 N1 C4
CONF C18 C13 N1 C4
CONF C14 C13 N1 C19
CONF C18 C13 N1 C19
CONF N1 C13 C18 S2
CONF C14 C13 C18 S2
CONF C17 C18 C13 N1
CONF C14 C13 C18 C17
CONF C13 C18 S2 C24
CONF C17 C18 S2 C24
CONF C23 C24 S2 C18
CONF C19 C24 S2 C18
CONF N1 C19 C24 S2
CONF C23 C24 C19 N1
CONF C20 C19 C24 S2
CONF C23 C24 C19 C20
CONF C24 C19 N1 C4
CONF C20 C19 N1 C4
CONF C24 C19 N1 C13
CONF C20 C19 N1 C13
CONF C10 C9 N2 C31
CONF C8 C9 N2 C31
CONF C10 C9 N2 C25
CONF C8 C9 N2 C25
CONF C32 C31 N2 C9
CONF C36 C31 N2 C9
CONF C32 C31 N2 C25
CONF C36 C31 N2 C25
CONF N2 C31 C36 S3
CONF C32 C31 C36 S3
CONF C35 C36 C31 N2
CONF C32 C31 C36 C35
CONF C31 C36 S3 C30
CONF C35 C36 S3 C30
CONF C29 C30 S3 C36
CONF C25 C30 S3 C36
CONF N2 C25 C30 S3
CONF C29 C30 C25 N2
CONF C26 C25 C30 S3
CONF C29 C30 C25 C26
CONF C30 C25 N2 C9
CONF C26 C25 N2 C9
CONF C30 C25 N2 C31
CONF C26 C25 N2 C31
fmap 2 53
acta
OMIT -3 50
REM
REM
REM
WGHT 0.036800 0.597900
EXTI 0.004683
FVAR 0.21937 0.03998
S1 5 0.251978 0.044847 0.445836 11.00000 0.01714 0.01200 =
0.01217 -0.00041 -0.00351 -0.00667
S2 5 0.202162 0.215493 1.054296 11.00000 0.02191 0.02901 =
0.01466 -0.00638 -0.00555 -0.00086
S3 5 0.599500 0.626157 0.226881 11.00000 0.01982 0.01478 =
0.02091 0.00225 -0.00197 -0.00704
O1 4 0.377559 -0.050372 0.423255 11.00000 0.02599 0.01080 =
0.02099 -0.00491 -0.00167 -0.00206
O2 4 0.100750 0.060254 0.415198 11.00000 0.02016 0.02510 =
0.02018 0.00274 -0.00995 -0.01322
N1 3 0.195483 0.142005 0.856670 11.00000 0.01350 0.01618 =
0.01299 -0.00379 -0.00337 -0.00332
N2 3 0.484974 0.435744 0.339352 11.00000 0.01320 0.01062 =
0.02023 -0.00059 -0.00219 -0.00544
C1 1 0.221438 0.063408 0.573418 11.00000 0.00862 0.01434 =
0.01111 -0.00331 -0.00386 -0.00087
C2 1 0.173876 -0.004182 0.656424 11.00000 0.01329 0.01256 =
0.01740 -0.00066 -0.00445 -0.00540
AFIX 43
H2 2 0.147372 -0.066527 0.648632 11.00000 -1.20000
AFIX 0
C3 1 0.165175 0.020299 0.752293 11.00000 0.01321 0.01551 =
0.01530 0.00105 -0.00503 -0.00152
C4 1 0.199338 0.114655 0.759547 11.00000 0.01346 0.01513 =
0.01212 -0.00335 -0.00190 -0.00392
C5 1 0.246788 0.182066 0.675131 11.00000 0.01648 0.01206 =
0.01668 -0.00253 -0.00532 -0.00334
AFIX 43
H5 2 0.268878 0.246055 0.682565 11.00000 -1.20000
AFIX 0
C6 1 0.261614 0.155800 0.580918 11.00000 0.01087 0.00842 =
0.01582 -0.00037 -0.00423 -0.00027
C7 1 0.323364 0.210289 0.482302 11.00000 0.00996 0.01395 =
0.01282 0.00089 -0.00348 -0.00012
C8 1 0.378138 0.301925 0.461892 11.00000 0.01315 0.01490 =
0.01866 -0.00402 -0.00340 -0.00579
AFIX 43
H8 2 0.382306 0.336681 0.515267 11.00000 -1.20000
AFIX 0
C9 1 0.426636 0.342016 0.362661 11.00000 0.01079 0.00875 =
0.02031 -0.00013 -0.00219 -0.00444
C10 1 0.425872 0.291961 0.281658 11.00000 0.01099 0.01284 =
0.01511 0.00023 -0.00261 -0.00149
C11 1 0.375887 0.198085 0.303065 11.00000 0.01227 0.01384 =
0.01626 -0.00511 -0.00330 -0.00230
AFIX 43
H11 2 0.376247 0.161162 0.250043 11.00000 -1.20000
AFIX 0
C12 1 0.325914 0.159367 0.401990 11.00000 0.00897 0.01036 =
0.01368 -0.00147 -0.00122 -0.00243
C13 1 0.352374 0.122913 0.878673 11.00000 0.01840 0.00933 =
0.01411 0.00294 -0.00536 -0.00579
C14 1 0.492219 0.068752 0.816117 11.00000 0.02240 0.01469 =
0.01193 0.00049 -0.00574 -0.00561
AFIX 43
H14 2 0.481606 0.043627 0.758572 11.00000 -1.20000
AFIX 0
C15 1 0.646285 0.050375 0.835177 11.00000 0.01735 0.01918 =
0.01826 0.00255 -0.00023 -0.00439
AFIX 43
H15 2 0.739899 0.012843 0.791292 11.00000 -1.20000
AFIX 0
C16 1 0.663591 0.086777 0.918242 11.00000 0.01479 0.02156 =
0.02662 -0.00087 -0.00960 -0.00242
AFIX 43
H16 2 0.769088 0.075384 0.931644 11.00000 -1.20000
AFIX 0
C17 1 0.526102 0.139787 0.981413 11.00000 0.02309 0.01912 =
0.01837 -0.00263 -0.00780 -0.00503
AFIX 43
H17 2 0.537868 0.165426 1.038345 11.00000 -1.20000
AFIX 0
C18 1 0.371667 0.156545 0.963982 11.00000 0.01714 0.01298 =
0.01420 0.00114 -0.00340 -0.00509
C19 1 0.062999 0.227236 0.892830 11.00000 0.01640 0.01808 =
0.01480 -0.00179 -0.00010 -0.00860
C20 1 -0.068356 0.267604 0.845550 11.00000 0.01712 0.02318 =
0.01809 -0.00193 -0.00324 -0.00849
AFIX 43
H20 2 -0.068605 0.237993 0.787887 11.00000 -1.20000
AFIX 0
C21 1 -0.199106 0.350319 0.880974 11.00000 0.01555 0.02725 =
0.02382 0.00098 -0.00477 -0.00670
AFIX 43
H21 2 -0.288984 0.375171 0.848679 11.00000 -1.20000
AFIX 0
C22 1 -0.199122 0.396567 0.962810 11.00000 0.01808 0.02374 =
0.02136 -0.00408 0.00145 -0.00084
AFIX 43
H22 2 -0.286169 0.455090 0.985455 11.00000 -1.20000
AFIX 0
C23 1 -0.070231 0.356349 1.011463 11.00000 0.02128 0.02862 =
0.01462 -0.00757 -0.00035 -0.00737
AFIX 43
H23 2 -0.069501 0.387475 1.068097 11.00000 -1.20000
AFIX 0
C24 1 0.057511 0.271427 0.978683 11.00000 0.01754 0.01926 =
0.01404 0.00207 -0.00396 -0.00682
C25 1 0.657472 0.420820 0.313918 11.00000 0.01498 0.01488 =
0.01491 -0.00150 -0.00334 -0.00563
C26 1 0.762582 0.322344 0.333639 11.00000 0.02212 0.01326 =
0.02334 0.00166 -0.00506 -0.00732
AFIX 43
H26 2 0.718387 0.264249 0.365959 11.00000 -1.20000
AFIX 0
C27 1 0.930725 0.308078 0.306710 11.00000 0.01609 0.02048 =
0.02869 0.00087 -0.00739 -0.00094
AFIX 43
H27 2 1.000969 0.239897 0.318977 11.00000 -1.20000
AFIX 0
C28 1 0.997114 0.392008 0.262228 11.00000 0.01364 0.02940 =
0.02746 -0.00514 -0.00372 -0.00366
AFIX 43
H28 2 1.112650 0.382108 0.244566 11.00000 -1.20000
AFIX 0
C29 1 0.894334 0.490646 0.243525 11.00000 0.01973 0.02054 =
0.02094 -0.00277 -0.00042 -0.01046
AFIX 43
H29 2 0.939362 0.549257 0.214790 11.00000 -1.20000
AFIX 0
C30 1 0.725887 0.504643 0.266422 11.00000 0.01778 0.01442 =
0.01528 -0.00308 -0.00222 -0.00398
C31 1 0.376838 0.534239 0.366113 11.00000 0.01547 0.01304 =
0.01443 -0.00193 -0.00648 -0.00373
C32 1 0.222071 0.543192 0.428590 11.00000 0.02079 0.01477 =
0.02799 -0.00050 -0.00214 -0.00775
AFIX 43
H32 2 0.184166 0.481354 0.454839 11.00000 -1.20000
AFIX 0
C33 1 0.123141 0.640764 0.452820 11.00000 0.01153 0.02306 =
0.03367 -0.00683 0.00315 -0.00015
AFIX 43
H33 2 0.016864 0.645243 0.494508 11.00000 -1.20000
AFIX 0
C34 1 0.174721 0.731819 0.418040 11.00000 0.02159 0.01838 =
0.03329 -0.00581 -0.00741 -0.00080
AFIX 43
H34 2 0.107326 0.798301 0.437804 11.00000 -1.20000
AFIX 0
C35 1 0.325755 0.724844 0.354084 11.00000 0.02407 0.01411 =
0.02562 0.00032 -0.01093 -0.00707
AFIX 43
H35 2 0.362869 0.787185 0.329255 11.00000 -1.20000
AFIX 0
C36 1 0.424308 0.628079 0.325469 11.00000 0.01544 0.01477 =
0.01651 -0.00024 -0.00677 -0.00384
C37 1 0.125703 -0.056545 0.843951 11.00000 0.02592 0.01780 =
0.01559 0.00162 -0.00629 -0.01204
AFIX 123
H37A 2 0.105470 -0.117696 0.823278 10.50000 -1.20000
H37B 2 0.218324 -0.080493 0.877387 10.50000 -1.20000
H37C 2 0.027728 -0.021260 0.890604 10.50000 -1.20000
H37D 2 0.128878 -0.028603 0.904235 10.50000 -1.20000
H37E 2 0.016024 -0.065806 0.850126 10.50000 -1.20000
H37F 2 0.206620 -0.125039 0.836908 10.50000 -1.20000
AFIX 0
C38 1 0.478517 0.337279 0.174808 11.00000 0.02716 0.01855 =
0.01571 -0.00136 -0.00243 -0.00812
AFIX 137
H38A 2 0.597409 0.310934 0.152184 11.00000 21.00000
H38B 2 0.449537 0.414771 0.170783 11.00000 21.00000
H38C 2 0.422971 0.315716 0.131700 11.00000 21.00000
AFIX 0
HKLF 4
REM 15srv293
REM wR2 = 0.0981, GooF = S = 1.014, Restrained GooF = 1.014 for all data
REM R1 = 0.0460 for 3435 Fo > 4sig(Fo) and 0.0931 for all 5185 data
REM 409 parameters refined using 0 restraints
END
WGHT 0.0366 0.6100
REM Highest difference peak 0.329, deepest hole -0.306, 1-sigma level 0.066
Q1 1 0.2292 0.0621 0.5192 11.00000 0.05 0.33
Q2 1 0.3232 0.0972 0.4205 11.00000 0.05 0.32
Q3 1 0.2985 0.2192 0.9873 11.00000 0.05 0.28
Q4 1 0.4884 0.6225 0.2755 11.00000 0.05 0.27
Q5 1 0.5606 0.0813 0.2547 11.00000 0.05 0.26
Q6 1 0.6847 0.4645 0.2755 11.00000 0.05 0.26
Q7 1 0.1416 0.0766 0.7592 11.00000 0.05 0.26
Q8 1 0.6752 0.5558 0.2592 11.00000 0.05 0.25
Q9 1 -0.0347 0.7974 0.5437 11.00000 0.05 0.24
Q10 1 0.5246 0.1463 1.0988 11.00000 0.05 0.24
;
_shelx_res_checksum 98612
#===END
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CD2Cl2'
_exptl_crystal_preparation Luminescent
#######################################################################
#
# 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_8-16s487
_database_code_depnum_ccdc_archive 'CCDC 1884009'
loop_
_audit_author_name
_audit_author_address
'Andrei S. Batsanov'
;Durham University
United Kingdom
;
_audit_update_record
;
2018-12-10 deposited with the CCDC. 2019-05-29 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2018/3
_shelx_SHELXL_version_number 2018/3
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C44 H39 N2 O2 S3, C Cl3 D'
_chemical_formula_sum 'C45 H38 Cl3 D N2 O2 S3'
_chemical_formula_weight 843.32
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0032 0.0015 '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'
Cl Cl 0.1418 0.1507 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D D 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0108 0.0057 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1181 0.1169 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 11
_space_group_name_H-M_alt 'P 21/m'
_space_group_name_Hall '-P 2yb'
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
_cell_length_a 7.6155(19)
_cell_length_b 31.336(8)
_cell_length_c 8.892(2)
_cell_angle_alpha 90
_cell_angle_beta 108.991(5)
_cell_angle_gamma 90
_cell_volume 2006.4(9)
_cell_formula_units_Z 2
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9617
_cell_measurement_theta_min 2.35
_cell_measurement_theta_max 35.00
_exptl_crystal_description needle
_exptl_crystal_colour colourless
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.396
_exptl_crystal_F_000 876
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.115
_exptl_crystal_size_mid 0.015
_exptl_crystal_size_min 0.008
_exptl_absorpt_coefficient_mu 0.394
_shelx_estimated_absorpt_T_min 0.956
_shelx_estimated_absorpt_T_max 0.994
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6492
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_process_details
; SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
wR2(int) was 0.1572 before and 0.1101 after correction.
The Ratio of minimum to maximum transmission is 0.6492.
The \l/2 correction factor is Not present.
;
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.6889
_diffrn_measurement_device_type
'Dectris Pilatus 2M pixel-array photon-counting detector'
_diffrn_measurement_device 'dual air-bearing fixed-\c diffractometer'
_diffrn_measurement_method 'thin-slice \f and \w scans'
_diffrn_radiation_monochromator 'double crystal silicon 111'
_diffrn_radiation_type 'synchrotron '
_diffrn_radiation_source
'undulator, Beamline I19, Diamond Light Source, RAL'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 20383
_diffrn_reflns_av_unetI/netI 0.1132
_diffrn_reflns_av_R_equivalents 0.0891
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -38
_diffrn_reflns_limit_k_max 38
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_theta_min 2.520
_diffrn_reflns_theta_max 25.000
_diffrn_reflns_theta_full 25.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total 3922
_reflns_number_gt 3441
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_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.
;
_computing_data_collection
'Diamond I19 EH1 GDA (Allan et al., 2017), DIALS (Winter et al., 2018)'
_computing_cell_refinement 'APEX3 v2017.3-0 (Bruker AXS, 2005-2017)'
_computing_data_reduction
'cbf_to_sfrm.py (Johnson & Probert, 2016), SAINT V8.38A (Bruker AXS, 2017)'
_computing_structure_solution 'SHELXT-2018/2 (Sheldrick, 2015)'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015a)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_refine_special_details
; The methyl-phenothiazine moiety is disordered between two
orientations with methyl group on different sides of the dibenzothiophene
plane, refined with geometries restrained to similarity (SAME). Their
occupancies refined to 0.898(3) and 0.102(3). The minor orientation is
labelled B. The CDCl~3~ molecule is disordered between two positions related
by a mirror plane, Cl(1) lying on this plane and belonging to both positions.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1352P)^2^+4.6037P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens mixed
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 3922
_refine_ls_number_parameters 327
_refine_ls_number_restraints 271
_refine_ls_R_factor_all 0.1060
_refine_ls_R_factor_gt 0.0994
_refine_ls_wR_factor_ref 0.2703
_refine_ls_wR_factor_gt 0.2634
_refine_ls_goodness_of_fit_ref 1.059
_refine_ls_restrained_S_all 1.025
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
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
S1 S 0.94159(17) 0.750000 0.78073(18) 0.0301(4) Uani 1 2 d S T P . .
O1 O 1.0606(6) 0.750000 0.9446(6) 0.0521(13) Uani 1 2 d S T P . .
O2 O 1.0326(6) 0.750000 0.6613(6) 0.0438(11) Uani 1 2 d S T P . .
C1 C 0.7733(5) 0.70911(10) 0.7454(5) 0.0250(8) Uani 1 1 d . . . . .
C2 C 0.7983(5) 0.66590(11) 0.7294(5) 0.0268(8) Uani 1 1 d . . . . .
H2 H 0.919103 0.654915 0.744269 0.032 Uiso 1 1 calc R U . . .
C3 C 0.6466(5) 0.63852(10) 0.6915(4) 0.0238(7) Uani 1 1 d . . . . .
C4 C 0.4713(5) 0.65553(11) 0.6806(5) 0.0250(8) Uani 1 1 d D . . . .
C5 C 0.4513(5) 0.69935(11) 0.7024(5) 0.0259(8) Uani 1 1 d . . . . .
H5 H 0.333876 0.710434 0.698854 0.031 Uiso 1 1 calc R U . . .
C6 C 0.6006(5) 0.72640(10) 0.7289(4) 0.0247(8) Uani 1 1 d . . . . .
C7 C 0.6723(5) 0.59220(11) 0.6548(5) 0.0286(8) Uani 1 1 d . . . . .
H7 H 0.547554 0.578220 0.624135 0.034 Uiso 1 1 calc R U . . .
C8 C 0.7418(10) 0.58882(16) 0.5140(7) 0.0585(14) Uani 1 1 d . . . . .
H8A H 0.652001 0.602269 0.421097 0.088 Uiso 1 1 d R U . . .
H8B H 0.756223 0.558654 0.490895 0.088 Uiso 1 1 d R U . . .
H8C H 0.861979 0.603284 0.538535 0.088 Uiso 1 1 d R U . . .
C9 C 0.7985(9) 0.56862(14) 0.7988(7) 0.0564(14) Uani 1 1 d . . . . .
H9A H 0.923349 0.580992 0.829538 0.085 Uiso 1 1 d R U . . .
H9B H 0.804585 0.538354 0.772587 0.085 Uiso 1 1 d R U . . .
H9C H 0.749197 0.571261 0.887438 0.085 Uiso 1 1 d R U . . .
S2 S 0.21693(17) 0.54306(3) 0.47222(16) 0.0383(4) Uani 0.898(3) 1 d D . P A 1
N1 N 0.3086(6) 0.62937(12) 0.6384(8) 0.0264(8) Uani 0.898(3) 1 d D . P A 1
C10 C 0.3611(12) 0.6444(3) 0.9763(7) 0.0419(15) Uani 0.898(3) 1 d D . P A 1
H10A H 0.490337 0.653294 0.997373 0.063 Uiso 0.898(3) 1 d R U P A 1
H10B H 0.333719 0.643385 1.076542 0.063 Uiso 0.898(3) 1 d R U P A 1
H10C H 0.278050 0.664927 0.904191 0.063 Uiso 0.898(3) 1 d R U P A 1
C11 C 0.3004(5) 0.59456(12) 0.7380(6) 0.0275(9) Uani 0.898(3) 1 d D . P A 1
C12 C 0.2550(6) 0.55376(14) 0.6756(6) 0.0328(10) Uani 0.898(3) 1 d D . P A 1
C13 C 0.2482(7) 0.51894(15) 0.7719(7) 0.0414(11) Uani 0.898(3) 1 d D . P A 1
H13 H 0.213844 0.491433 0.727068 0.050 Uiso 0.898(3) 1 calc R U P A 1
C14 C 0.2919(8) 0.52534(17) 0.9319(7) 0.0483(12) Uani 0.898(3) 1 d D . P A 1
H14 H 0.295744 0.501680 0.999678 0.058 Uiso 0.898(3) 1 calc R U P A 1
C15 C 0.3306(8) 0.56565(19) 0.9963(7) 0.0438(12) Uani 0.898(3) 1 d D . P A 1
H15 H 0.356997 0.569363 1.107477 0.053 Uiso 0.898(3) 1 calc R U P A 1
C16 C 0.3317(6) 0.60123(15) 0.9014(6) 0.0351(10) Uani 0.898(3) 1 d D . P A 1
C17 C 0.1833(6) 0.63034(14) 0.4786(6) 0.0306(9) Uani 0.898(3) 1 d D . P A 1
C18 C 0.1313(6) 0.59299(14) 0.3912(6) 0.0342(10) Uani 0.898(3) 1 d D . P A 1
C19 C 0.0093(8) 0.5944(2) 0.2345(6) 0.0462(12) Uani 0.898(3) 1 d D . P A 1
H19 H -0.029341 0.568639 0.176865 0.055 Uiso 0.898(3) 1 calc R U P A 1
C20 C -0.0543(9) 0.6328(2) 0.1642(7) 0.0578(15) Uani 0.898(3) 1 d D . P A 1
H20 H -0.133187 0.633707 0.056624 0.069 Uiso 0.898(3) 1 calc R U P A 1
C21 C -0.0038(10) 0.6700(2) 0.2496(8) 0.0621(17) Uani 0.898(3) 1 d D . P A 1
H21 H -0.048736 0.696635 0.201252 0.074 Uiso 0.898(3) 1 calc R U P A 1
C22 C 0.112(3) 0.66862(19) 0.4053(11) 0.0487(15) Uani 0.898(3) 1 d D . P A 1
H22 H 0.144036 0.694462 0.463739 0.058 Uiso 0.898(3) 1 calc R U P A 1
S2B S 0.3051(16) 0.5275(3) 0.6972(13) 0.0383(4) Uani 0.102(3) 1 d D . P A 2
N1B N 0.334(5) 0.6256(10) 0.686(2) 0.026(14) Uiso 0.102(3) 1 d D . P A 2
C10B C 0.12(3) 0.6762(16) 0.412(9) 0.0487(15) Uani 0.102(3) 1 d D . P A 2
H10D H 0.178624 0.686776 0.519827 0.073 Uiso 0.102(3) 1 calc R U P A 2
H10E H 0.166800 0.691475 0.337574 0.073 Uiso 0.102(3) 1 calc R U P A 2
H10F H -0.016356 0.681005 0.381550 0.073 Uiso 0.102(3) 1 calc R U P A 2
C11B C 0.238(4) 0.6050(7) 0.542(2) 0.017(5) Uiso 0.102(3) 1 d D . P A 2
C12B C 0.221(5) 0.5610(7) 0.532(2) 0.032(6) Uiso 0.102(3) 1 d D . P A 2
C13B C 0.110(6) 0.5405(9) 0.394(3) 0.042(8) Uiso 0.102(3) 1 d D . P A 2
H13B H 0.065815 0.512257 0.395077 0.050 Uiso 0.102(3) 1 calc R U P A 2
C14B C 0.069(8) 0.5640(11) 0.256(3) 0.057(13) Uiso 0.102(3) 1 d D . P A 2
H14B H 0.033099 0.549681 0.156021 0.068 Uiso 0.102(3) 1 calc R U P A 2
C15B C 0.080(8) 0.6079(11) 0.260(3) 0.046(13) Uiso 0.102(3) 1 d D . P A 2
H15B H 0.036631 0.623638 0.163703 0.055 Uiso 0.102(3) 1 calc R U P A 2
C16B C 0.155(7) 0.6296(9) 0.405(3) 0.043(14) Uiso 0.102(3) 1 d D . P A 2
C17B C 0.331(5) 0.6062(7) 0.831(3) 0.017(5) Uiso 0.102(3) 1 d D . P A 2
C18B C 0.326(5) 0.5628(7) 0.853(2) 0.032(6) Uiso 0.102(3) 1 d D . P A 2
C19B C 0.333(8) 0.5462(10) 1.001(3) 0.042(8) Uiso 0.102(3) 1 d D . P A 2
H19B H 0.319072 0.516476 1.014453 0.050 Uiso 0.102(3) 1 calc R U P A 2
C20B C 0.361(9) 0.5736(11) 1.127(4) 0.067(15) Uiso 0.102(3) 1 d D . P A 2
H20B H 0.369730 0.562257 1.228186 0.080 Uiso 0.102(3) 1 calc R U P A 2
C21B C 0.377(7) 0.6168(11) 1.111(3) 0.049(11) Uiso 0.102(3) 1 d D . P A 2
H21B H 0.403953 0.635185 1.200489 0.058 Uiso 0.102(3) 1 calc R U P A 2
C22B C 0.353(13) 0.6327(10) 0.961(4) 0.05(3) Uiso 0.102(3) 1 d D . P A 2
H22B H 0.352132 0.662764 0.946432 0.059 Uiso 0.102(3) 1 calc R U P A 2
Cl1 Cl 0.5742(5) 0.750000 0.0778(3) 0.0822(8) Uani 1 2 d DS T P . .
Cl2 Cl 0.5856(5) 0.80174(11) 0.3420(3) 0.0607(8) Uani 0.5 1 d D . P B -1
Cl3 Cl 0.4253(16) 0.7214(2) 0.3195(6) 0.182(4) Uani 0.5 1 d D . P B -1
C1S C 0.4664(19) 0.7628(3) 0.2148(12) 0.080(5) Uani 0.5 1 d D . P B -1
D1S D 0.342603 0.775144 0.153516 0.096 Uiso 0.5 1 d R U 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
S1 0.0163(6) 0.0144(6) 0.0567(9) 0.000 0.0077(5) 0.000
O1 0.032(2) 0.031(2) 0.071(3) 0.000 -0.014(2) 0.000
O2 0.030(2) 0.0212(19) 0.087(3) 0.000 0.029(2) 0.000
C1 0.0172(16) 0.0127(15) 0.043(2) 0.0025(13) 0.0071(14) -0.0004(12)
C2 0.0194(16) 0.0145(15) 0.046(2) 0.0011(14) 0.0104(15) 0.0032(13)
C3 0.0211(16) 0.0139(15) 0.0377(19) 0.0008(13) 0.0114(14) 0.0017(12)
C4 0.0217(17) 0.0141(15) 0.041(2) -0.0010(13) 0.0124(14) -0.0014(12)
C5 0.0208(16) 0.0150(16) 0.043(2) -0.0002(14) 0.0121(14) 0.0026(13)
C6 0.0215(16) 0.0143(17) 0.0391(19) -0.0001(13) 0.0108(14) 0.0005(13)
C7 0.0232(17) 0.0133(15) 0.052(2) -0.0036(14) 0.0157(16) -0.0003(13)
C8 0.089(4) 0.029(2) 0.077(3) -0.009(2) 0.054(3) -0.002(2)
C9 0.076(4) 0.0192(19) 0.066(3) 0.0047(19) 0.013(3) 0.013(2)
S2 0.0372(7) 0.0192(6) 0.0568(8) -0.0089(5) 0.0130(6) -0.0044(4)
N1 0.0180(18) 0.0154(18) 0.045(3) 0.0029(17) 0.0084(18) -0.0010(13)
C10 0.045(4) 0.038(3) 0.044(3) -0.004(2) 0.017(2) -0.009(3)
C11 0.0185(18) 0.0178(17) 0.048(2) 0.0045(16) 0.0132(17) 0.0006(14)
C12 0.026(2) 0.020(2) 0.051(3) -0.0018(17) 0.0114(18) -0.0029(17)
C13 0.037(2) 0.024(2) 0.069(3) 0.005(2) 0.026(2) -0.0044(19)
C14 0.047(3) 0.034(2) 0.070(3) 0.015(2) 0.028(3) 0.002(2)
C15 0.038(3) 0.043(3) 0.051(3) 0.008(2) 0.015(2) -0.002(2)
C16 0.027(2) 0.031(2) 0.048(3) 0.0006(19) 0.013(2) -0.0007(18)
C17 0.022(2) 0.026(2) 0.042(3) -0.0037(17) 0.0086(19) -0.0033(16)
C18 0.027(2) 0.025(2) 0.050(2) -0.0068(17) 0.0107(18) -0.0037(17)
C19 0.046(3) 0.044(3) 0.043(3) -0.011(2) 0.007(2) -0.007(3)
C20 0.060(4) 0.057(3) 0.042(3) 0.000(2) -0.003(3) 0.000(3)
C21 0.067(4) 0.043(3) 0.059(3) 0.007(2) -0.004(3) 0.012(3)
C22 0.046(3) 0.030(3) 0.055(3) -0.004(2) -0.003(2) 0.009(5)
S2B 0.0372(7) 0.0192(6) 0.0568(8) -0.0089(5) 0.0130(6) -0.0044(4)
C10B 0.046(3) 0.030(3) 0.055(3) -0.004(2) -0.003(2) 0.009(5)
Cl1 0.132(2) 0.0614(13) 0.0619(13) 0.000 0.0440(14) 0.000
Cl2 0.0779(19) 0.0631(17) 0.0397(13) -0.0074(11) 0.0171(12) -0.0029(15)
Cl3 0.358(12) 0.130(5) 0.077(3) -0.036(3) 0.097(5) -0.148(7)
C1S 0.084(8) 0.094(14) 0.055(6) -0.020(6) 0.013(6) -0.024(7)
_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
S1 O1 1.444(5) . ?
S1 O2 1.445(5) . ?
S1 C1 1.767(3) . ?
S1 C1 1.767(3) 4_575 ?
C1 C2 1.381(5) . ?
C1 C6 1.385(5) . ?
C2 C3 1.390(5) . ?
C3 C4 1.412(5) . ?
C3 C7 1.514(4) . ?
C4 C5 1.402(5) . ?
C4 N1B 1.420(18) . ?
C4 N1 1.430(5) . ?
C5 C6 1.376(5) . ?
C6 C6 1.479(6) 4_575 ?
C7 C8 1.513(6) . ?
C7 C9 1.519(6) . ?
S2 C18 1.757(5) . ?
S2 C12 1.768(5) . ?
N1 C11 1.419(6) . ?
N1 C17 1.431(8) . ?
C10 C16 1.492(10) . ?
C11 C12 1.392(6) . ?
C11 C16 1.410(7) . ?
C12 C13 1.398(7) . ?
C13 C14 1.366(8) . ?
C14 C15 1.379(8) . ?
C15 C16 1.399(7) . ?
C17 C22 1.388(8) . ?
C17 C18 1.389(6) . ?
C18 C19 1.402(7) . ?
C19 C20 1.369(9) . ?
C20 C21 1.377(9) . ?
C21 C22 1.380(11) . ?
S2B C18B 1.739(17) . ?
S2B C12B 1.750(17) . ?
N1B C11B 1.405(18) . ?
N1B C17B 1.432(18) . ?
C10B C16B 1.49(2) . ?
C11B C12B 1.384(18) . ?
C11B C16B 1.409(18) . ?
C12B C13B 1.400(19) . ?
C13B C14B 1.38(2) . ?
C14B C15B 1.38(2) . ?
C15B C16B 1.41(2) . ?
C17B C18B 1.373(18) . ?
C17B C22B 1.39(2) . ?
C18B C19B 1.404(19) . ?
C19B C20B 1.37(2) . ?
C20B C21B 1.37(2) . ?
C21B C22B 1.38(2) . ?
Cl1 C1S 1.723(10) . ?
Cl2 C1S 1.709(9) . ?
Cl3 C1S 1.686(10) . ?
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 S1 O2 116.6(3) . . ?
O1 S1 C1 111.1(2) . . ?
O2 S1 C1 111.29(19) . . ?
O1 S1 C1 111.1(2) . 4_575 ?
O2 S1 C1 111.29(18) . 4_575 ?
C1 S1 C1 93.0(2) . 4_575 ?
C2 C1 C6 122.1(3) . . ?
C2 C1 S1 127.8(3) . . ?
C6 C1 S1 110.1(2) . . ?
C1 C2 C3 119.9(3) . . ?
C2 C3 C4 118.5(3) . . ?
C2 C3 C7 119.3(3) . . ?
C4 C3 C7 122.2(3) . . ?
C5 C4 C3 120.2(3) . . ?
C5 C4 N1B 121.9(17) . . ?
C3 C4 N1B 116.1(17) . . ?
C5 C4 N1 118.3(3) . . ?
C3 C4 N1 121.4(3) . . ?
C6 C5 C4 120.4(3) . . ?
C5 C6 C1 118.7(3) . . ?
C5 C6 C6 128.0(2) . 4_575 ?
C1 C6 C6 113.03(19) . 4_575 ?
C8 C7 C3 110.5(3) . . ?
C8 C7 C9 111.6(4) . . ?
C3 C7 C9 112.0(3) . . ?
C18 S2 C12 99.5(2) . . ?
C11 N1 C4 119.2(5) . . ?
C11 N1 C17 119.0(3) . . ?
C4 N1 C17 119.3(4) . . ?
C12 C11 C16 118.9(4) . . ?
C12 C11 N1 120.9(4) . . ?
C16 C11 N1 120.2(4) . . ?
C11 C12 C13 121.8(5) . . ?
C11 C12 S2 121.2(4) . . ?
C13 C12 S2 116.9(4) . . ?
C14 C13 C12 118.6(5) . . ?
C13 C14 C15 120.9(5) . . ?
C14 C15 C16 121.5(5) . . ?
C15 C16 C11 118.1(4) . . ?
C15 C16 C10 118.9(5) . . ?
C11 C16 C10 123.0(4) . . ?
C22 C17 C18 118.0(6) . . ?
C22 C17 N1 121.1(5) . . ?
C18 C17 N1 120.9(4) . . ?
C17 C18 C19 120.4(5) . . ?
C17 C18 S2 121.4(4) . . ?
C19 C18 S2 118.2(4) . . ?
C20 C19 C18 120.2(5) . . ?
C19 C20 C21 119.9(5) . . ?
C20 C21 C22 120.0(5) . . ?
C21 C22 C17 121.5(6) . . ?
C18B S2B C12B 101.5(12) . . ?
C11B N1B C4 116.0(18) . . ?
C11B N1B C17B 118.1(17) . . ?
C4 N1B C17B 122.8(19) . . ?
C12B C11B N1B 121.9(18) . . ?
C12B C11B C16B 118.7(17) . . ?
N1B C11B C16B 119.5(19) . . ?
C11B C12B C13B 122.2(18) . . ?
C11B C12B S2B 122.6(15) . . ?
C13B C12B S2B 114.4(16) . . ?
C14B C13B C12B 116(2) . . ?
C13B C14B C15B 121(2) . . ?
C14B C15B C16B 121(2) . . ?
C15B C16B C11B 117.6(19) . . ?
C15B C16B C10B 119(3) . . ?
C11B C16B C10B 123(3) . . ?
C18B C17B C22B 118.6(19) . . ?
C18B C17B N1B 124(2) . . ?
C22B C17B N1B 117(2) . . ?
C17B C18B C19B 120.2(18) . . ?
C17B C18B S2B 121.3(15) . . ?
C19B C18B S2B 118.5(17) . . ?
C20B C19B C18B 119(2) . . ?
C19B C20B C21B 122(2) . . ?
C20B C21B C22B 118(2) . . ?
C21B C22B C17B 122(2) . . ?
Cl3 C1S Cl2 109.8(6) . . ?
Cl3 C1S Cl1 115.3(7) . . ?
Cl2 C1S Cl1 111.2(6) . . ?
_refine_diff_density_max 0.699
_refine_diff_density_min -1.059
_refine_diff_density_rms 0.116
_shelx_res_file
;
TITL 16srv102_a.res in P2(1)/m
16srv487.res
created by SHELXL-2018/3 at 21:30:26 on 27-Jul-2018
REM Old TITL 16srv102 in P2(1)/m
REM SHELXT solution in P2(1)/m: R1 0.234, Rweak 0.012, Alpha 0.049
REM 1.019 for 20 systematic absences, Orientation as input
REM Formula found by SHELXT: C20 N4 O2 S2
CELL 0.6889 7.6155 31.3356 8.8919 90 108.991 90
ZERR 2 0.0019 0.0079 0.0023 0 0.005 0
LATT 1
SYMM -X,0.5+Y,-Z
SFAC C H Cl D N O S
DISP C 0.0032 0.0015 10.8482
DISP Cl 0.1418 0.1507 623.9827
DISP D -0 0
DISP H -0 0 0.6228
DISP N 0.006 0.003 18.3366
DISP O 0.0108 0.0057 30.1916
DISP S 0.1181 0.1169 489.4073
UNIT 90 76 6 2 4 4 6
SADI N1 C4 N1B C4
SADI Cl3 C1S Cl1 C1S Cl2 C1S
RIGU
EADP C19B C13B
EADP C18B C12B
EADP C17B C11B
EADP C10B C22
EADP S2B S2
L.S. 7
PLAN 8
SIZE 0.015 0.08 0.115
TEMP -173.15
BOND
list 4
fmap 2 53
acta
OMIT -3 50
OMIT 0 2 0
OMIT -1 3 1
OMIT 0 1 1
OMIT 0 0 1
OMIT 0 2 2
OMIT 1 5 1
OMIT 0 0 2
OMIT -1 0 3
OMIT 2 2 0
OMIT -1 13 1
OMIT 3 0 0
OMIT -3 9 1
OMIT 1 1 1
OMIT -1 12 1
OMIT -2 7 3
OMIT -2 16 2
OMIT -2 12 1
OMIT -2 10 2
OMIT 2 1 0
OMIT -1 6 3
OMIT 0 8 2
OMIT 1 6 0
OMIT -4 3 3
OMIT 3 8 2
REM
REM
REM
WGHT 0.135200 4.603700
FVAR 0.30180 0.89842
S1 7 0.941587 0.750000 0.780729 10.50000 0.01633 0.01436 =
0.05671 0.00000 0.00773 0.00000
O1 6 1.060625 0.750000 0.944556 10.50000 0.03186 0.03101 =
0.07081 0.00000 -0.01431 0.00000
O2 6 1.032589 0.750000 0.661307 10.50000 0.03039 0.02120 =
0.08722 0.00000 0.02926 0.00000
C1 1 0.773268 0.709107 0.745382 11.00000 0.01720 0.01271 =
0.04300 0.00247 0.00705 -0.00043
C2 1 0.798344 0.665899 0.729377 11.00000 0.01942 0.01449 =
0.04619 0.00107 0.01044 0.00317
AFIX 43
H2 2 0.919103 0.654915 0.744269 11.00000 -1.20000
AFIX 0
C3 1 0.646629 0.638523 0.691453 11.00000 0.02109 0.01390 =
0.03774 0.00082 0.01136 0.00168
C4 1 0.471262 0.655529 0.680582 11.00000 0.02169 0.01408 =
0.04091 -0.00100 0.01236 -0.00143
C5 1 0.451267 0.699352 0.702391 11.00000 0.02076 0.01497 =
0.04320 -0.00016 0.01211 0.00259
AFIX 43
H5 2 0.333876 0.710434 0.698854 11.00000 -1.20000
AFIX 0
C6 1 0.600560 0.726402 0.728879 11.00000 0.02147 0.01433 =
0.03912 -0.00007 0.01081 0.00055
C7 1 0.672289 0.592199 0.654796 11.00000 0.02321 0.01332 =
0.05190 -0.00362 0.01572 -0.00035
AFIX 13
H7 2 0.547554 0.578220 0.624135 11.00000 -1.20000
AFIX 0
C8 1 0.741848 0.588816 0.514009 11.00000 0.08911 0.02923 =
0.07674 -0.00921 0.05383 -0.00243
AFIX 7
H8A 2 0.652001 0.602269 0.421097 11.00000 -1.50000
H8B 2 0.756223 0.558654 0.490895 11.00000 -1.50000
H8C 2 0.861979 0.603284 0.538535 11.00000 -1.50000
AFIX 0
C9 1 0.798484 0.568616 0.798804 11.00000 0.07648 0.01918 =
0.06579 0.00469 0.01266 0.01250
AFIX 7
H9A 2 0.923349 0.580992 0.829538 11.00000 -1.50000
H9B 2 0.804585 0.538354 0.772587 11.00000 -1.50000
H9C 2 0.749197 0.571261 0.887438 11.00000 -1.50000
AFIX 0
PART 1
S2 7 0.216930 0.543056 0.472216 21.00000 0.03723 0.01923 =
0.05682 -0.00887 0.01302 -0.00437
N1 5 0.308610 0.629373 0.638401 21.00000 0.01801 0.01545 =
0.04457 0.00289 0.00842 -0.00098
C10 1 0.361125 0.644395 0.976282 21.00000 0.04542 0.03800 =
0.04419 -0.00449 0.01737 -0.00896
AFIX 7
H10A 2 0.490337 0.653294 0.997373 21.00000 -1.50000
H10B 2 0.333719 0.643385 1.076542 21.00000 -1.50000
H10C 2 0.278050 0.664927 0.904191 21.00000 -1.50000
AFIX 0
C11 1 0.300413 0.594560 0.737999 21.00000 0.01848 0.01775 =
0.04809 0.00452 0.01321 0.00063
C12 1 0.255006 0.553755 0.675638 21.00000 0.02635 0.02041 =
0.05073 -0.00177 0.01138 -0.00288
C13 1 0.248167 0.518940 0.771922 21.00000 0.03721 0.02372 =
0.06943 0.00492 0.02593 -0.00435
AFIX 43
H13 2 0.213844 0.491433 0.727068 21.00000 -1.20000
AFIX 0
C14 1 0.291905 0.525337 0.931865 21.00000 0.04749 0.03384 =
0.06968 0.01459 0.02757 0.00205
AFIX 43
H14 2 0.295744 0.501680 0.999678 21.00000 -1.20000
AFIX 0
C15 1 0.330559 0.565650 0.996258 21.00000 0.03810 0.04281 =
0.05071 0.00779 0.01489 -0.00166
AFIX 43
H15 2 0.356997 0.569363 1.107477 21.00000 -1.20000
AFIX 0
C16 1 0.331719 0.601226 0.901442 21.00000 0.02666 0.03128 =
0.04771 0.00057 0.01268 -0.00071
C17 1 0.183326 0.630345 0.478564 21.00000 0.02229 0.02619 =
0.04205 -0.00365 0.00859 -0.00327
C18 1 0.131318 0.592987 0.391244 21.00000 0.02665 0.02488 =
0.04976 -0.00675 0.01067 -0.00370
C19 1 0.009321 0.594396 0.234494 21.00000 0.04608 0.04434 =
0.04280 -0.01090 0.00711 -0.00696
AFIX 43
H19 2 -0.029341 0.568639 0.176865 21.00000 -1.20000
AFIX 0
C20 1 -0.054295 0.632771 0.164179 21.00000 0.05953 0.05742 =
0.04240 0.00023 -0.00290 -0.00021
AFIX 43
H20 2 -0.133187 0.633707 0.056624 21.00000 -1.20000
AFIX 0
C21 1 -0.003775 0.670003 0.249560 21.00000 0.06669 0.04307 =
0.05880 0.00659 -0.00383 0.01228
AFIX 43
H21 2 -0.048736 0.696635 0.201252 21.00000 -1.20000
AFIX 0
C22 1 0.112165 0.668623 0.405295 21.00000 0.04616 0.02999 =
0.05542 -0.00400 -0.00334 0.00918
AFIX 43
H22 2 0.144036 0.694462 0.463739 21.00000 -1.20000
AFIX 0
SAME 0.02 0.04 S2 > C22
PART 0
PART 2
S2B 7 0.305122 0.527503 0.697209 -21.00000 0.03723 0.01923 =
0.05682 -0.00887 0.01302 -0.00437
N1B 5 0.333705 0.625553 0.686324 -21.00000 0.02640
C10B 1 0.117822 0.676216 0.411571 -21.00000 0.04616 0.02999 =
0.05542 -0.00400 -0.00334 0.00918
AFIX 33
H10D 2 0.178624 0.686776 0.519827 -21.00000 -1.50000
H10E 2 0.166800 0.691475 0.337574 -21.00000 -1.50000
H10F 2 -0.016356 0.681005 0.381550 -21.00000 -1.50000
AFIX 0
C11B 1 0.238463 0.604997 0.542430 -21.00000 0.01722
C12B 1 0.220971 0.561029 0.531850 -21.00000 0.03164
C13B 1 0.110094 0.540547 0.393660 -21.00000 0.04204
AFIX 43
H13B 2 0.065815 0.512257 0.395077 -21.00000 -1.20000
AFIX 0
C14B 1 0.069289 0.563968 0.255664 -21.00000 0.05653
AFIX 43
H14B 2 0.033099 0.549681 0.156021 -21.00000 -1.20000
AFIX 0
C15B 1 0.080197 0.607873 0.260009 -21.00000 0.04604
AFIX 43
H15B 2 0.036631 0.623638 0.163703 -21.00000 -1.20000
AFIX 0
C16B 1 0.154962 0.629625 0.405122 -21.00000 0.04317
C17B 1 0.330648 0.606167 0.831309 -21.00000 0.01722
C18B 1 0.325981 0.562848 0.852787 -21.00000 0.03164
C19B 1 0.333281 0.546226 1.001360 -21.00000 0.04204
AFIX 43
H19B 2 0.319072 0.516476 1.014453 -21.00000 -1.20000
AFIX 0
C20B 1 0.361173 0.573552 1.126897 -21.00000 0.06651
AFIX 43
H20B 2 0.369730 0.562257 1.228186 -21.00000 -1.20000
AFIX 0
C21B 1 0.377161 0.616784 1.110932 -21.00000 0.04866
AFIX 43
H21B 2 0.403953 0.635185 1.200489 -21.00000 -1.20000
AFIX 0
C22B 1 0.353225 0.632728 0.961222 -21.00000 0.04877
AFIX 43
H22B 2 0.352132 0.662764 0.946432 -21.00000 -1.20000
AFIX 0
PART 0
CL1 3 0.574182 0.750000 0.077760 10.50000 0.13233 0.06138 =
0.06187 0.00000 0.04397 0.00000
PART -1
CL2 3 0.585635 0.801740 0.341998 10.50000 0.07789 0.06310 =
0.03974 -0.00736 0.01706 -0.00290
CL3 3 0.425290 0.721367 0.319460 10.50000 0.35779 0.13010 =
0.07741 -0.03631 0.09739 -0.14773
C1S 1 0.466423 0.762844 0.214766 10.50000 0.08419 0.09408 =
0.05512 -0.01963 0.01336 -0.02432
AFIX 3
D1S 4 0.342603 0.775144 0.153516 10.50000 -1.20000
AFIX 0
HKLF 4
REM 16srv102_a.res in P2(1)/m
REM wR2 = 0.2703, GooF = S = 1.059, Restrained GooF = 1.025 for all data
REM R1 = 0.0994 for 3441 Fo > 4sig(Fo) and 0.1060 for all 3922 data
REM 327 parameters refined using 271 restraints
END
WGHT 0.1366 4.5818
REM Highest difference peak 0.699, deepest hole -1.059, 1-sigma level 0.116
Q1 1 0.2219 0.5403 0.5624 11.00000 0.05 0.70
Q2 1 0.9548 0.7500 0.6978 10.50000 0.05 0.57
Q3 1 0.7141 0.7500 0.1179 10.50000 0.05 0.54
Q4 1 0.8478 0.7194 0.7602 11.00000 0.05 0.52
Q5 1 0.8851 0.7500 0.7556 10.50000 0.05 0.50
Q6 1 0.6996 0.7190 0.7252 11.00000 0.05 0.50
Q7 1 0.1611 0.5588 0.4329 11.00000 0.05 0.48
Q8 1 0.3095 0.5364 0.7193 11.00000 0.05 0.48
;
_shelx_res_checksum 84480
#===END
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone/d-chloroform'
_exptl_crystal_preparation Luminescent
#######################################################################
#
# 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_8-16s102
_database_code_depnum_ccdc_archive 'CCDC 1884008'
loop_
_audit_author_name
_audit_author_address
'Andrei S. Batsanov'
;Durham University
United Kingdom
;
_audit_update_record
;
2018-12-10 deposited with the CCDC. 2019-05-29 downloaded from the CCDC.
;
_audit_creation_date 2018-07-26
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C44 H38 N2 O2 S3'
_chemical_formula_sum 'C44 H38 N2 O2 S3'
_chemical_formula_weight 722.94
_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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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 'C 1 2/c 1'
_space_group_name_Hall '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 16.766(4)
_cell_length_b 7.6903(19)
_cell_length_c 28.118(7)
_cell_angle_alpha 90
_cell_angle_beta 90.899(4)
_cell_angle_gamma 90
_cell_volume 3625.0(16)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 665
_cell_measurement_temperature 120
_cell_measurement_theta_max 40.39
_cell_measurement_theta_min 3.14
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.190
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.8317
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
; SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
wR2(int) was 0.0950 before and 0.0707 after correction. The Ratio
of minimum to maximum transmission is 0.8317. The \l/2 correction
factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.325
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description lathe
_exptl_crystal_F_000 1520
_exptl_crystal_size_max 0.316
_exptl_crystal_size_mid 0.125
_exptl_crystal_size_min 0.042
_exptl_special_details
; Data were collected in shutterless mode. Full sphere of reciprocal
space was nominally covered by 12 runs of narrow-frame \w-scans
(8 x 340 + 180 + 60 + 2 x 40 scans, scan width 0.5\%, exposure 10s for
low 2\q, 20s for medium and 30s for high 2\q), every run at a different
2\q and/or \f angle.
Two runs of 358 \f-scans (scan width 1\%, 1.5s exposure) were used for
scaling overflowing intensities. Crystal to detector distance 3.49 cm.
The crystal was a 2-component pseudo-orthorhombic twin with partial
overlap of 3305 out of 3518 reflections: R(sym)=0.043 for orthorhombic
vs 0.031 for monoclinic setting. Twin law:
-1 0 0
0 -1 0
0 0 1,
i.e. a 180 \% rotation around the direct (or reciprocal) axis [0 0 1].
The accurate unit cell parameters were measured on a different crystal
which was not twinned (but too small for full data collection), a
colourless prism of 0.014 x 0.016 x 0.26 mm. Global refinement of the
lattice for the twinned crystal on 9757 reflections with 3.15<\q<75.32\%,
converged at a=16.7106(9), b=7.6972(3), c=28.0540(13) \%A, \a=90,
\b=90.056(3), \g=90 \%, V=3608.4(3) \%A^3^.
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0602
_diffrn_reflns_av_unetI/netI 0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 35
_diffrn_reflns_limit_l_min -32
_diffrn_reflns_number 18203
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 75.549
_diffrn_reflns_theta_min 3.144
_diffrn_ambient_temperature 120
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type 'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device '3-circle area detector 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 CuK\a
_diffrn_radiation_wavelength 1.54184
_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 3035
_reflns_number_total 3518
_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. Completness statistics refer to single and
composite reflections containing twin component 1 only.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.38A (Bruker, 2016)'
_computing_data_collection 'APEX3 v.2016.1-0 (Bruker, 2016)'
_computing_data_reduction 'SAINT v8.38A (Bruker, 2016)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement
'ShelXL 2018/3 multi-CPU version (Sheldrick, 2015a)'
_computing_structure_solution 'ShelXT 2018/2 (Sheldrick, 2015)'
_refine_diff_density_max 0.311
_refine_diff_density_min -0.331
_refine_diff_density_rms 0.052
_refine_ls_extinction_coef 0.00027(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_ls_goodness_of_fit_ref 1.062
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 291
_refine_ls_number_reflns 3518
_refine_ls_number_restraints 253
_refine_ls_R_factor_all 0.0625
_refine_ls_R_factor_gt 0.0493
_refine_ls_restrained_S_all 1.032
_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^)+(0.0189P)^2^+7.2320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0988
_refine_ls_wR_factor_ref 0.1068
_refine_special_details
;Refined as a 2-component twin.
The methyl-phenothiazine moiety is disordered between two
orientations with methyl group on different sides of the dibenzothiophene
plane, refined with geometries restrained to similarity (SAME). Their
occupancies refined to 0.857(3) and 0.143(3). The minor orientation is
labelled B.,Twin
;
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.4969(14) ref 1 0 0 0 1 0 0 0 1
2 0.5031(14) mt_II -1 0 0 0 -1 0 0 0 1
_olex2_refinement_description
;
1. Twinned data refinement
Scales: 0.4969(14)
0.5031(14)
2. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
3. Shared sites
{N1, N1B}
4. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(N1B)
Uiso(C17B) = Uiso(C11B)
Uiso(C18B) = Uiso(C12B)
5. 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
6. Same fragment restrains
{S2, N1, C10, C11, C12, C13, C14, C15, C16, C17, C18, C19, C20, C21, C22} sigma
for 1-2: 0.02, 1-3: 0.04
as
{S2B, N1B, C10B, C11B, C12B, C13B, C14B, C15B, C16B, C17B, C18B, C19B, C20B,
C21B, C22B}
7. Others
Sof(S2B)=Sof(N1B)=Sof(C10B)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C11B)=Sof(C12B)=
Sof(C13B)=Sof(H13B)=Sof(C14B)=Sof(H14B)=Sof(C15B)=Sof(H15B)=Sof(C16B)=
Sof(C17B)=Sof(C18B)=Sof(C19B)=Sof(H19B)=Sof(C20B)=Sof(H20B)=Sof(C21B)=
Sof(H21B)=Sof(C22B)=Sof(H22B)=1-FVAR(1)
Sof(S2)=Sof(N1)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11)=Sof(C12)=
Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(C17)=
Sof(C18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=Sof(C22)=
Sof(H22)=FVAR(1)
8.a Rotating group:
C10(H10A,H10B,H10C)
8.b Ternary CH refined with riding coordinates:
C7(H7)
8.c Me refined with riding coordinates:
C10B(H10D,H10E,H10F)
8.d Aromatic/amide H refined with riding coordinates:
C2(H2), C5(H5), C13(H13), C14(H14), C15(H15), C19(H19), C20(H20), C21(H21),
C22(H22), C13B(H13B), C14B(H14B), C15B(H15B), C19B(H19B), C20B(H20B),
C21B(H21B), C22B(H22B)
8.e Idealised Me refined as rotating group:
C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_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
S1 S 0.500000 0.41600(12) 0.250000 0.0456(4) Uani 1 2 d S TU P . .
O1 O 0.55989(18) 0.3168(3) 0.22567(9) 0.0611(9) Uani 1 1 d . U . . .
C1 C 0.4552(2) 0.5758(4) 0.21296(11) 0.0362(9) Uani 1 1 d . U . . .
C2 C 0.4055(2) 0.5470(4) 0.17443(12) 0.0400(10) Uani 1 1 d . U . . .
H2 H 0.391856 0.431463 0.165557 0.048 Uiso 1 1 calc R . . . .
C3 C 0.3752(2) 0.6863(4) 0.14839(12) 0.0378(9) Uani 1 1 d . U . . .
C4 C 0.3966(2) 0.8560(4) 0.16258(11) 0.0348(9) Uani 1 1 d . U . . .
C5 C 0.4441(2) 0.8832(4) 0.20323(11) 0.0368(10) Uani 1 1 d . U . . .
H5 H 0.455518 0.998220 0.213633 0.044 Uiso 1 1 calc R . . . .
C6 C 0.4747(2) 0.7423(4) 0.22832(10) 0.0351(9) Uani 1 1 d . U . . .
C7 C 0.3221(3) 0.6479(4) 0.10573(13) 0.0518(11) Uani 1 1 d . U . . .
H7 H 0.302879 0.761111 0.092327 0.062 Uiso 1 1 calc R . . . .
C8 C 0.3691(3) 0.5563(6) 0.06807(14) 0.0803(16) Uani 1 1 d . U . . .
H8A H 0.387181 0.443259 0.080188 0.121 Uiso 1 1 calc GR . . . .
H8B H 0.415379 0.627055 0.059722 0.121 Uiso 1 1 calc GR . . . .
H8C H 0.335174 0.538742 0.039753 0.121 Uiso 1 1 calc GR . . . .
C9 C 0.2496(3) 0.5423(6) 0.1204(2) 0.0818(17) Uani 1 1 d . U . . .
H9A H 0.267262 0.431625 0.134233 0.123 Uiso 1 1 calc GR . . . .
H9B H 0.215684 0.519649 0.092349 0.123 Uiso 1 1 calc GR . . . .
H9C H 0.219292 0.607693 0.143908 0.123 Uiso 1 1 calc GR . . . .
S2 S 0.31915(8) 1.03480(12) 0.03230(4) 0.0493(4) Uani 0.857(3) 1 d D U . A 1
N1 N 0.37052(17) 1.0048(3) 0.13532(9) 0.0341(7) Uani 0.857(3) 1 d D U . A 1
C10 C 0.2681(3) 1.0630(7) 0.21794(19) 0.0501(12) Uani 0.857(3) 1 d D U . A 1
H10A H 0.278353 0.941377 0.226481 0.075 Uiso 0.857(3) 1 d GR . . A 1
H10B H 0.227005 1.110635 0.238639 0.075 Uiso 0.857(3) 1 d GR . . A 1
H10C H 0.317366 1.130464 0.221938 0.075 Uiso 0.857(3) 1 d GR . . A 1
C11 C 0.2887(3) 1.0459(4) 0.12843(16) 0.0362(10) Uani 0.857(3) 1 d D U . A 1
C12 C 0.2594(3) 1.0730(5) 0.08257(16) 0.0454(12) Uani 0.857(3) 1 d D U . A 1
C13 C 0.1811(3) 1.1171(5) 0.07433(18) 0.0512(13) Uani 0.857(3) 1 d D U . A 1
H13 H 0.161771 1.131631 0.042636 0.061 Uiso 0.857(3) 1 calc R . . A 1
C14 C 0.1313(3) 1.1400(6) 0.1112(2) 0.0624(14) Uani 0.857(3) 1 d D U . A 1
H14 H 0.077170 1.171308 0.105468 0.075 Uiso 0.857(3) 1 calc R . . A 1
C15 C 0.1598(3) 1.1172(7) 0.1581(3) 0.0605(15) Uani 0.857(3) 1 d D U . A 1
H15 H 0.124320 1.130975 0.183853 0.073 Uiso 0.857(3) 1 calc R . . A 1
C16 C 0.2405(3) 1.0740(5) 0.16741(17) 0.0425(10) Uani 0.857(3) 1 d D U . A 1
C17 C 0.4286(3) 1.0822(4) 0.10450(14) 0.0343(10) Uani 0.857(3) 1 d D U . A 1
C18 C 0.4122(3) 1.1050(5) 0.05607(15) 0.0430(11) Uani 0.857(3) 1 d D U . A 1
C19 C 0.4669(4) 1.1836(7) 0.02675(19) 0.0588(14) Uani 0.857(3) 1 d D U . A 1
H19 H 0.454148 1.199662 -0.005997 0.071 Uiso 0.857(3) 1 calc R . . A 1
C20 C 0.5397(3) 1.2390(7) 0.04452(18) 0.0600(13) Uani 0.857(3) 1 d D U . A 1
H20 H 0.577721 1.289985 0.024093 0.072 Uiso 0.857(3) 1 calc R . . A 1
C21 C 0.5564(3) 1.2192(5) 0.09232(17) 0.0520(12) Uani 0.857(3) 1 d D U . A 1
H21 H 0.606042 1.258678 0.104964 0.062 Uiso 0.857(3) 1 calc R . . A 1
C22 C 0.5017(3) 1.1423(5) 0.12224(15) 0.0379(10) Uani 0.857(3) 1 d D U . A 1
H22 H 0.514145 1.130466 0.155154 0.046 Uiso 0.857(3) 1 calc R . . A 1
S2B S 0.2364(6) 1.0442(12) 0.0624(3) 0.059(3) Uiso 0.143(3) 1 d D U . A 2
N1B N 0.37052(17) 1.0048(3) 0.13532(9) 0.0341(7) Uani 0.143(3) 1 d D U . A 2
C10B C 0.5372(18) 1.103(5) 0.1187(11) 0.063(11) Uiso 0.143(3) 1 d D U . A 2
H10D H 0.588883 1.112422 0.103070 0.095 Uiso 0.143(3) 1 calc R . . A 2
H10E H 0.526771 1.209949 0.136497 0.095 Uiso 0.143(3) 1 calc R . . A 2
H10F H 0.538118 1.003834 0.140559 0.095 Uiso 0.143(3) 1 calc R . . A 2
C11B C 0.3929(11) 1.058(4) 0.0902(6) 0.053(6) Uiso 0.143(3) 1 d D U . A 2
C12B C 0.3381(10) 1.076(4) 0.0536(7) 0.055(6) Uiso 0.143(3) 1 d D U . A 2
C13B C 0.3591(15) 1.119(4) 0.0080(8) 0.070(9) Uiso 0.143(3) 1 d D U . A 2
H13B H 0.319278 1.131553 -0.016134 0.083 Uiso 0.143(3) 1 calc R . . A 2
C14B C 0.4365(15) 1.142(5) -0.0020(9) 0.075(10) Uiso 0.143(3) 1 d D U . A 2
H14B H 0.453123 1.166429 -0.033419 0.090 Uiso 0.143(3) 1 calc R . . A 2
C15B C 0.4914(17) 1.129(5) 0.0356(9) 0.069(12) Uiso 0.143(3) 1 d D U . A 2
H15B H 0.545395 1.156403 0.029214 0.083 Uiso 0.143(3) 1 calc R . . A 2
C16B C 0.4735(12) 1.077(5) 0.0823(8) 0.071(11) Uiso 0.143(3) 1 d D U . A 2
C17B C 0.2950(11) 1.072(4) 0.1535(7) 0.053(6) Uiso 0.143(3) 1 d D U . A 2
C18B C 0.2305(13) 1.101(4) 0.1234(6) 0.055(6) Uiso 0.143(3) 1 d D U . A 2
C19B C 0.1585(17) 1.164(5) 0.1401(10) 0.068(14) Uiso 0.143(3) 1 d D U . A 2
H19B H 0.113216 1.170469 0.119399 0.082 Uiso 0.143(3) 1 calc R . . A 2
C20B C 0.153(2) 1.218(6) 0.1866(11) 0.115(16) Uiso 0.143(3) 1 d D U . A 2
H20B H 0.105780 1.273585 0.197299 0.139 Uiso 0.143(3) 1 calc R . . A 2
C21B C 0.217(2) 1.190(7) 0.2178(12) 0.15(2) Uiso 0.143(3) 1 d D U . A 2
H21B H 0.212170 1.219464 0.250406 0.181 Uiso 0.143(3) 1 calc R . . A 2
C22B C 0.287(2) 1.118(6) 0.2014(9) 0.089(17) Uiso 0.143(3) 1 d D U . A 2
H22B H 0.330341 1.099876 0.223016 0.106 Uiso 0.143(3) 1 calc R . . A 2
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
S1 0.0769(11) 0.0151(4) 0.0434(7) 0.000 -0.0411(8) 0.000
O1 0.096(2) 0.0279(11) 0.0577(16) -0.0146(11) -0.0452(17) 0.0268(14)
C1 0.054(2) 0.0207(13) 0.0326(16) 0.0006(12) -0.0231(17) 0.0002(14)
C2 0.062(3) 0.0133(12) 0.0434(18) -0.0023(13) -0.0255(18) 0.0005(14)
C3 0.055(2) 0.0195(13) 0.0385(18) -0.0024(13) -0.0244(18) 0.0043(14)
C4 0.053(2) 0.0181(13) 0.0333(17) 0.0026(12) -0.0201(17) 0.0033(13)
C5 0.059(3) 0.0151(12) 0.0353(18) -0.0016(12) -0.0225(18) 0.0001(14)
C6 0.050(2) 0.0210(13) 0.0333(17) -0.0012(12) -0.0234(16) 0.0006(13)
C7 0.084(3) 0.0194(14) 0.051(2) -0.0031(14) -0.045(2) 0.0078(16)
C8 0.119(4) 0.077(3) 0.044(2) -0.014(2) -0.044(3) 0.012(3)
C9 0.076(3) 0.064(3) 0.104(4) 0.000(3) -0.060(3) -0.007(2)
S2 0.0777(9) 0.0327(5) 0.0365(6) -0.0019(4) -0.0332(7) 0.0029(5)
N1 0.0472(17) 0.0185(11) 0.0361(14) 0.0026(10) -0.0198(13) 0.0030(11)
C10 0.052(3) 0.047(3) 0.052(3) -0.004(2) 0.005(3) 0.009(2)
C11 0.047(2) 0.0129(14) 0.048(2) 0.0044(16) -0.0221(19) -0.0007(15)
C12 0.072(3) 0.0176(17) 0.045(2) -0.0047(17) -0.031(2) 0.0047(18)
C13 0.055(3) 0.039(2) 0.059(3) 0.000(2) -0.028(2) -0.007(2)
C14 0.040(3) 0.053(3) 0.094(4) 0.013(3) -0.024(3) 0.003(2)
C15 0.054(3) 0.042(3) 0.085(4) 0.004(3) -0.007(3) -0.001(2)
C16 0.046(3) 0.0253(18) 0.055(2) 0.0019(18) -0.010(2) 0.0013(18)
C17 0.047(3) 0.0159(15) 0.039(2) 0.0009(15) -0.019(2) 0.0070(16)
C18 0.065(3) 0.0256(18) 0.038(2) -0.0034(16) -0.013(2) 0.0085(18)
C19 0.076(4) 0.056(3) 0.044(3) 0.003(2) -0.006(3) 0.009(3)
C20 0.064(4) 0.058(3) 0.058(3) 0.010(2) 0.009(3) -0.001(3)
C21 0.055(3) 0.039(2) 0.062(3) 0.005(2) -0.003(2) 0.000(2)
C22 0.045(3) 0.0283(17) 0.040(2) -0.0026(15) -0.012(2) 0.006(2)
N1B 0.0472(17) 0.0185(11) 0.0361(14) 0.0026(10) -0.0198(13) 0.0030(11)
_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
S1 O1 1.442(3) . ?
S1 O1 1.442(3) 2_655 ?
S1 C1 1.771(3) . ?
S1 C1 1.771(3) 2_655 ?
C1 C2 1.374(4) . ?
C1 C6 1.389(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.389(4) . ?
C3 C4 1.409(4) . ?
C3 C7 1.512(4) . ?
C4 C5 1.399(4) . ?
C4 N1 1.441(3) . ?
C4 N1B 1.441(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.387(4) . ?
C6 C6 1.475(5) 2_655 ?
C7 H7 1.0000 . ?
C7 C8 1.505(7) . ?
C7 C9 1.524(7) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
S2 C12 1.769(5) . ?
S2 C18 1.772(5) . ?
N1 C11 1.418(5) . ?
N1 C17 1.442(6) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9805 . ?
C10 C16 1.490(6) . ?
C11 C12 1.388(6) . ?
C11 C16 1.389(7) . ?
C12 C13 1.373(7) . ?
C13 H13 0.9500 . ?
C13 C14 1.354(8) . ?
C14 H14 0.9500 . ?
C14 C15 1.406(8) . ?
C15 H15 0.9500 . ?
C15 C16 1.414(7) . ?
C17 C18 1.396(5) . ?
C17 C22 1.395(6) . ?
C18 C19 1.382(7) . ?
C19 H19 0.9500 . ?
C19 C20 1.379(7) . ?
C20 H20 0.9500 . ?
C20 C21 1.377(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.386(7) . ?
C22 H22 0.9500 . ?
S2B C12B 1.745(16) . ?
S2B C18B 1.773(16) . ?
N1B C11B 1.391(16) . ?
N1B C17B 1.467(16) . ?
C10B H10D 0.9800 . ?
C10B H10E 0.9800 . ?
C10B H10F 0.9800 . ?
C10B C16B 1.482(18) . ?
C11B C12B 1.377(17) . ?
C11B C16B 1.380(18) . ?
C12B C13B 1.372(18) . ?
C13B H13B 0.9500 . ?
C13B C14B 1.345(19) . ?
C14B H14B 0.9500 . ?
C14B C15B 1.395(19) . ?
C15B H15B 0.9500 . ?
C15B C16B 1.406(19) . ?
C17B C18B 1.381(17) . ?
C17B C22B 1.403(18) . ?
C18B C19B 1.391(19) . ?
C19B H19B 0.9500 . ?
C19B C20B 1.38(2) . ?
C20B H20B 0.9500 . ?
C20B C21B 1.39(2) . ?
C21B H21B 0.9500 . ?
C21B C22B 1.38(2) . ?
C22B H22B 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
O1 S1 O1 116.1(2) . 2_655 ?
O1 S1 C1 112.36(16) . . ?
O1 S1 C1 110.72(16) . 2_655 ?
O1 S1 C1 110.72(16) 2_655 . ?
O1 S1 C1 112.36(16) 2_655 2_655 ?
C1 S1 C1 92.12(18) 2_655 . ?
C2 C1 S1 126.8(2) . . ?
C2 C1 C6 122.0(3) . . ?
C6 C1 S1 111.18(19) . . ?
C1 C2 H2 119.9 . . ?
C1 C2 C3 120.2(3) . . ?
C3 C2 H2 119.9 . . ?
C2 C3 C4 118.4(3) . . ?
C2 C3 C7 118.3(2) . . ?
C4 C3 C7 123.3(2) . . ?
C3 C4 N1 120.8(2) . . ?
C3 C4 N1B 120.8(2) . . ?
C5 C4 C3 120.6(3) . . ?
C5 C4 N1 118.7(2) . . ?
C5 C4 N1B 118.7(2) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 120.0(3) . . ?
C6 C5 H5 120.0 . . ?
C1 C6 C6 112.75(15) . 2_655 ?
C5 C6 C1 118.6(2) . . ?
C5 C6 C6 128.60(16) . 2_655 ?
C3 C7 H7 108.2 . . ?
C3 C7 C9 110.6(3) . . ?
C8 C7 C3 110.0(3) . . ?
C8 C7 H7 108.2 . . ?
C8 C7 C9 111.6(3) . . ?
C9 C7 H7 108.2 . . ?
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 . . ?
C12 S2 C18 98.9(2) . . ?
C4 N1 C17 116.5(3) . . ?
C11 N1 C4 122.3(3) . . ?
C11 N1 C17 119.1(3) . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.4 . . ?
H10B C10 H10C 109.4 . . ?
C16 C10 H10A 109.8 . . ?
C16 C10 H10B 109.5 . . ?
C16 C10 H10C 109.1 . . ?
C12 C11 N1 119.2(4) . . ?
C12 C11 C16 120.5(4) . . ?
C16 C11 N1 120.0(3) . . ?
C11 C12 S2 121.4(4) . . ?
C13 C12 S2 117.3(4) . . ?
C13 C12 C11 121.1(5) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 C12 120.2(4) . . ?
C14 C13 H13 119.9 . . ?
C13 C14 H14 120.1 . . ?
C13 C14 C15 119.8(5) . . ?
C15 C14 H14 120.1 . . ?
C14 C15 H15 119.6 . . ?
C14 C15 C16 120.9(6) . . ?
C16 C15 H15 119.6 . . ?
C11 C16 C10 124.6(4) . . ?
C11 C16 C15 117.2(4) . . ?
C15 C16 C10 118.2(5) . . ?
C18 C17 N1 120.9(4) . . ?
C22 C17 N1 121.3(3) . . ?
C22 C17 C18 117.7(4) . . ?
C17 C18 S2 119.2(4) . . ?
C19 C18 S2 119.8(3) . . ?
C19 C18 C17 121.0(5) . . ?
C18 C19 H19 119.7 . . ?
C20 C19 C18 120.7(5) . . ?
C20 C19 H19 119.7 . . ?
C19 C20 H20 120.5 . . ?
C21 C20 C19 119.0(5) . . ?
C21 C20 H20 120.5 . . ?
C20 C21 H21 119.6 . . ?
C20 C21 C22 120.9(5) . . ?
C22 C21 H21 119.6 . . ?
C17 C22 H22 119.7 . . ?
C21 C22 C17 120.7(4) . . ?
C21 C22 H22 119.7 . . ?
C12B S2B C18B 99.9(10) . . ?
C4 N1B C17B 110.5(11) . . ?
C11B N1B C4 129.5(12) . . ?
C11B N1B C17B 117.4(13) . . ?
H10D C10B H10E 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?
C16B C10B H10D 109.5 . . ?
C16B C10B H10E 109.5 . . ?
C16B C10B H10F 109.5 . . ?
C12B C11B N1B 121.7(15) . . ?
C12B C11B C16B 120.8(15) . . ?
C16B C11B N1B 117.2(16) . . ?
C11B C12B S2B 121.5(14) . . ?
C13B C12B S2B 115.6(15) . . ?
C13B C12B C11B 123.0(16) . . ?
C12B C13B H13B 120.3 . . ?
C14B C13B C12B 119.3(19) . . ?
C14B C13B H13B 120.3 . . ?
C13B C14B H14B 121.3 . . ?
C13B C14B C15B 117(2) . . ?
C15B C14B H14B 121.3 . . ?
C14B C15B H15B 117.3 . . ?
C14B C15B C16B 125(2) . . ?
C16B C15B H15B 117.3 . . ?
C11B C16B C10B 127(2) . . ?
C11B C16B C15B 113.9(18) . . ?
C15B C16B C10B 116(2) . . ?
C18B C17B N1B 121.0(16) . . ?
C18B C17B C22B 117.6(17) . . ?
C22B C17B N1B 121.3(18) . . ?
C17B C18B S2B 119.9(15) . . ?
C17B C18B C19B 121.6(17) . . ?
C19B C18B S2B 118.3(16) . . ?
C18B C19B H19B 120.0 . . ?
C20B C19B C18B 120(2) . . ?
C20B C19B H19B 120.0 . . ?
C19B C20B H20B 120.4 . . ?
C19B C20B C21B 119(2) . . ?
C21B C20B H20B 120.4 . . ?
C20B C21B H21B 119.9 . . ?
C22B C21B C20B 120(2) . . ?
C22B C21B H21B 119.9 . . ?
C17B C22B H22B 119.5 . . ?
C21B C22B C17B 121(2) . . ?
C21B C22B H22B 119.5 . . ?
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
S1 C1 C2 C3 -179.5(3) . . . . ?
S1 C1 C6 C5 -179.8(3) . . . . ?
S1 C1 C6 C6 -1.5(5) . . . 2_655 ?
O1 S1 C1 C2 68.7(4) . . . . ?
O1 S1 C1 C2 -63.0(4) 2_655 . . . ?
O1 S1 C1 C6 -112.9(3) . . . . ?
O1 S1 C1 C6 115.5(3) 2_655 . . . ?
C1 S1 C1 C2 -177.9(5) 2_655 . . . ?
C1 S1 C1 C6 0.56(19) 2_655 . . . ?
C1 C2 C3 C4 -0.2(6) . . . . ?
C1 C2 C3 C7 178.9(4) . . . . ?
C2 C1 C6 C5 -1.3(6) . . . . ?
C2 C1 C6 C6 177.0(4) . . . 2_655 ?
C2 C3 C4 C5 -2.9(6) . . . . ?
C2 C3 C4 N1 176.5(4) . . . . ?
C2 C3 C4 N1B 176.5(4) . . . . ?
C2 C3 C7 C8 -65.5(5) . . . . ?
C2 C3 C7 C9 58.3(5) . . . . ?
C3 C4 C5 C6 3.8(6) . . . . ?
C3 C4 N1 C11 61.6(5) . . . . ?
C3 C4 N1 C17 -101.6(4) . . . . ?
C3 C4 N1B C11B -68.9(13) . . . . ?
C3 C4 N1B C17B 92.1(11) . . . . ?
C4 C3 C7 C8 113.4(4) . . . . ?
C4 C3 C7 C9 -122.8(4) . . . . ?
C4 C5 C6 C1 -1.7(6) . . . . ?
C4 C5 C6 C6 -179.8(5) . . . 2_655 ?
C4 N1 C11 C12 -127.8(4) . . . . ?
C4 N1 C11 C16 58.0(4) . . . . ?
C4 N1 C17 C18 125.2(3) . . . . ?
C4 N1 C17 C22 -57.1(4) . . . . ?
C4 N1B C11B C12B 121(2) . . . . ?
C4 N1B C11B C16B -53(3) . . . . ?
C4 N1B C17B C18B -129(2) . . . . ?
C4 N1B C17B C22B 55(3) . . . . ?
C5 C4 N1 C11 -119.0(4) . . . . ?
C5 C4 N1 C17 77.8(4) . . . . ?
C5 C4 N1B C11B 110.5(13) . . . . ?
C5 C4 N1B C17B -88.6(11) . . . . ?
C6 C1 C2 C3 2.3(6) . . . . ?
C7 C3 C4 C5 178.2(4) . . . . ?
C7 C3 C4 N1 -2.5(6) . . . . ?
C7 C3 C4 N1B -2.5(6) . . . . ?
S2 C12 C13 C14 176.8(4) . . . . ?
S2 C18 C19 C20 -179.9(4) . . . . ?
N1 C4 C5 C6 -175.5(4) . . . . ?
N1 C11 C12 S2 6.9(5) . . . . ?
N1 C11 C12 C13 -178.4(3) . . . . ?
N1 C11 C16 C10 -0.5(6) . . . . ?
N1 C11 C16 C15 179.0(3) . . . . ?
N1 C17 C18 S2 -0.9(5) . . . . ?
N1 C17 C18 C19 178.1(4) . . . . ?
N1 C17 C22 C21 -178.9(4) . . . . ?
C11 N1 C17 C18 -38.5(5) . . . . ?
C11 N1 C17 C22 139.2(4) . . . . ?
C11 C12 C13 C14 1.9(6) . . . . ?
C12 S2 C18 C17 32.4(3) . . . . ?
C12 S2 C18 C19 -146.7(4) . . . . ?
C12 C11 C16 C10 -174.6(4) . . . . ?
C12 C11 C16 C15 4.9(6) . . . . ?
C12 C13 C14 C15 -0.5(7) . . . . ?
C13 C14 C15 C16 1.3(8) . . . . ?
C14 C15 C16 C10 176.1(4) . . . . ?
C14 C15 C16 C11 -3.5(7) . . . . ?
C16 C11 C12 S2 -179.0(3) . . . . ?
C16 C11 C12 C13 -4.3(6) . . . . ?
C17 N1 C11 C12 34.9(4) . . . . ?
C17 N1 C11 C16 -139.3(3) . . . . ?
C17 C18 C19 C20 1.1(7) . . . . ?
C18 S2 C12 C11 -36.2(3) . . . . ?
C18 S2 C12 C13 149.0(3) . . . . ?
C18 C17 C22 C21 -1.1(6) . . . . ?
C18 C19 C20 C21 -1.8(8) . . . . ?
C19 C20 C21 C22 1.0(8) . . . . ?
C20 C21 C22 C17 0.4(7) . . . . ?
C22 C17 C18 S2 -178.6(3) . . . . ?
C22 C17 C18 C19 0.4(6) . . . . ?
S2B C12B C13B C14B -179(3) . . . . ?
S2B C18B C19B C20B -177(4) . . . . ?
N1B C4 C5 C6 -175.5(4) . . . . ?
N1B C11B C12B S2B 4(4) . . . . ?
N1B C11B C12B C13B -176(3) . . . . ?
N1B C11B C16B C10B -21(5) . . . . ?
N1B C11B C16B C15B 179(3) . . . . ?
N1B C17B C18B S2B 4(4) . . . . ?
N1B C17B C18B C19B 180(3) . . . . ?
N1B C17B C22B C21B 177(4) . . . . ?
C11B N1B C17B C18B 35(3) . . . . ?
C11B N1B C17B C22B -142(3) . . . . ?
C11B C12B C13B C14B 1(5) . . . . ?
C12B S2B C18B C17B -31(3) . . . . ?
C12B S2B C18B C19B 153(3) . . . . ?
C12B C11B C16B C10B 165(3) . . . . ?
C12B C11B C16B C15B 5(5) . . . . ?
C12B C13B C14B C15B -3(5) . . . . ?
C13B C14B C15B C16B 6(6) . . . . ?
C14B C15B C16B C10B -169(3) . . . . ?
C14B C15B C16B C11B -7(6) . . . . ?
C16B C11B C12B S2B 177(3) . . . . ?
C16B C11B C12B C13B -2(5) . . . . ?
C17B N1B C11B C12B -39(3) . . . . ?
C17B N1B C11B C16B 147(3) . . . . ?
C17B C18B C19B C20B 7(6) . . . . ?
C18B S2B C12B C11B 28(3) . . . . ?
C18B S2B C12B C13B -152(3) . . . . ?
C18B C17B C22B C21B 0(6) . . . . ?
C18B C19B C20B C21B -7(8) . . . . ?
C19B C20B C21B C22B 4(9) . . . . ?
C20B C21B C22B C17B 0(8) . . . . ?
C22B C17B C18B S2B -180(3) . . . . ?
C22B C17B C18B C19B -3(5) . . . . ?
_shelx_res_file
;
TITL 16srv102_a.res in Cc New: C2/c
16srv102.res
created by SHELXL-2018/3 at 15:47:42 on 26-Jul-2018
CELL 1.54178 16.7659 7.6903 28.1183 90 90.8986 90
ZERR 4 0.0044 0.0019 0.0072 0 0.0044 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H N O S
UNIT 176 152 8 8 12
RIGU
EADP N1 N1B
EADP C17B C11B
EADP C18B C12B
EXYZ N1 N1B
L.S. 7
PLAN -10
TEMP -153.15
CONN 4 S2B
BOND $H
CONF
fmap 2
acta
TWIN -1 0 0 0 -1 0 0 0 1 2
REM
REM
REM
WGHT 0.018900 7.232000
EXTI 0.000270
BASF 0.50313
FVAR 0.28945 0.85655
S1 5 0.500000 0.416003 0.250000 10.50000 0.07694 0.01505 =
0.04341 0.00000 -0.04114 0.00000
O1 4 0.559890 0.316794 0.225673 11.00000 0.09629 0.02791 =
0.05773 -0.01465 -0.04516 0.02681
C1 1 0.455160 0.575777 0.212957 11.00000 0.05437 0.02074 =
0.03264 0.00064 -0.02313 0.00019
C2 1 0.405523 0.547011 0.174426 11.00000 0.06250 0.01335 =
0.04343 -0.00234 -0.02555 0.00051
AFIX 43
H2 2 0.391856 0.431463 0.165557 11.00000 -1.20000
AFIX 0
C3 1 0.375242 0.686316 0.148386 11.00000 0.05452 0.01947 =
0.03855 -0.00244 -0.02437 0.00428
C4 1 0.396554 0.856037 0.162581 11.00000 0.05251 0.01807 =
0.03332 0.00262 -0.02005 0.00328
C5 1 0.444133 0.883217 0.203225 11.00000 0.05914 0.01510 =
0.03529 -0.00160 -0.02255 0.00013
AFIX 43
H5 2 0.455518 0.998220 0.213633 11.00000 -1.20000
AFIX 0
C6 1 0.474669 0.742329 0.228316 11.00000 0.05036 0.02098 =
0.03330 -0.00119 -0.02338 0.00063
C7 1 0.322124 0.647929 0.105733 11.00000 0.08351 0.01945 =
0.05106 -0.00306 -0.04547 0.00780
AFIX 13
H7 2 0.302879 0.761111 0.092327 11.00000 -1.20000
AFIX 0
C8 1 0.369056 0.556254 0.068065 11.00000 0.11861 0.07736 =
0.04361 -0.01411 -0.04430 0.01184
AFIX 137
H8A 2 0.387181 0.443259 0.080188 11.00000 -1.50000
H8B 2 0.415379 0.627055 0.059722 11.00000 -1.50000
H8C 2 0.335174 0.538742 0.039753 11.00000 -1.50000
AFIX 0
C9 1 0.249621 0.542298 0.120361 11.00000 0.07579 0.06411 =
0.10359 0.00013 -0.06004 -0.00682
AFIX 137
H9A 2 0.267262 0.431625 0.134233 11.00000 -1.50000
H9B 2 0.215684 0.519649 0.092349 11.00000 -1.50000
H9C 2 0.219292 0.607693 0.143908 11.00000 -1.50000
AFIX 0
PART 1
S2 5 0.319147 1.034796 0.032302 21.00000 0.07768 0.03274 =
0.03651 -0.00187 -0.03322 0.00285
N1 3 0.370519 1.004813 0.135321 21.00000 0.04718 0.01845 =
0.03607 0.00263 -0.01978 0.00298
C10 1 0.268101 1.062979 0.217939 21.00000 0.05197 0.04682 =
0.05152 -0.00362 0.00519 0.00947
AFIX 7
H10A 2 0.278353 0.941377 0.226481 21.00000 -1.50000
H10B 2 0.227005 1.110635 0.238639 21.00000 -1.50000
H10C 2 0.317366 1.130464 0.221938 21.00000 -1.50000
AFIX 0
C11 1 0.288687 1.045900 0.128434 21.00000 0.04661 0.01295 =
0.04839 0.00440 -0.02212 -0.00072
C12 1 0.259429 1.073043 0.082566 21.00000 0.07219 0.01763 =
0.04524 -0.00467 -0.03066 0.00474
C13 1 0.181086 1.117115 0.074330 21.00000 0.05457 0.03903 =
0.05904 -0.00037 -0.02772 -0.00732
AFIX 43
H13 2 0.161771 1.131631 0.042636 21.00000 -1.20000
AFIX 0
C14 1 0.131270 1.139955 0.111231 21.00000 0.04008 0.05277 =
0.09362 0.01267 -0.02369 0.00333
AFIX 43
H14 2 0.077170 1.171308 0.105468 21.00000 -1.20000
AFIX 0
C15 1 0.159765 1.117178 0.158094 21.00000 0.05440 0.04167 =
0.08523 0.00375 -0.00694 -0.00081
AFIX 43
H15 2 0.124320 1.130975 0.183853 21.00000 -1.20000
AFIX 0
C16 1 0.240488 1.074002 0.167409 21.00000 0.04646 0.02529 =
0.05546 0.00195 -0.00983 0.00125
C17 1 0.428596 1.082177 0.104503 21.00000 0.04713 0.01585 =
0.03918 0.00094 -0.01889 0.00698
C18 1 0.412194 1.104990 0.056075 21.00000 0.06515 0.02562 =
0.03767 -0.00341 -0.01254 0.00853
C19 1 0.466852 1.183585 0.026753 21.00000 0.07625 0.05573 =
0.04415 0.00336 -0.00643 0.00859
AFIX 43
H19 2 0.454148 1.199662 -0.005997 21.00000 -1.20000
AFIX 0
C20 1 0.539669 1.238954 0.044522 21.00000 0.06429 0.05827 =
0.05777 0.01029 0.00914 -0.00071
AFIX 43
H20 2 0.577721 1.289985 0.024093 21.00000 -1.20000
AFIX 0
C21 1 0.556386 1.219154 0.092324 21.00000 0.05466 0.03886 =
0.06225 0.00531 -0.00285 -0.00015
AFIX 43
H21 2 0.606042 1.258678 0.104964 21.00000 -1.20000
AFIX 0
C22 1 0.501702 1.142305 0.122235 21.00000 0.04539 0.02834 =
0.03962 -0.00264 -0.01248 0.00601
AFIX 43
H22 2 0.514145 1.130466 0.155154 21.00000 -1.20000
AFIX 0
SAME 0.02 0.04 S2 > C22
PART 0
PART 2
S2B 5 0.236359 1.044243 0.062394 -21.00000 0.05870
N1B 3 0.370519 1.004813 0.135321 -21.00000 0.04718 0.01845 =
0.03607 0.00263 -0.01978 0.00298
C10B 1 0.537208 1.103033 0.118679 -21.00000 0.06312
AFIX 33
H10D 2 0.588883 1.112422 0.103070 -21.00000 -1.50000
H10E 2 0.526771 1.209949 0.136497 -21.00000 -1.50000
H10F 2 0.538118 1.003834 0.140559 -21.00000 -1.50000
AFIX 0
C11B 1 0.392894 1.058319 0.090197 -21.00000 0.05264
C12B 1 0.338087 1.076023 0.053552 -21.00000 0.05469
C13B 1 0.359051 1.118622 0.008044 -21.00000 0.06954
AFIX 43
H13B 2 0.319278 1.131553 -0.016134 -21.00000 -1.20000
AFIX 0
C14B 1 0.436488 1.141881 -0.001983 -21.00000 0.07524
AFIX 43
H14B 2 0.453123 1.166429 -0.033419 -21.00000 -1.20000
AFIX 0
C15B 1 0.491422 1.128517 0.035630 -21.00000 0.06914
AFIX 43
H15B 2 0.545395 1.156403 0.029214 -21.00000 -1.20000
AFIX 0
C16B 1 0.473472 1.077167 0.082256 -21.00000 0.07061
C17B 1 0.294965 1.071953 0.153480 -21.00000 0.05264
C18B 1 0.230484 1.100766 0.123364 -21.00000 0.05469
C19B 1 0.158473 1.164196 0.140084 -21.00000 0.06816
AFIX 43
H19B 2 0.113216 1.170469 0.119399 -21.00000 -1.20000
AFIX 0
C20B 1 0.152791 1.217883 0.186609 -21.00000 0.11546
AFIX 43
H20B 2 0.105780 1.273585 0.197299 -21.00000 -1.20000
AFIX 0
C21B 1 0.216716 1.189583 0.217778 -21.00000 0.15108
AFIX 43
H21B 2 0.212170 1.219464 0.250406 -21.00000 -1.20000
AFIX 0
C22B 1 0.286966 1.118020 0.201441 -21.00000 0.08873
AFIX 43
H22B 2 0.330341 1.099876 0.223016 -21.00000 -1.20000
AFIX 0
HKLF 4
REM 16srv102_a.res in Cc New: C2/c
REM wR2 = 0.1068, GooF = S = 1.062, Restrained GooF = 1.032 for all data
REM R1 = 0.0493 for 3035 Fo > 4sig(Fo) and 0.0625 for all 3518 data
REM 291 parameters refined using 253 restraints
END
WGHT 0.0186 7.2446
REM Highest difference peak 0.311, deepest hole -0.331, 1-sigma level 0.052
Q1 1 0.2638 1.0464 0.0453 11.00000 0.05 0.31
Q2 1 0.4798 0.4059 0.2923 11.00000 0.05 0.30
Q3 1 0.5241 0.5010 0.2706 11.00000 0.05 0.24
Q4 1 0.4369 0.4419 0.2629 11.00000 0.05 0.24
Q5 1 0.3095 1.0414 0.0720 11.00000 0.05 0.23
Q6 1 0.3371 1.0466 -0.0075 11.00000 0.05 0.23
Q7 1 0.2828 1.1986 0.1221 11.00000 0.05 0.22
Q8 1 0.3239 0.7702 0.0824 11.00000 0.05 0.21
Q9 1 0.5382 0.7531 0.2317 11.00000 0.05 0.19
Q10 1 0.2993 1.1500 0.0174 11.00000 0.05 0.18
;
_shelx_res_checksum 71302
#===END
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone/d-chloroform'
_exptl_crystal_preparation Luminescent
#######################################################################
#
# 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_7-16s065
_database_code_depnum_ccdc_archive 'CCDC 1884011'
loop_
_audit_author_name
_audit_author_address
'Andrei S. Batsanov'
;Durham University
United Kingdom
;
_audit_update_record
;
2018-12-10 deposited with the CCDC. 2019-05-29 downloaded from the CCDC.
;
_ccdc_polymorph 'low-temperature phase'
_audit_creation_date 2016-02-22
_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 'C42 H34 N2 O2 S3'
_chemical_formula_sum 'C42 H34 N2 O2 S3'
_chemical_formula_weight 694.89
_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'
S S 0.1246 0.1234 '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 12.9513(10)
_cell_length_b 14.1812(11)
_cell_length_c 18.9798(15)
_cell_angle_alpha 76.632(3)
_cell_angle_beta 83.723(3)
_cell_angle_gamma 83.531(3)
_cell_volume 3357.3(5)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9918
_cell_measurement_temperature 120
_cell_measurement_theta_max 29.89
_cell_measurement_theta_min 2.27
_shelx_estimated_absorpt_T_max 0.985
_shelx_estimated_absorpt_T_min 0.921
_exptl_absorpt_coefficient_mu 0.263
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.9495
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1459 before and 0.0550 after correction.
The Ratio of minimum to maximum transmission is 0.9495.
The \l/2 correction factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.375
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description prism
_exptl_crystal_F_000 1456
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 1.00 0.0030
0.00 0.00 -1.00 0.0270
1.00 0.00 0.00 0.0300
-1.00 0.00 0.00 0.0320
0.00 1.00 0.00 0.1410
0.00 -1.00 0.00 0.1450
_exptl_crystal_size_max 0.319
_exptl_crystal_size_mid 0.067
_exptl_crystal_size_min 0.058
_exptl_special_details
; A reversible phase transition occurs on cooling below 180 K, with
doubling of the c parameter.
Data were collected in shutterless mode. Full sphere of reciprocal
space was nominally covered by 4 runs of narrow-frame \w-scans (scan
width 0.5\%, 30s exposure), every run at a different \f angle.
Two runs of \f-scans (scan width 1\%, 1.5s exposure) were used for
scaling overflowing intensities. Crystal to detector distance 3.49 cm.
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0469
_diffrn_reflns_av_unetI/netI 0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 53040
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 24.999
_diffrn_reflns_theta_max 24.999
_diffrn_reflns_theta_min 1.856
_diffrn_ambient_temperature 120
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type 'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device '3-circle area detector 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 'I\mS microsource'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 8686
_reflns_number_total 11804
_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 v8.34A (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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution 'ShelXS 2013/1 (Sheldrick, 2008)'
_refine_diff_density_max 0.442
_refine_diff_density_min -0.397
_refine_diff_density_rms 0.056
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.028
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 899
_refine_ls_number_reflns 11804
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0694
_refine_ls_R_factor_gt 0.0433
_refine_ls_restrained_S_all 1.028
_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^)+(0.0590P)^2^+1.6770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1082
_refine_ls_wR_factor_ref 0.1207
_refine_special_details
; Subcell with c/2 present, similar to the cell of high-T phase.
Methyl groups were refined as rigid bodies rotating around C---C bonds,
with a common refined U for three H atoms. Other H atoms: riding model.
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2. Others
Uiso(H38A)=Uiso(H38B)=Uiso(H38C)=FVAR(1)
Uiso(H41A)=Uiso(H41B)=Uiso(H41C)=FVAR(2)
Uiso(H39D)=Uiso(H39E)=Uiso(H39F)=FVAR(3)
Uiso(H38D)=Uiso(H38E)=Uiso(H38F)=FVAR(4)
Uiso(H42A)=Uiso(H42B)=Uiso(H42C)=FVAR(5)
Uiso(H39A)=Uiso(H39B)=Uiso(H39C)=FVAR(6)
Uiso(H42D)=Uiso(H42E)=Uiso(H42F)=FVAR(7)
Uiso(H41D)=Uiso(H41E)=Uiso(H41F)=FVAR(8)
3.a Ternary CH refined with riding coordinates:
C37B(H37B), C40A(H40A), C37A(H37A), C40B(H40B)
3.b Aromatic/amide H refined with riding coordinates:
C2A(H2A), C2B(H2B), C5B(H5B), C33A(H33A), C11A(H11A), C32B(H32B), C27B(H27B),
C14B(H14B), C17B(H17B), C28A(H28A), C26A(H26A), C35B(H35B), C11B(H11B),
C8B(H8B), C32A(H32A), C28B(H28B), C20A(H20A), C33B(H33B), C5A(H5A), C8A(H8A),
C35A(H35A), C14A(H14A), C26B(H26B), C27A(H27A), C21A(H21A), C15B(H15B),
C16B(H16B), C34B(H34B), C23B(H23B), C20B(H20B), C16A(H16A), C21B(H21B),
C15A(H15A), C22A(H22A), C17A(H17A), C29B(H29B), C29A(H29A), C34A(H34A),
C22B(H22B), C23A(H23A)
3.c Idealised Me refined as rotating group:
C38A(H38A,H38B,H38C), C41A(H41A,H41B,H41C), C39B(H39D,H39E,H39F), C38B(H38D,
H38E,H38F), C42A(H42A,H42B,H42C), C39A(H39A,H39B,H39C), C42B(H42D,H42E,H42F),
C41B(H41D,H41E,H41F)
;
_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
S1A S -0.01919(4) 0.54173(4) 0.11849(3) 0.01594(14) Uani 1 1 d . . . . .
S1B S -0.00556(4) 0.55237(4) 0.61471(3) 0.01795(15) Uani 1 1 d . . . . .
S3A S 0.34599(5) -0.03880(4) 0.24808(3) 0.02137(15) Uani 1 1 d . . . . .
S3B S 0.32785(5) -0.04047(4) 0.76328(3) 0.02467(16) Uani 1 1 d . . . . .
S2B S 0.56126(5) 0.76277(5) 0.72933(4) 0.03112(18) Uani 1 1 d . . . . .
S2A S 0.54446(5) 0.75617(5) 0.23081(4) 0.02975(17) Uani 1 1 d . . . . .
O2B O -0.02350(14) 0.58584(12) 0.53956(9) 0.0290(4) Uani 1 1 d . . . . .
O2A O -0.04021(13) 0.58132(12) 0.04438(9) 0.0239(4) Uani 1 1 d . . . . .
O1A O -0.10313(12) 0.54988(12) 0.17327(9) 0.0240(4) Uani 1 1 d . . . . .
N1A N 0.37179(14) 0.65117(14) 0.20089(10) 0.0186(4) Uani 1 1 d . . . . .
N2B N 0.21086(14) 0.15870(13) 0.70650(10) 0.0164(4) Uani 1 1 d . . . . .
N2A N 0.20848(14) 0.15012(13) 0.19201(10) 0.0148(4) Uani 1 1 d . . . . .
O1B O -0.09018(12) 0.56742(12) 0.66716(9) 0.0260(4) Uani 1 1 d . . . . .
N1B N 0.38504(15) 0.66362(14) 0.69597(11) 0.0202(5) Uani 1 1 d . . . . .
C12A C 0.03915(17) 0.42015(16) 0.13331(12) 0.0150(5) Uani 1 1 d . . . . .
C1B C 0.10846(17) 0.59734(17) 0.63351(12) 0.0160(5) Uani 1 1 d . . . . .
C31B C 0.29492(17) 0.12940(17) 0.65920(12) 0.0165(5) Uani 1 1 d . . . . .
C30A C 0.27298(17) 0.03679(16) 0.30042(12) 0.0159(5) Uani 1 1 d . . . . .
C4B C 0.29051(17) 0.64071(17) 0.67283(12) 0.0166(5) Uani 1 1 d . . . . .
C25A C 0.20982(17) 0.11900(16) 0.26905(12) 0.0161(5) Uani 1 1 d . . . . .
C30B C 0.26500(17) 0.03994(17) 0.81568(13) 0.0181(5) Uani 1 1 d . . . . .
C2A C 0.10916(17) 0.68290(17) 0.13371(12) 0.0158(5) Uani 1 1 d . . . . .
H2A H 0.0563 0.7329 0.1174 0.019 Uiso 1 1 calc R . . . .
C3A C 0.20270(17) 0.70618(17) 0.15224(12) 0.0158(5) Uani 1 1 d . . . . .
C25B C 0.21124(17) 0.12821(16) 0.78364(12) 0.0158(5) Uani 1 1 d . . . . .
C6A C 0.16813(17) 0.51056(16) 0.16248(12) 0.0160(5) Uani 1 1 d . . . . .
C37B C 0.24378(18) 0.82234(17) 0.63079(13) 0.0187(5) Uani 1 1 d . . . . .
H37B H 0.2785 0.8291 0.6737 0.022 Uiso 1 1 calc R . . . .
C2B C 0.12540(17) 0.69387(17) 0.62453(12) 0.0161(5) Uani 1 1 d . . . . .
H2B H 0.0739 0.7437 0.6056 0.019 Uiso 1 1 calc R . . . .
C5B C 0.27241(18) 0.54362(17) 0.68155(12) 0.0185(5) Uani 1 1 d . . . . .
H5B H 0.3223 0.4931 0.7020 0.022 Uiso 1 1 calc R . . . .
C31A C 0.29616(17) 0.12754(16) 0.14458(12) 0.0152(5) Uani 1 1 d . . . . .
C33A C 0.39760(19) 0.16290(18) 0.02816(13) 0.0223(6) Uani 1 1 d . . . . .
H33A H 0.4067 0.2016 -0.0197 0.027 Uiso 1 1 calc R . . . .
C9B C 0.15477(17) 0.25160(16) 0.68028(12) 0.0153(5) Uani 1 1 d . . . . .
C11A C -0.00102(17) 0.33958(16) 0.12195(12) 0.0159(5) Uani 1 1 d . . . . .
H11A H -0.0670 0.3461 0.1029 0.019 Uiso 1 1 calc R . . . .
C1A C 0.09371(17) 0.58678(17) 0.13913(12) 0.0157(5) Uani 1 1 d . . . . .
C40A C 0.01738(18) 0.15766(17) 0.12294(13) 0.0202(5) Uani 1 1 d . . . . .
H40A H 0.0803 0.1181 0.1064 0.024 Uiso 1 1 calc R . . . .
C13A C 0.37003(19) 0.65791(17) 0.27450(13) 0.0214(6) Uani 1 1 d . . . . .
C32B C 0.31527(18) 0.18509(18) 0.58917(13) 0.0207(5) Uani 1 1 d . . . . .
H32B H 0.2729 0.2436 0.5726 0.025 Uiso 1 1 calc R . . . .
C27B C 0.15671(19) 0.15374(19) 0.90448(13) 0.0249(6) Uani 1 1 d . . . . .
H27B H 0.1191 0.1931 0.9347 0.030 Uiso 1 1 calc R . . . .
C14B C 0.29948(19) 0.63993(19) 0.82023(14) 0.0264(6) Uani 1 1 d . . . . .
H14B H 0.2448 0.6108 0.8062 0.032 Uiso 1 1 calc R . . . .
C36B C 0.35799(18) 0.04291(17) 0.68138(13) 0.0188(5) Uani 1 1 d . . . . .
C10A C 0.05516(17) 0.24809(16) 0.13839(12) 0.0160(5) Uani 1 1 d . . . . .
C6B C 0.18082(17) 0.52140(16) 0.66016(12) 0.0158(5) Uani 1 1 d . . . . .
C3B C 0.21855(17) 0.71781(17) 0.64341(12) 0.0165(5) Uani 1 1 d . . . . .
C17B C 0.4591(2) 0.72125(19) 0.86388(15) 0.0320(7) Uani 1 1 d . . . . .
H17B H 0.5147 0.7480 0.8790 0.038 Uiso 1 1 calc R . . . .
C13B C 0.38125(18) 0.67139(17) 0.76959(13) 0.0217(6) Uani 1 1 d . . . . .
C12B C 0.04915(17) 0.42972(16) 0.63608(12) 0.0153(5) Uani 1 1 d . . . . .
C28A C 0.21314(19) 0.05969(19) 0.42052(13) 0.0251(6) Uani 1 1 d . . . . .
H28A H 0.2151 0.0403 0.4718 0.030 Uiso 1 1 calc R . . . .
C9A C 0.15043(17) 0.24285(16) 0.16813(11) 0.0142(5) Uani 1 1 d . . . . .
C26A C 0.14680(18) 0.16879(18) 0.31533(13) 0.0215(6) Uani 1 1 d . . . . .
H26A H 0.1020 0.2241 0.2954 0.026 Uiso 1 1 calc R . . . .
C35B C 0.44278(18) 0.01725(18) 0.63621(13) 0.0225(6) Uani 1 1 d . . . . .
H35B H 0.4882 -0.0391 0.6529 0.027 Uiso 1 1 calc R . . . .
C11B C 0.00447(18) 0.34796(17) 0.63162(12) 0.0172(5) Uani 1 1 d . . . . .
H11B H -0.0621 0.3540 0.6135 0.021 Uiso 1 1 calc R . . . .
C8B C 0.20017(17) 0.33473(17) 0.68372(12) 0.0167(5) Uani 1 1 d . . . . .
H8B H 0.2671 0.3293 0.7012 0.020 Uiso 1 1 calc R . . . .
C4A C 0.27641(17) 0.62894(17) 0.17809(12) 0.0170(5) Uani 1 1 d . . . . .
C36A C 0.36727(18) 0.04674(17) 0.16610(12) 0.0173(5) Uani 1 1 d . . . . .
C32A C 0.31178(18) 0.18498(18) 0.07438(12) 0.0197(5) Uani 1 1 d . . . . .
H32A H 0.2636 0.2393 0.0581 0.024 Uiso 1 1 calc R . . . .
C19B C 0.48093(18) 0.64653(17) 0.65528(13) 0.0216(6) Uani 1 1 d . . . . .
C28B C 0.21048(19) 0.06732(19) 0.93536(13) 0.0260(6) Uani 1 1 d . . . . .
H28B H 0.2105 0.0468 0.9867 0.031 Uiso 1 1 calc R . . . .
C18A C 0.44773(19) 0.70327(18) 0.29624(14) 0.0256(6) Uani 1 1 d . . . . .
C7A C 0.13699(17) 0.41488(16) 0.15945(12) 0.0149(5) Uani 1 1 d . . . . .
C38A C 0.30422(19) 0.83892(18) 0.07650(13) 0.0237(6) Uani 1 1 d . . . . .
H38A H 0.3691 0.7963 0.0832 0.028(4) Uiso 1 1 calc GR . . . .
H38B H 0.3189 0.9067 0.0708 0.028(4) Uiso 1 1 calc GR . . . .
H38C H 0.2744 0.8317 0.0329 0.028(4) Uiso 1 1 calc GR . . . .
C20A C 0.47745(19) 0.58378(18) 0.10417(14) 0.0247(6) Uani 1 1 d . . . . .
H20A H 0.4178 0.5593 0.0923 0.030 Uiso 1 1 calc R . . . .
C33B C 0.39744(18) 0.15502(19) 0.54366(13) 0.0234(6) Uani 1 1 d . . . . .
H33B H 0.4091 0.1921 0.4954 0.028 Uiso 1 1 calc R . . . .
C10B C 0.05727(17) 0.25608(17) 0.65373(12) 0.0164(5) Uani 1 1 d . . . . .
C5A C 0.25966(18) 0.53212(17) 0.18419(12) 0.0179(5) Uani 1 1 d . . . . .
H5A H 0.3104 0.4814 0.2030 0.021 Uiso 1 1 calc R . . . .
C8A C 0.19246(17) 0.32519(16) 0.17691(12) 0.0156(5) Uani 1 1 d . . . . .
H8A H 0.2591 0.3195 0.1949 0.019 Uiso 1 1 calc R . . . .
C19A C 0.46770(18) 0.63417(17) 0.16010(13) 0.0202(5) Uani 1 1 d . . . . .
C37A C 0.22661(17) 0.81090(17) 0.14283(13) 0.0182(5) Uani 1 1 d . . . . .
H37A H 0.2605 0.8154 0.1867 0.022 Uiso 1 1 calc R . . . .
C35A C 0.45435(18) 0.02802(17) 0.12021(13) 0.0203(5) Uani 1 1 d . . . . .
H35A H 0.5043 -0.0249 0.1363 0.024 Uiso 1 1 calc R . . . .
C41A C -0.0560(2) 0.18009(19) 0.06264(14) 0.0280(6) Uani 1 1 d . . . . .
H41A H -0.1245 0.2062 0.0808 0.046(5) Uiso 1 1 calc GR . . . .
H41B H -0.0633 0.1203 0.0468 0.046(5) Uiso 1 1 calc GR . . . .
H41C H -0.0275 0.2283 0.0215 0.046(5) Uiso 1 1 calc GR . . . .
C14A C 0.2918(2) 0.62090(19) 0.32647(13) 0.0265(6) Uani 1 1 d . . . . .
H14A H 0.2397 0.5875 0.3134 0.032 Uiso 1 1 calc R . . . .
C24B C 0.57100(19) 0.68291(18) 0.66940(14) 0.0250(6) Uani 1 1 d . . . . .
C40B C 0.01289(18) 0.16535(18) 0.64554(13) 0.0224(6) Uani 1 1 d . . . . .
H40B H 0.0468 0.1083 0.6793 0.027 Uiso 1 1 calc R . . . .
C26B C 0.15717(18) 0.18372(18) 0.82936(13) 0.0206(5) Uani 1 1 d . . . . .
H26B H 0.1196 0.2435 0.8089 0.025 Uiso 1 1 calc R . . . .
C39B C 0.14741(19) 0.89606(18) 0.62278(14) 0.0245(6) Uani 1 1 d . . . . .
H39D H 0.0954 0.8770 0.6638 0.022(4) Uiso 1 1 calc GR . . . .
H39E H 0.1176 0.8975 0.5772 0.022(4) Uiso 1 1 calc GR . . . .
H39F H 0.1675 0.9608 0.6222 0.022(4) Uiso 1 1 calc GR . . . .
C7B C 0.14736(17) 0.42482(16) 0.66162(12) 0.0150(5) Uani 1 1 d . . . . .
C38B C 0.32055(19) 0.84660(18) 0.56364(13) 0.0244(6) Uani 1 1 d . . . . .
H38D H 0.2899 0.8369 0.5212 0.031(4) Uiso 1 1 calc GR . . . .
H38E H 0.3853 0.8039 0.5710 0.031(4) Uiso 1 1 calc GR . . . .
H38F H 0.3358 0.9146 0.5556 0.031(4) Uiso 1 1 calc GR . . . .
C27A C 0.14843(19) 0.13893(19) 0.38993(13) 0.0256(6) Uani 1 1 d . . . . .
H27A H 0.1042 0.1736 0.4205 0.031 Uiso 1 1 calc R . . . .
C18B C 0.4618(2) 0.71216(17) 0.79247(14) 0.0256(6) Uani 1 1 d . . . . .
C21A C 0.57265(19) 0.56921(19) 0.06603(15) 0.0285(6) Uani 1 1 d . . . . .
H21A H 0.5773 0.5368 0.0271 0.034 Uiso 1 1 calc R . . . .
C15B C 0.2972(2) 0.6509(2) 0.89140(15) 0.0312(6) Uani 1 1 d . . . . .
H15B H 0.2404 0.6299 0.9253 0.037 Uiso 1 1 calc R . . . .
C24A C 0.55673(19) 0.67206(18) 0.17407(14) 0.0242(6) Uani 1 1 d . . . . .
C16B C 0.3763(2) 0.6917(2) 0.91316(16) 0.0353(7) Uani 1 1 d . . . . .
H16B H 0.3739 0.6995 0.9617 0.042 Uiso 1 1 calc R . . . .
C42A C -0.0333(2) 0.0950(2) 0.19121(14) 0.0315(7) Uani 1 1 d . . . . .
H42A H 0.0152 0.0794 0.2293 0.040(5) Uiso 1 1 calc GR . . . .
H42B H -0.0508 0.0347 0.1804 0.040(5) Uiso 1 1 calc GR . . . .
H42C H -0.0970 0.1306 0.2080 0.040(5) Uiso 1 1 calc GR . . . .
C34B C 0.46160(19) 0.07345(18) 0.56677(14) 0.0244(6) Uani 1 1 d . . . . .
H34B H 0.5189 0.0551 0.5355 0.029 Uiso 1 1 calc R . . . .
C23B C 0.66557(19) 0.66507(19) 0.63164(15) 0.0316(7) Uani 1 1 d . . . . .
H23B H 0.7265 0.6867 0.6442 0.038 Uiso 1 1 calc R . . . .
C20B C 0.48937(19) 0.59774(18) 0.59886(14) 0.0261(6) Uani 1 1 d . . . . .
H20B H 0.4294 0.5730 0.5876 0.031 Uiso 1 1 calc R . . . .
C16A C 0.3654(2) 0.6790(2) 0.41760(16) 0.0378(7) Uani 1 1 d . . . . .
H16A H 0.3628 0.6872 0.4660 0.045 Uiso 1 1 calc R . . . .
C21B C 0.5843(2) 0.58459(19) 0.55860(16) 0.0320(6) Uani 1 1 d . . . . .
H21B H 0.5881 0.5536 0.5189 0.038 Uiso 1 1 calc R . . . .
C15A C 0.2896(2) 0.6325(2) 0.39726(14) 0.0323(7) Uani 1 1 d . . . . .
H15A H 0.2351 0.6081 0.4321 0.039 Uiso 1 1 calc R . . . .
C39A C 0.12993(19) 0.88405(18) 0.13634(15) 0.0272(6) Uani 1 1 d . . . . .
H39A H 0.1021 0.8896 0.0894 0.023(4) Uiso 1 1 calc GR . . . .
H39B H 0.1489 0.9477 0.1397 0.023(4) Uiso 1 1 calc GR . . . .
H39C H 0.0768 0.8617 0.1758 0.023(4) Uiso 1 1 calc GR . . . .
C22A C 0.6616(2) 0.6012(2) 0.08387(16) 0.0330(7) Uani 1 1 d . . . . .
H22A H 0.7276 0.5882 0.0591 0.040 Uiso 1 1 calc R . . . .
C17A C 0.4451(2) 0.7134(2) 0.36741(15) 0.0336(7) Uani 1 1 d . . . . .
H17A H 0.4984 0.7443 0.3815 0.040 Uiso 1 1 calc R . . . .
C29B C 0.26447(18) 0.01089(18) 0.89058(13) 0.0217(6) Uani 1 1 d . . . . .
H29B H 0.3018 -0.0488 0.9115 0.026 Uiso 1 1 calc R . . . .
C29A C 0.27498(18) 0.00906(18) 0.37541(13) 0.0213(5) Uani 1 1 d . . . . .
H29A H 0.3198 -0.0458 0.3959 0.026 Uiso 1 1 calc R . . . .
C34A C 0.46875(19) 0.08627(18) 0.05095(13) 0.0226(6) Uani 1 1 d . . . . .
H34A H 0.5280 0.0728 0.0195 0.027 Uiso 1 1 calc R . . . .
C42B C -0.1043(2) 0.1662(2) 0.66354(16) 0.0383(7) Uani 1 1 d . . . . .
H42D H -0.1398 0.2096 0.6236 0.080(7) Uiso 1 1 calc GR . . . .
H42E H -0.1237 0.1895 0.7084 0.080(7) Uiso 1 1 calc GR . . . .
H42F H -0.1252 0.1002 0.6702 0.080(7) Uiso 1 1 calc GR . . . .
C22B C 0.6733(2) 0.6167(2) 0.57637(17) 0.0361(7) Uani 1 1 d . . . . .
H22B H 0.7388 0.6053 0.5505 0.043 Uiso 1 1 calc R . . . .
C41B C 0.0392(2) 0.1514(2) 0.56887(15) 0.0364(7) Uani 1 1 d . . . . .
H41D H 0.1151 0.1444 0.5585 0.051(5) Uiso 1 1 calc GR . . . .
H41E H 0.0095 0.2080 0.5346 0.051(5) Uiso 1 1 calc GR . . . .
H41F H 0.0100 0.0927 0.5638 0.051(5) Uiso 1 1 calc GR . . . .
C23A C 0.65262(19) 0.65219(19) 0.13803(15) 0.0292(6) Uani 1 1 d . . . . .
H23A H 0.7132 0.6741 0.1509 0.035 Uiso 1 1 calc R . . . .
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
S1A 0.0137(3) 0.0129(3) 0.0215(3) -0.0036(2) -0.0056(2) 0.0007(2)
S1B 0.0174(3) 0.0129(3) 0.0241(3) -0.0026(3) -0.0091(3) 0.0001(2)
S3A 0.0275(3) 0.0109(3) 0.0242(3) -0.0029(3) -0.0027(3) 0.0032(3)
S3B 0.0347(4) 0.0124(3) 0.0253(3) -0.0029(3) -0.0041(3) 0.0036(3)
S2B 0.0287(4) 0.0188(4) 0.0485(4) -0.0032(3) -0.0193(3) -0.0071(3)
S2A 0.0263(3) 0.0191(4) 0.0486(4) -0.0104(3) -0.0169(3) -0.0030(3)
O2B 0.0393(11) 0.0201(10) 0.0285(10) -0.0004(8) -0.0193(9) -0.0010(8)
O2A 0.0269(9) 0.0202(9) 0.0248(9) -0.0015(8) -0.0127(8) 0.0003(8)
O1A 0.0168(8) 0.0243(10) 0.0311(10) -0.0085(8) 0.0010(8) -0.0009(7)
N1A 0.0181(10) 0.0158(11) 0.0239(11) -0.0052(9) -0.0094(9) -0.0012(9)
N2B 0.0165(10) 0.0123(10) 0.0189(10) -0.0011(8) -0.0023(8) 0.0004(8)
N2A 0.0144(10) 0.0126(10) 0.0168(10) -0.0019(8) -0.0041(8) 0.0016(8)
O1B 0.0157(9) 0.0230(10) 0.0393(11) -0.0093(8) -0.0020(8) 0.0022(7)
N1B 0.0185(10) 0.0179(11) 0.0251(11) -0.0026(9) -0.0096(9) -0.0031(9)
C12A 0.0150(11) 0.0139(12) 0.0157(12) -0.0030(10) -0.0017(10) 0.0010(10)
C1B 0.0154(11) 0.0166(13) 0.0162(12) -0.0026(10) -0.0035(10) -0.0023(10)
C31B 0.0153(12) 0.0160(13) 0.0208(12) -0.0082(10) -0.0026(10) -0.0029(10)
C30A 0.0143(11) 0.0112(12) 0.0222(13) -0.0022(10) -0.0023(10) -0.0036(10)
C4B 0.0166(12) 0.0160(13) 0.0176(12) -0.0030(10) -0.0046(10) -0.0020(10)
C25A 0.0133(11) 0.0146(13) 0.0204(12) -0.0014(10) -0.0041(10) -0.0038(10)
C30B 0.0154(12) 0.0138(12) 0.0249(13) -0.0026(10) -0.0030(10) -0.0028(10)
C2A 0.0162(12) 0.0137(12) 0.0170(12) -0.0030(10) -0.0039(10) 0.0031(10)
C3A 0.0180(12) 0.0149(13) 0.0147(12) -0.0042(10) -0.0011(10) -0.0010(10)
C25B 0.0118(11) 0.0146(13) 0.0206(12) -0.0018(10) -0.0014(10) -0.0044(10)
C6A 0.0182(12) 0.0130(12) 0.0158(12) -0.0010(10) -0.0031(10) -0.0004(10)
C37B 0.0209(12) 0.0158(13) 0.0209(13) -0.0047(10) -0.0066(10) -0.0025(10)
C2B 0.0173(12) 0.0129(12) 0.0173(12) -0.0029(10) -0.0036(10) 0.0026(10)
C5B 0.0188(12) 0.0147(13) 0.0204(12) 0.0005(10) -0.0070(10) 0.0017(10)
C31A 0.0149(11) 0.0134(12) 0.0193(12) -0.0066(10) -0.0023(10) -0.0026(10)
C33A 0.0265(13) 0.0249(15) 0.0174(12) -0.0069(11) -0.0004(11) -0.0065(12)
C9B 0.0183(12) 0.0127(12) 0.0134(11) -0.0015(9) -0.0005(10) 0.0011(10)
C11A 0.0124(11) 0.0175(13) 0.0173(12) -0.0016(10) -0.0031(10) -0.0022(10)
C1A 0.0142(11) 0.0185(13) 0.0144(12) -0.0032(10) -0.0039(10) -0.0006(10)
C40A 0.0165(12) 0.0136(13) 0.0307(14) -0.0045(11) -0.0051(11) 0.0002(10)
C13A 0.0243(13) 0.0132(13) 0.0279(14) -0.0047(11) -0.0136(11) 0.0042(11)
C32B 0.0208(13) 0.0188(13) 0.0229(13) -0.0052(11) -0.0016(11) -0.0021(11)
C27B 0.0209(13) 0.0280(15) 0.0244(14) -0.0058(12) 0.0030(11) -0.0014(11)
C14B 0.0256(14) 0.0238(15) 0.0323(15) -0.0087(12) -0.0115(12) 0.0017(12)
C36B 0.0205(12) 0.0159(13) 0.0227(13) -0.0076(10) -0.0071(11) -0.0016(10)
C10A 0.0166(12) 0.0134(12) 0.0167(12) -0.0013(10) -0.0006(10) -0.0007(10)
C6B 0.0175(12) 0.0136(13) 0.0153(12) -0.0014(10) -0.0013(10) -0.0011(10)
C3B 0.0194(12) 0.0164(13) 0.0142(12) -0.0047(10) -0.0016(10) -0.0011(10)
C17B 0.0344(16) 0.0206(15) 0.0468(18) -0.0128(13) -0.0248(14) 0.0040(12)
C13B 0.0231(13) 0.0138(13) 0.0294(14) -0.0037(11) -0.0134(11) 0.0021(11)
C12B 0.0149(11) 0.0142(12) 0.0155(12) -0.0014(10) -0.0016(10) 0.0014(10)
C28A 0.0265(14) 0.0286(15) 0.0180(13) -0.0018(11) -0.0023(11) 0.0004(12)
C9A 0.0168(12) 0.0118(12) 0.0116(11) 0.0003(9) 0.0010(9) 0.0011(10)
C26A 0.0175(12) 0.0213(14) 0.0233(13) -0.0031(11) -0.0008(11) 0.0028(11)
C35B 0.0198(13) 0.0186(14) 0.0320(15) -0.0118(12) -0.0063(11) 0.0026(11)
C11B 0.0165(12) 0.0179(13) 0.0179(12) -0.0032(10) -0.0048(10) -0.0030(10)
C8B 0.0133(11) 0.0184(13) 0.0180(12) -0.0026(10) -0.0033(10) -0.0007(10)
C4A 0.0184(12) 0.0174(13) 0.0163(12) -0.0042(10) -0.0038(10) -0.0027(10)
C36A 0.0202(12) 0.0141(13) 0.0210(12) -0.0082(10) -0.0042(10) -0.0044(10)
C32A 0.0226(13) 0.0184(13) 0.0193(13) -0.0057(10) -0.0037(11) -0.0016(11)
C19B 0.0182(12) 0.0132(13) 0.0318(14) 0.0012(11) -0.0096(11) 0.0003(10)
C28B 0.0252(14) 0.0326(16) 0.0194(13) -0.0023(12) -0.0034(11) -0.0043(12)
C18A 0.0282(14) 0.0140(13) 0.0379(15) -0.0088(12) -0.0179(12) 0.0043(11)
C7A 0.0164(12) 0.0149(12) 0.0137(11) -0.0030(10) -0.0030(10) -0.0012(10)
C38A 0.0251(13) 0.0156(13) 0.0287(14) -0.0006(11) -0.0032(11) -0.0029(11)
C20A 0.0220(13) 0.0194(14) 0.0352(15) -0.0074(12) -0.0089(12) -0.0027(11)
C33B 0.0222(13) 0.0277(15) 0.0229(13) -0.0094(11) 0.0020(11) -0.0088(12)
C10B 0.0168(12) 0.0160(13) 0.0158(12) -0.0022(10) -0.0019(10) -0.0016(10)
C5A 0.0170(12) 0.0148(13) 0.0205(12) -0.0008(10) -0.0059(10) 0.0020(10)
C8A 0.0126(11) 0.0161(13) 0.0183(12) -0.0031(10) -0.0035(10) -0.0008(10)
C19A 0.0186(12) 0.0112(12) 0.0297(14) -0.0001(11) -0.0094(11) 0.0013(10)
C37A 0.0202(12) 0.0138(13) 0.0220(13) -0.0040(10) -0.0071(10) -0.0022(10)
C35A 0.0176(12) 0.0152(13) 0.0309(14) -0.0111(11) -0.0024(11) 0.0002(10)
C41A 0.0323(15) 0.0246(15) 0.0306(15) -0.0109(12) -0.0065(12) -0.0044(12)
C14A 0.0298(14) 0.0234(15) 0.0285(14) -0.0071(12) -0.0138(12) 0.0025(12)
C24B 0.0226(13) 0.0145(13) 0.0357(15) 0.0041(11) -0.0136(12) -0.0025(11)
C40B 0.0239(13) 0.0162(13) 0.0272(14) -0.0012(11) -0.0092(11) -0.0026(11)
C26B 0.0175(12) 0.0173(13) 0.0245(13) -0.0012(11) -0.0001(11) 0.0005(10)
C39B 0.0259(13) 0.0158(13) 0.0311(15) -0.0044(11) -0.0029(12) 0.0003(11)
C7B 0.0148(11) 0.0137(13) 0.0152(12) -0.0014(10) -0.0010(10) -0.0003(10)
C38B 0.0246(13) 0.0166(14) 0.0295(14) -0.0002(11) -0.0017(12) -0.0029(11)
C27A 0.0247(13) 0.0286(15) 0.0214(13) -0.0058(12) 0.0020(11) 0.0036(12)
C18B 0.0290(14) 0.0113(13) 0.0387(16) -0.0051(11) -0.0196(12) 0.0040(11)
C21A 0.0241(14) 0.0236(15) 0.0387(16) -0.0092(12) -0.0059(12) 0.0017(12)
C15B 0.0305(15) 0.0309(16) 0.0331(15) -0.0105(13) -0.0095(13) 0.0071(13)
C24A 0.0219(13) 0.0152(13) 0.0351(15) -0.0009(11) -0.0134(12) 0.0010(11)
C16B 0.0473(18) 0.0277(16) 0.0352(16) -0.0152(13) -0.0195(15) 0.0113(14)
C42A 0.0312(15) 0.0289(16) 0.0343(16) -0.0033(13) -0.0023(13) -0.0113(13)
C34B 0.0198(13) 0.0260(15) 0.0306(14) -0.0135(12) 0.0001(11) -0.0030(11)
C23B 0.0187(13) 0.0231(15) 0.0492(18) 0.0036(13) -0.0126(13) -0.0001(11)
C20B 0.0223(13) 0.0186(14) 0.0366(15) -0.0039(12) -0.0061(12) -0.0003(11)
C16A 0.0534(19) 0.0339(17) 0.0315(16) -0.0166(14) -0.0232(15) 0.0113(15)
C21B 0.0274(15) 0.0242(15) 0.0421(17) -0.0043(13) -0.0052(13) 0.0032(12)
C15A 0.0404(16) 0.0287(16) 0.0270(15) -0.0062(12) -0.0090(13) 0.0053(13)
C39A 0.0250(14) 0.0144(14) 0.0432(16) -0.0088(12) -0.0043(12) 0.0005(11)
C22A 0.0196(14) 0.0274(16) 0.0477(18) -0.0021(14) -0.0015(13) 0.0014(12)
C17A 0.0393(16) 0.0259(16) 0.0421(17) -0.0147(13) -0.0233(14) 0.0037(13)
C29B 0.0185(12) 0.0190(14) 0.0251(14) 0.0014(11) -0.0049(11) -0.0018(11)
C29A 0.0187(12) 0.0175(13) 0.0246(13) 0.0026(11) -0.0056(11) -0.0005(10)
C34A 0.0240(13) 0.0235(14) 0.0229(13) -0.0102(11) 0.0016(11) -0.0062(11)
C42B 0.0317(16) 0.0363(18) 0.0512(19) -0.0154(15) 0.0021(14) -0.0156(14)
C22B 0.0193(14) 0.0283(16) 0.0529(19) 0.0032(14) -0.0016(13) 0.0044(12)
C41B 0.0423(17) 0.0325(17) 0.0395(17) -0.0185(14) -0.0029(14) -0.0042(14)
C23A 0.0185(13) 0.0216(15) 0.0464(17) -0.0016(13) -0.0121(13) -0.0009(11)
_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
S1A O2A 1.4324(17) . ?
S1A O1A 1.4340(17) . ?
S1A C12A 1.775(2) . ?
S1A C1A 1.775(2) . ?
S1B O2B 1.4312(17) . ?
S1B O1B 1.4299(17) . ?
S1B C1B 1.774(2) . ?
S1B C12B 1.775(2) . ?
S3A C30A 1.757(2) . ?
S3A C36A 1.754(2) . ?
S3B C30B 1.758(2) . ?
S3B C36B 1.757(2) . ?
S2B C24B 1.768(3) . ?
S2B C18B 1.756(3) . ?
S2A C18A 1.765(3) . ?
S2A C24A 1.767(3) . ?
N1A C13A 1.420(3) . ?
N1A C4A 1.442(3) . ?
N1A C19A 1.417(3) . ?
N2B C31B 1.421(3) . ?
N2B C25B 1.428(3) . ?
N2B C9B 1.439(3) . ?
N2A C25A 1.428(3) . ?
N2A C31A 1.425(3) . ?
N2A C9A 1.441(3) . ?
N1B C4B 1.439(3) . ?
N1B C13B 1.422(3) . ?
N1B C19B 1.416(3) . ?
C12A C11A 1.377(3) . ?
C12A C7A 1.399(3) . ?
C1B C2B 1.379(3) . ?
C1B C6B 1.385(3) . ?
C31B C32B 1.395(3) . ?
C31B C36B 1.400(3) . ?
C30A C25A 1.398(3) . ?
C30A C29A 1.389(3) . ?
C4B C5B 1.392(3) . ?
C4B C3B 1.406(3) . ?
C25A C26A 1.392(3) . ?
C30B C25B 1.402(3) . ?
C30B C29B 1.385(3) . ?
C2A C3A 1.392(3) . ?
C2A C1A 1.379(3) . ?
C3A C4A 1.404(3) . ?
C3A C37A 1.517(3) . ?
C25B C26B 1.386(3) . ?
C6A C1A 1.390(3) . ?
C6A C7A 1.474(3) . ?
C6A C5A 1.384(3) . ?
C37B C3B 1.513(3) . ?
C37B C39B 1.532(3) . ?
C37B C38B 1.526(3) . ?
C2B C3B 1.394(3) . ?
C5B C6B 1.386(3) . ?
C31A C36A 1.399(3) . ?
C31A C32A 1.399(3) . ?
C33A C32A 1.392(3) . ?
C33A C34A 1.364(3) . ?
C9B C8B 1.393(3) . ?
C9B C10B 1.400(3) . ?
C11A C10A 1.400(3) . ?
C40A C10A 1.522(3) . ?
C40A C41A 1.522(3) . ?
C40A C42A 1.521(3) . ?
C13A C18A 1.399(3) . ?
C13A C14A 1.392(4) . ?
C32B C33B 1.388(3) . ?
C27B C28B 1.377(3) . ?
C27B C26B 1.390(3) . ?
C14B C13B 1.389(4) . ?
C14B C15B 1.392(4) . ?
C36B C35B 1.386(3) . ?
C10A C9A 1.400(3) . ?
C6B C7B 1.476(3) . ?
C17B C18B 1.387(4) . ?
C17B C16B 1.379(4) . ?
C13B C18B 1.401(3) . ?
C12B C11B 1.376(3) . ?
C12B C7B 1.399(3) . ?
C28A C27A 1.376(3) . ?
C28A C29A 1.377(3) . ?
C9A C8A 1.393(3) . ?
C26A C27A 1.383(3) . ?
C35B C34B 1.385(3) . ?
C11B C10B 1.397(3) . ?
C8B C7B 1.376(3) . ?
C4A C5A 1.391(3) . ?
C36A C35A 1.388(3) . ?
C19B C24B 1.402(3) . ?
C19B C20B 1.392(4) . ?
C28B C29B 1.382(3) . ?
C18A C17A 1.388(4) . ?
C7A C8A 1.377(3) . ?
C38A C37A 1.528(3) . ?
C20A C19A 1.398(3) . ?
C20A C21A 1.380(3) . ?
C33B C34B 1.360(3) . ?
C10B C40B 1.513(3) . ?
C19A C24A 1.400(3) . ?
C37A C39A 1.530(3) . ?
C35A C34A 1.387(3) . ?
C14A C15A 1.388(4) . ?
C24B C23B 1.378(4) . ?
C40B C42B 1.519(3) . ?
C40B C41B 1.511(3) . ?
C21A C22A 1.386(4) . ?
C15B C16B 1.375(4) . ?
C24A C23A 1.384(3) . ?
C23B C22B 1.370(4) . ?
C20B C21B 1.392(4) . ?
C16A C15A 1.376(4) . ?
C16A C17A 1.376(4) . ?
C21B C22B 1.387(4) . ?
C22A C23A 1.375(4) . ?
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
O2A S1A O1A 117.24(10) . . ?
O2A S1A C12A 113.07(10) . . ?
O2A S1A C1A 110.99(10) . . ?
O1A S1A C12A 109.79(10) . . ?
O1A S1A C1A 110.31(10) . . ?
C1A S1A C12A 92.79(11) . . ?
O2B S1B C1B 110.70(11) . . ?
O2B S1B C12B 112.89(11) . . ?
O1B S1B O2B 117.45(11) . . ?
O1B S1B C1B 110.49(10) . . ?
O1B S1B C12B 109.90(10) . . ?
C1B S1B C12B 92.69(11) . . ?
C36A S3A C30A 99.67(11) . . ?
C36B S3B C30B 99.89(11) . . ?
C18B S2B C24B 99.40(12) . . ?
C24A S2A C18A 98.73(12) . . ?
C13A N1A C4A 116.63(19) . . ?
C19A N1A C13A 120.54(19) . . ?
C19A N1A C4A 119.53(18) . . ?
C31B N2B C25B 121.48(18) . . ?
C31B N2B C9B 116.39(17) . . ?
C25B N2B C9B 115.56(18) . . ?
C25A N2A C9A 114.29(17) . . ?
C31A N2A C25A 121.05(18) . . ?
C31A N2A C9A 115.81(17) . . ?
C13B N1B C4B 116.20(19) . . ?
C19B N1B C4B 119.01(19) . . ?
C19B N1B C13B 121.56(19) . . ?
C11A C12A S1A 127.80(17) . . ?
C11A C12A C7A 122.2(2) . . ?
C7A C12A S1A 110.04(16) . . ?
C2B C1B S1B 126.30(18) . . ?
C2B C1B C6B 123.0(2) . . ?
C6B C1B S1B 110.73(17) . . ?
C32B C31B N2B 120.8(2) . . ?
C32B C31B C36B 118.4(2) . . ?
C36B C31B N2B 120.7(2) . . ?
C25A C30A S3A 122.01(17) . . ?
C29A C30A S3A 117.60(18) . . ?
C29A C30A C25A 120.3(2) . . ?
C5B C4B N1B 119.2(2) . . ?
C5B C4B C3B 122.3(2) . . ?
C3B C4B N1B 118.5(2) . . ?
C30A C25A N2A 121.2(2) . . ?
C26A C25A N2A 120.9(2) . . ?
C26A C25A C30A 117.9(2) . . ?
C25B C30B S3B 121.59(18) . . ?
C29B C30B S3B 117.90(18) . . ?
C29B C30B C25B 120.4(2) . . ?
C1A C2A C3A 119.6(2) . . ?
C2A C3A C4A 117.5(2) . . ?
C2A C3A C37A 121.8(2) . . ?
C4A C3A C37A 120.6(2) . . ?
C30B C25B N2B 120.9(2) . . ?
C26B C25B N2B 121.3(2) . . ?
C26B C25B C30B 117.8(2) . . ?
C1A C6A C7A 113.1(2) . . ?
C5A C6A C1A 118.3(2) . . ?
C5A C6A C7A 128.5(2) . . ?
C3B C37B C39B 113.53(19) . . ?
C3B C37B C38B 110.05(19) . . ?
C38B C37B C39B 109.5(2) . . ?
C1B C2B C3B 119.6(2) . . ?
C6B C5B C4B 119.3(2) . . ?
C36A C31A N2A 121.24(19) . . ?
C36A C31A C32A 118.3(2) . . ?
C32A C31A N2A 120.4(2) . . ?
C34A C33A C32A 120.7(2) . . ?
C8B C9B N2B 117.7(2) . . ?
C8B C9B C10B 122.3(2) . . ?
C10B C9B N2B 120.0(2) . . ?
C12A C11A C10A 120.1(2) . . ?
C2A C1A S1A 126.70(18) . . ?
C2A C1A C6A 122.8(2) . . ?
C6A C1A S1A 110.49(17) . . ?
C10A C40A C41A 113.5(2) . . ?
C10A C40A C42A 111.6(2) . . ?
C42A C40A C41A 110.0(2) . . ?
C18A C13A N1A 120.0(2) . . ?
C14A C13A N1A 121.6(2) . . ?
C14A C13A C18A 118.3(2) . . ?
C33B C32B C31B 120.0(2) . . ?
C28B C27B C26B 120.3(2) . . ?
C13B C14B C15B 120.4(2) . . ?
C31B C36B S3B 121.79(18) . . ?
C35B C36B S3B 117.76(18) . . ?
C35B C36B C31B 120.3(2) . . ?
C11A C10A C40A 122.3(2) . . ?
C9A C10A C11A 117.2(2) . . ?
C9A C10A C40A 120.5(2) . . ?
C1B C6B C5B 118.3(2) . . ?
C1B C6B C7B 113.1(2) . . ?
C5B C6B C7B 128.6(2) . . ?
C4B C3B C37B 120.7(2) . . ?
C2B C3B C4B 117.5(2) . . ?
C2B C3B C37B 121.8(2) . . ?
C16B C17B C18B 120.5(2) . . ?
C14B C13B N1B 122.1(2) . . ?
C14B C13B C18B 118.3(2) . . ?
C18B C13B N1B 119.6(2) . . ?
C11B C12B S1B 127.48(18) . . ?
C11B C12B C7B 122.3(2) . . ?
C7B C12B S1B 110.17(16) . . ?
C29A C28A C27A 118.7(2) . . ?
C10A C9A N2A 120.4(2) . . ?
C8A C9A N2A 117.28(19) . . ?
C8A C9A C10A 122.3(2) . . ?
C27A C26A C25A 120.9(2) . . ?
C36B C35B C34B 120.3(2) . . ?
C12B C11B C10B 119.8(2) . . ?
C7B C8B C9B 119.5(2) . . ?
C3A C4A N1A 118.5(2) . . ?
C5A C4A N1A 119.0(2) . . ?
C5A C4A C3A 122.5(2) . . ?
C31A C36A S3A 121.97(17) . . ?
C35A C36A S3A 117.48(18) . . ?
C35A C36A C31A 120.4(2) . . ?
C33A C32A C31A 120.3(2) . . ?
C24B C19B N1B 119.8(2) . . ?
C20B C19B N1B 122.5(2) . . ?
C20B C19B C24B 117.6(2) . . ?
C27B C28B C29B 119.0(2) . . ?
C13A C18A S2A 119.4(2) . . ?
C17A C18A S2A 119.7(2) . . ?
C17A C18A C13A 120.7(3) . . ?
C12A C7A C6A 113.2(2) . . ?
C8A C7A C12A 118.4(2) . . ?
C8A C7A C6A 128.4(2) . . ?
C21A C20A C19A 120.8(2) . . ?
C34B C33B C32B 121.3(2) . . ?
C9B C10B C40B 121.4(2) . . ?
C11B C10B C9B 117.6(2) . . ?
C11B C10B C40B 121.0(2) . . ?
C6A C5A C4A 119.2(2) . . ?
C7A C8A C9A 119.7(2) . . ?
C20A C19A N1A 123.0(2) . . ?
C20A C19A C24A 117.7(2) . . ?
C24A C19A N1A 119.2(2) . . ?
C3A C37A C38A 110.12(19) . . ?
C3A C37A C39A 113.80(19) . . ?
C38A C37A C39A 109.6(2) . . ?
C34A C35A C36A 120.3(2) . . ?
C15A C14A C13A 120.3(2) . . ?
C19B C24B S2B 119.8(2) . . ?
C23B C24B S2B 119.19(19) . . ?
C23B C24B C19B 120.7(2) . . ?
C10B C40B C42B 113.7(2) . . ?
C10B C40B C41B 109.8(2) . . ?
C41B C40B C42B 109.0(2) . . ?
C25B C26B C27B 121.4(2) . . ?
C12B C7B C6B 113.1(2) . . ?
C8B C7B C6B 128.5(2) . . ?
C8B C7B C12B 118.5(2) . . ?
C28A C27A C26A 121.0(2) . . ?
C17B C18B S2B 118.9(2) . . ?
C17B C18B C13B 120.5(3) . . ?
C13B C18B S2B 120.4(2) . . ?
C20A C21A C22A 120.8(3) . . ?
C16B C15B C14B 120.8(3) . . ?
C19A C24A S2A 119.72(19) . . ?
C23A C24A S2A 119.37(19) . . ?
C23A C24A C19A 120.6(2) . . ?
C15B C16B C17B 119.4(3) . . ?
C33B C34B C35B 119.6(2) . . ?
C22B C23B C24B 121.2(2) . . ?
C19B C20B C21B 121.0(2) . . ?
C17A C16A C15A 119.7(3) . . ?
C22B C21B C20B 120.1(3) . . ?
C16A C15A C14A 120.8(3) . . ?
C23A C22A C21A 118.9(2) . . ?
C16A C17A C18A 120.2(3) . . ?
C28B C29B C30B 121.1(2) . . ?
C28A C29A C30A 121.2(2) . . ?
C33A C34A C35A 119.9(2) . . ?
C23B C22B C21B 119.2(3) . . ?
C22A C23A C24A 121.0(2) . . ?
_shelx_SHELXL_version_number 2014/7
_iucr_refine_instructions_details
;
16srv065.res created by SHELXL-2014/7
TITL 16srv065 in P-1 #2
REM reset to P-1 #2
CELL 0.71073 12.9513 14.1812 18.9798 76.6319 83.7227 83.5306
ZERR 4 0.001 0.0011 0.0015 0.0027 0.0028 0.0027
LATT 1
SFAC C H N O S
UNIT 168 136 8 8 12
L.S. 7
PLAN 7
SIZE 0.058 0.067 0.319
TEMP -153.15
BOND
fmap 2
acta 50
OMIT -3 50
REM
REM
REM
WGHT 0.059000 1.677000
FVAR 0.09714 0.02754 0.04562 0.02245 0.03078 0.03969 0.02289
FVAR 0.07974 0.05119
S1A 5 -0.019191 0.541726 0.118486 11.00000 0.01370 0.01294 =
0.02155 -0.00361 -0.00557 0.00068
S1B 5 -0.005557 0.552369 0.614712 11.00000 0.01738 0.01294 =
0.02411 -0.00261 -0.00909 0.00011
S3A 5 0.345986 -0.038800 0.248084 11.00000 0.02753 0.01088 =
0.02417 -0.00287 -0.00271 0.00315
S3B 5 0.327850 -0.040472 0.763283 11.00000 0.03471 0.01237 =
0.02532 -0.00289 -0.00411 0.00356
S2B 5 0.561263 0.762769 0.729331 11.00000 0.02873 0.01884 =
0.04848 -0.00318 -0.01926 -0.00711
S2A 5 0.544458 0.756166 0.230807 11.00000 0.02634 0.01911 =
0.04855 -0.01037 -0.01686 -0.00305
O2B 4 -0.023504 0.585843 0.539562 11.00000 0.03927 0.02010 =
0.02849 -0.00037 -0.01928 -0.00095
O2A 4 -0.040208 0.581323 0.044380 11.00000 0.02686 0.02023 =
0.02478 -0.00146 -0.01272 0.00034
O1A 4 -0.103132 0.549879 0.173271 11.00000 0.01683 0.02427 =
0.03111 -0.00847 0.00100 -0.00094
N1A 3 0.371792 0.651167 0.200895 11.00000 0.01806 0.01583 =
0.02391 -0.00520 -0.00935 -0.00121
N2B 3 0.210857 0.158696 0.706501 11.00000 0.01652 0.01234 =
0.01895 -0.00114 -0.00232 0.00044
N2A 3 0.208484 0.150119 0.192012 11.00000 0.01444 0.01256 =
0.01678 -0.00194 -0.00409 0.00155
O1B 4 -0.090182 0.567417 0.667161 11.00000 0.01574 0.02299 =
0.03934 -0.00930 -0.00202 0.00217
N1B 3 0.385041 0.663620 0.695968 11.00000 0.01854 0.01787 =
0.02515 -0.00257 -0.00956 -0.00309
C12A 1 0.039153 0.420146 0.133311 11.00000 0.01501 0.01391 =
0.01565 -0.00302 -0.00172 0.00099
C1B 1 0.108455 0.597345 0.633508 11.00000 0.01541 0.01663 =
0.01620 -0.00260 -0.00346 -0.00231
C31B 1 0.294920 0.129405 0.659201 11.00000 0.01526 0.01597 =
0.02075 -0.00815 -0.00261 -0.00294
C30A 1 0.272975 0.036794 0.300417 11.00000 0.01428 0.01116 =
0.02220 -0.00218 -0.00230 -0.00362
C4B 1 0.290506 0.640710 0.672831 11.00000 0.01661 0.01598 =
0.01756 -0.00304 -0.00462 -0.00195
C25A 1 0.209817 0.119000 0.269049 11.00000 0.01335 0.01461 =
0.02039 -0.00141 -0.00407 -0.00381
C30B 1 0.265002 0.039945 0.815681 11.00000 0.01542 0.01378 =
0.02493 -0.00256 -0.00305 -0.00277
C2A 1 0.109159 0.682899 0.133712 11.00000 0.01616 0.01370 =
0.01698 -0.00301 -0.00386 0.00315
AFIX 43
H2A 2 0.056307 0.732913 0.117440 11.00000 -1.20000
AFIX 0
C3A 1 0.202705 0.706184 0.152237 11.00000 0.01801 0.01493 =
0.01468 -0.00424 -0.00112 -0.00095
C25B 1 0.211235 0.128209 0.783640 11.00000 0.01183 0.01464 =
0.02060 -0.00176 -0.00141 -0.00442
C6A 1 0.168129 0.510556 0.162480 11.00000 0.01823 0.01295 =
0.01580 -0.00098 -0.00310 -0.00039
C37B 1 0.243782 0.822337 0.630795 11.00000 0.02093 0.01576 =
0.02092 -0.00467 -0.00655 -0.00254
AFIX 13
H37B 2 0.278457 0.829111 0.673703 11.00000 -1.20000
AFIX 0
C2B 1 0.125397 0.693873 0.624530 11.00000 0.01734 0.01294 =
0.01732 -0.00286 -0.00362 0.00261
AFIX 43
H2B 2 0.073894 0.743722 0.605596 11.00000 -1.20000
AFIX 0
C5B 1 0.272410 0.543620 0.681552 11.00000 0.01876 0.01471 =
0.02037 0.00050 -0.00704 0.00172
AFIX 43
H5B 2 0.322310 0.493128 0.701951 11.00000 -1.20000
AFIX 0
C31A 1 0.296155 0.127538 0.144576 11.00000 0.01493 0.01340 =
0.01932 -0.00660 -0.00231 -0.00258
C33A 1 0.397603 0.162900 0.028163 11.00000 0.02650 0.02494 =
0.01737 -0.00694 -0.00039 -0.00653
AFIX 43
H33A 2 0.406723 0.201609 -0.019748 11.00000 -1.20000
AFIX 0
C9B 1 0.154771 0.251602 0.680277 11.00000 0.01827 0.01265 =
0.01339 -0.00150 -0.00049 0.00113
C11A 1 -0.001022 0.339576 0.121955 11.00000 0.01236 0.01750 =
0.01732 -0.00156 -0.00305 -0.00222
AFIX 43
H11A 2 -0.066966 0.346067 0.102938 11.00000 -1.20000
AFIX 0
C1A 1 0.093707 0.586780 0.139132 11.00000 0.01425 0.01853 =
0.01443 -0.00319 -0.00391 -0.00062
C40A 1 0.017382 0.157663 0.122935 11.00000 0.01652 0.01361 =
0.03070 -0.00453 -0.00506 0.00019
AFIX 13
H40A 2 0.080285 0.118062 0.106406 11.00000 -1.20000
AFIX 0
C13A 1 0.370026 0.657907 0.274497 11.00000 0.02430 0.01316 =
0.02790 -0.00471 -0.01362 0.00421
C32B 1 0.315273 0.185085 0.589168 11.00000 0.02076 0.01884 =
0.02287 -0.00522 -0.00156 -0.00210
AFIX 43
H32B 2 0.272918 0.243583 0.572602 11.00000 -1.20000
AFIX 0
C27B 1 0.156707 0.153744 0.904477 11.00000 0.02088 0.02801 =
0.02444 -0.00582 0.00302 -0.00135
AFIX 43
H27B 2 0.119095 0.193094 0.934664 11.00000 -1.20000
AFIX 0
C14B 1 0.299481 0.639934 0.820227 11.00000 0.02559 0.02377 =
0.03225 -0.00871 -0.01150 0.00168
AFIX 43
H14B 2 0.244769 0.610766 0.806187 11.00000 -1.20000
AFIX 0
C36B 1 0.357989 0.042908 0.681377 11.00000 0.02051 0.01595 =
0.02272 -0.00756 -0.00714 -0.00157
C10A 1 0.055161 0.248087 0.138390 11.00000 0.01665 0.01344 =
0.01671 -0.00134 -0.00062 -0.00074
C6B 1 0.180816 0.521401 0.660157 11.00000 0.01749 0.01356 =
0.01527 -0.00139 -0.00125 -0.00114
C3B 1 0.218546 0.717808 0.643413 11.00000 0.01936 0.01645 =
0.01416 -0.00471 -0.00163 -0.00114
C17B 1 0.459103 0.721252 0.863884 11.00000 0.03445 0.02056 =
0.04684 -0.01281 -0.02482 0.00402
AFIX 43
H17B 2 0.514737 0.748042 0.878965 11.00000 -1.20000
AFIX 0
C13B 1 0.381246 0.671391 0.769586 11.00000 0.02310 0.01377 =
0.02944 -0.00367 -0.01336 0.00212
C12B 1 0.049148 0.429717 0.636077 11.00000 0.01489 0.01419 =
0.01546 -0.00144 -0.00161 0.00136
C28A 1 0.213137 0.059694 0.420522 11.00000 0.02650 0.02860 =
0.01798 -0.00185 -0.00233 0.00044
AFIX 43
H28A 2 0.215082 0.040328 0.471772 11.00000 -1.20000
AFIX 0
C9A 1 0.150425 0.242846 0.168132 11.00000 0.01677 0.01177 =
0.01162 0.00033 0.00104 0.00114
C26A 1 0.146799 0.168787 0.315329 11.00000 0.01754 0.02135 =
0.02332 -0.00306 -0.00085 0.00282
AFIX 43
H26A 2 0.102025 0.224072 0.295388 11.00000 -1.20000
AFIX 0
C35B 1 0.442783 0.017254 0.636210 11.00000 0.01985 0.01856 =
0.03197 -0.01176 -0.00629 0.00256
AFIX 43
H35B 2 0.488175 -0.039089 0.652939 11.00000 -1.20000
AFIX 0
C11B 1 0.004472 0.347959 0.631618 11.00000 0.01646 0.01792 =
0.01787 -0.00322 -0.00477 -0.00295
AFIX 43
H11B 2 -0.062088 0.353995 0.613550 11.00000 -1.20000
AFIX 0
C8B 1 0.200167 0.334727 0.683722 11.00000 0.01329 0.01835 =
0.01799 -0.00257 -0.00326 -0.00073
AFIX 43
H8B 2 0.267067 0.329280 0.701191 11.00000 -1.20000
AFIX 0
C4A 1 0.276406 0.628942 0.178089 11.00000 0.01838 0.01744 =
0.01631 -0.00421 -0.00381 -0.00266
C36A 1 0.367272 0.046739 0.166099 11.00000 0.02024 0.01412 =
0.02098 -0.00822 -0.00422 -0.00437
C32A 1 0.311777 0.184977 0.074377 11.00000 0.02257 0.01839 =
0.01934 -0.00565 -0.00365 -0.00157
AFIX 43
H32A 2 0.263583 0.239332 0.058146 11.00000 -1.20000
AFIX 0
C19B 1 0.480928 0.646527 0.655284 11.00000 0.01817 0.01317 =
0.03180 0.00121 -0.00964 0.00026
C28B 1 0.210480 0.067316 0.935360 11.00000 0.02522 0.03255 =
0.01938 -0.00228 -0.00341 -0.00433
AFIX 43
H28B 2 0.210473 0.046772 0.986683 11.00000 -1.20000
AFIX 0
C18A 1 0.447730 0.703270 0.296240 11.00000 0.02819 0.01402 =
0.03792 -0.00877 -0.01790 0.00426
C7A 1 0.136991 0.414878 0.159455 11.00000 0.01644 0.01494 =
0.01370 -0.00304 -0.00298 -0.00118
C38A 1 0.304222 0.838923 0.076495 11.00000 0.02505 0.01557 =
0.02867 -0.00057 -0.00317 -0.00295
AFIX 137
H38A 2 0.369099 0.796339 0.083208 11.00000 21.00000
H38B 2 0.318918 0.906701 0.070791 11.00000 21.00000
H38C 2 0.274420 0.831703 0.032948 11.00000 21.00000
AFIX 0
C20A 1 0.477450 0.583782 0.104168 11.00000 0.02196 0.01941 =
0.03518 -0.00740 -0.00890 -0.00269
AFIX 43
H20A 2 0.417829 0.559289 0.092286 11.00000 -1.20000
AFIX 0
C33B 1 0.397443 0.155016 0.543662 11.00000 0.02221 0.02770 =
0.02292 -0.00936 0.00196 -0.00877
AFIX 43
H33B 2 0.409080 0.192145 0.495440 11.00000 -1.20000
AFIX 0
C10B 1 0.057266 0.256085 0.653731 11.00000 0.01677 0.01597 =
0.01582 -0.00218 -0.00194 -0.00162
C5A 1 0.259662 0.532121 0.184189 11.00000 0.01696 0.01482 =
0.02045 -0.00082 -0.00593 0.00202
AFIX 43
H5A 2 0.310404 0.481428 0.203018 11.00000 -1.20000
AFIX 0
C8A 1 0.192461 0.325192 0.176910 11.00000 0.01259 0.01610 =
0.01826 -0.00311 -0.00352 -0.00079
AFIX 43
H8A 2 0.259073 0.319476 0.194851 11.00000 -1.20000
AFIX 0
C19A 1 0.467699 0.634173 0.160100 11.00000 0.01864 0.01124 =
0.02970 -0.00007 -0.00942 0.00133
C37A 1 0.226612 0.810895 0.142830 11.00000 0.02019 0.01377 =
0.02200 -0.00396 -0.00705 -0.00217
AFIX 13
H37A 2 0.260515 0.815439 0.186659 11.00000 -1.20000
AFIX 0
C35A 1 0.454347 0.028024 0.120212 11.00000 0.01765 0.01516 =
0.03087 -0.01114 -0.00241 0.00015
AFIX 43
H35A 2 0.504294 -0.024885 0.136293 11.00000 -1.20000
AFIX 0
C41A 1 -0.056018 0.180095 0.062640 11.00000 0.03232 0.02457 =
0.03062 -0.01087 -0.00655 -0.00442
AFIX 137
H41A 2 -0.124492 0.206169 0.080816 11.00000 31.00000
H41B 2 -0.063336 0.120306 0.046803 11.00000 31.00000
H41C 2 -0.027491 0.228253 0.021472 11.00000 31.00000
AFIX 0
C14A 1 0.291804 0.620896 0.326472 11.00000 0.02977 0.02344 =
0.02852 -0.00713 -0.01376 0.00249
AFIX 43
H14A 2 0.239715 0.587541 0.313443 11.00000 -1.20000
AFIX 0
C24B 1 0.571003 0.682908 0.669398 11.00000 0.02263 0.01451 =
0.03568 0.00412 -0.01359 -0.00251
C40B 1 0.012887 0.165345 0.645541 11.00000 0.02386 0.01616 =
0.02717 -0.00123 -0.00923 -0.00261
AFIX 13
H40B 2 0.046761 0.108293 0.679333 11.00000 -1.20000
AFIX 0
C26B 1 0.157169 0.183721 0.829355 11.00000 0.01751 0.01731 =
0.02447 -0.00117 -0.00009 0.00047
AFIX 43
H26B 2 0.119631 0.243529 0.808905 11.00000 -1.20000
AFIX 0
C39B 1 0.147412 0.896064 0.622778 11.00000 0.02586 0.01578 =
0.03114 -0.00437 -0.00289 0.00032
AFIX 137
H39D 2 0.095443 0.877015 0.663762 11.00000 41.00000
H39E 2 0.117641 0.897503 0.577200 11.00000 41.00000
H39F 2 0.167519 0.960826 0.622244 11.00000 41.00000
AFIX 0
C7B 1 0.147356 0.424821 0.661624 11.00000 0.01476 0.01372 =
0.01523 -0.00140 -0.00104 -0.00033
C38B 1 0.320553 0.846601 0.563644 11.00000 0.02462 0.01663 =
0.02954 -0.00022 -0.00166 -0.00293
AFIX 137
H38D 2 0.289891 0.836871 0.521170 11.00000 51.00000
H38E 2 0.385254 0.803921 0.571050 11.00000 51.00000
H38F 2 0.335818 0.914596 0.555587 11.00000 51.00000
AFIX 0
C27A 1 0.148430 0.138927 0.389928 11.00000 0.02473 0.02863 =
0.02135 -0.00581 0.00204 0.00357
AFIX 43
H27A 2 0.104238 0.173608 0.420519 11.00000 -1.20000
AFIX 0
C18B 1 0.461846 0.712158 0.792465 11.00000 0.02901 0.01126 =
0.03872 -0.00507 -0.01959 0.00397
C21A 1 0.572649 0.569212 0.066032 11.00000 0.02409 0.02365 =
0.03874 -0.00917 -0.00586 0.00168
AFIX 43
H21A 2 0.577321 0.536831 0.027065 11.00000 -1.20000
AFIX 0
C15B 1 0.297210 0.650879 0.891396 11.00000 0.03052 0.03092 =
0.03307 -0.01053 -0.00955 0.00712
AFIX 43
H15B 2 0.240377 0.629894 0.925344 11.00000 -1.20000
AFIX 0
C24A 1 0.556728 0.672060 0.174072 11.00000 0.02192 0.01516 =
0.03507 -0.00087 -0.01337 0.00101
C16B 1 0.376286 0.691723 0.913157 11.00000 0.04727 0.02772 =
0.03519 -0.01522 -0.01953 0.01129
AFIX 43
H16B 2 0.373865 0.699520 0.961711 11.00000 -1.20000
AFIX 0
C42A 1 -0.033303 0.095005 0.191209 11.00000 0.03123 0.02892 =
0.03426 -0.00327 -0.00226 -0.01126
AFIX 137
H42A 2 0.015229 0.079359 0.229288 11.00000 61.00000
H42B 2 -0.050754 0.034673 0.180379 11.00000 61.00000
H42C 2 -0.097048 0.130604 0.207959 11.00000 61.00000
AFIX 0
C34B 1 0.461596 0.073452 0.566770 11.00000 0.01980 0.02602 =
0.03056 -0.01354 0.00014 -0.00295
AFIX 43
H34B 2 0.518931 0.055128 0.535506 11.00000 -1.20000
AFIX 0
C23B 1 0.665567 0.665073 0.631643 11.00000 0.01866 0.02313 =
0.04917 0.00362 -0.01258 -0.00010
AFIX 43
H23B 2 0.726471 0.686724 0.644182 11.00000 -1.20000
AFIX 0
C20B 1 0.489368 0.597737 0.598859 11.00000 0.02233 0.01860 =
0.03660 -0.00392 -0.00613 -0.00027
AFIX 43
H20B 2 0.429436 0.573027 0.587642 11.00000 -1.20000
AFIX 0
C16A 1 0.365428 0.678991 0.417596 11.00000 0.05344 0.03392 =
0.03155 -0.01665 -0.02319 0.01128
AFIX 43
H16A 2 0.362801 0.687245 0.466046 11.00000 -1.20000
AFIX 0
C21B 1 0.584289 0.584587 0.558604 11.00000 0.02744 0.02420 =
0.04209 -0.00433 -0.00519 0.00321
AFIX 43
H21B 2 0.588097 0.553598 0.518933 11.00000 -1.20000
AFIX 0
C15A 1 0.289589 0.632520 0.397258 11.00000 0.04043 0.02872 =
0.02704 -0.00620 -0.00895 0.00531
AFIX 43
H15A 2 0.235079 0.608111 0.432092 11.00000 -1.20000
AFIX 0
C39A 1 0.129933 0.884049 0.136340 11.00000 0.02501 0.01439 =
0.04325 -0.00878 -0.00427 0.00047
AFIX 137
H39A 2 0.102099 0.889551 0.089432 11.00000 71.00000
H39B 2 0.148946 0.947747 0.139657 11.00000 71.00000
H39C 2 0.076833 0.861704 0.175772 11.00000 71.00000
AFIX 0
C22A 1 0.661569 0.601243 0.083873 11.00000 0.01957 0.02737 =
0.04774 -0.00207 -0.00152 0.00141
AFIX 43
H22A 2 0.727569 0.588212 0.059105 11.00000 -1.20000
AFIX 0
C17A 1 0.445063 0.713434 0.367411 11.00000 0.03933 0.02589 =
0.04211 -0.01474 -0.02331 0.00365
AFIX 43
H17A 2 0.498381 0.744266 0.381530 11.00000 -1.20000
AFIX 0
C29B 1 0.264470 0.010891 0.890575 11.00000 0.01848 0.01895 =
0.02514 0.00145 -0.00495 -0.00177
AFIX 43
H29B 2 0.301824 -0.048793 0.911505 11.00000 -1.20000
AFIX 0
C29A 1 0.274982 0.009058 0.375406 11.00000 0.01870 0.01754 =
0.02462 0.00257 -0.00560 -0.00051
AFIX 43
H29A 2 0.319826 -0.045833 0.395942 11.00000 -1.20000
AFIX 0
C34A 1 0.468748 0.086266 0.050951 11.00000 0.02400 0.02350 =
0.02292 -0.01023 0.00163 -0.00619
AFIX 43
H34A 2 0.528024 0.072822 0.019452 11.00000 -1.20000
AFIX 0
C42B 1 -0.104337 0.166233 0.663538 11.00000 0.03172 0.03626 =
0.05123 -0.01541 0.00213 -0.01559
AFIX 137
H42D 2 -0.139835 0.209589 0.623623 11.00000 81.00000
H42E 2 -0.123668 0.189490 0.708379 11.00000 81.00000
H42F 2 -0.125159 0.100192 0.670225 11.00000 81.00000
AFIX 0
C22B 1 0.673294 0.616691 0.576367 11.00000 0.01927 0.02831 =
0.05291 0.00321 -0.00162 0.00440
AFIX 43
H22B 2 0.738834 0.605255 0.550501 11.00000 -1.20000
AFIX 0
C41B 1 0.039184 0.151409 0.568868 11.00000 0.04231 0.03254 =
0.03948 -0.01852 -0.00293 -0.00424
AFIX 137
H41D 2 0.115118 0.144431 0.558506 11.00000 91.00000
H41E 2 0.009457 0.208041 0.534567 11.00000 91.00000
H41F 2 0.010037 0.092716 0.563793 11.00000 91.00000
AFIX 0
C23A 1 0.652623 0.652194 0.138026 11.00000 0.01854 0.02159 =
0.04643 -0.00164 -0.01212 -0.00091
AFIX 43
H23A 2 0.713171 0.674080 0.150883 11.00000 -1.20000
AFIX 0
HKLF 4
REM 16srv065 in P-1 #2
REM R1 = 0.0433 for 8686 Fo > 4sig(Fo) and 0.0694 for all 11804 data
REM 899 parameters refined using 0 restraints
END
WGHT 0.0531 1.9773
REM Highest difference peak 0.442, deepest hole -0.397, 1-sigma level 0.056
Q1 1 -0.0443 0.1838 0.5579 11.00000 0.05 0.44
Q2 1 0.3526 0.0029 0.2002 11.00000 0.05 0.40
Q3 1 0.3388 -0.0042 0.7102 11.00000 0.05 0.37
Q4 1 -0.0263 0.1004 0.6934 11.00000 0.05 0.32
Q5 1 0.5257 0.7206 0.7709 11.00000 0.05 0.29
Q6 1 0.2568 0.6204 0.9733 11.00000 0.05 0.28
Q7 1 -0.1149 0.1615 0.1710 11.00000 0.05 0.28
REM The information below was added by Olex2.
REM
REM R1 = 0.0433 for 8686 Fo > 4sig(Fo) and 0.0694 for all 75334 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.44, deepest hole -0.40
REM Mean Shift 0, Max Shift -0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0694
REM R1_gt = 0.0433
REM wR_ref = 0.1207
REM GOOF = 1.028
REM Shift_max = -0.001
REM Shift_mean = 0
REM Reflections_all = 75334
REM Reflections_gt = 8686
REM Parameters = n/a
REM Hole = -0.40
REM Peak = 0.44
REM Flack = n/a
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
#===END
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/hexane'
_exptl_crystal_preparation Luminescent