# 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_DAcDBT_17s183 _database_code_depnum_ccdc_archive 'CCDC 1901568' loop_ _audit_author_name _audit_author_address 'Andrei S. Batsanov' ;Durham University United Kingdom ; _audit_update_record ; 2019-03-06 deposited with the CCDC. 2019-10-14 downloaded from the CCDC. ; _audit_creation_date 2017-07-21 _audit_creation_method ; Olex2 1.2-beta (compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370) ; _shelx_SHELXL_version_number 2016/6 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C42 H34 N2 S, C Cl2 D2' _chemical_formula_sum 'C43 H34 Cl2 D2 N2 S' _chemical_formula_weight 685.71 _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' Cl Cl 0.1484 0.1585 '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 0.0061 0.0033 '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 monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 24.0937(12) _cell_length_b 7.9916(4) _cell_length_c 36.7515(18) _cell_angle_alpha 90 _cell_angle_beta 99.3094(16) _cell_angle_gamma 90 _cell_volume 6983.2(6) _cell_formula_units_Z 8 _cell_measurement_reflns_used 9901 _cell_measurement_temperature 120 _cell_measurement_theta_max 30.12 _cell_measurement_theta_min 2.54 _shelx_estimated_absorpt_T_max 0.983 _shelx_estimated_absorpt_T_min 0.872 _exptl_absorpt_coefficient_mu 0.280 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.9651 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Krause et al., 2015) was used for absorption correction. wR2(int) was 0.1508 before and 0.0549 after correction. The Ratio of minimum to maximum transmission is 0.9651. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description lathe _exptl_crystal_F_000 2864 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 -1.00 0.00 0.2050 0.00 1.00 1.00 0.2390 0.00 0.00 -1.00 0.0310 0.00 0.00 1.00 0.0240 -1.00 0.00 0.00 0.1320 1.00 0.00 0.00 0.0410 _exptl_crystal_size_max 0.503 _exptl_crystal_size_mid 0.275 _exptl_crystal_size_min 0.062 _exptl_special_details ; Phase transition with modulation (doubling of a) on coolong below ca 170 K. This is the low-temperature phase. Data were collected in shutterless mode. Full sphere of reciprocal space was nominally covered by 2 runs of 340 narrow-frame \w-scans (scan width 0.5\%, 20s exposure) and 2 runs of 340 & 215 scans (scan width 0.5\%, 10s exposure) , every run at a different \f angle. Two runs of 358 \f-scans (scan width 1\%, 1.5s exposure) were used for scaling overflowing intensities. Crystal to detector distance 4.48 cm. ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0643 _diffrn_reflns_av_unetI/netI 0.0419 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_number 88992 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.681 _diffrn_reflns_theta_min 2.010 _diffrn_ambient_temperature 120 _diffrn_detector_area_resol_mean 10.4 _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 '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 9504 _reflns_number_total 13247 _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 v8.37A (Bruker, 2016)' _computing_data_collection 'APEX3 v.2016.1-0 (Bruker, 2016)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL 2016/6 multi-CPU (Sheldrick, 2015)' _computing_structure_solution 'ShelXS 2013/1 (Sheldrick, 2008)' _refine_diff_density_max 0.344 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.052 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 903 _refine_ls_number_reflns 13247 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0467 _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^)+(0.0480P)^2^+4.6830P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1024 _refine_ls_wR_factor_ref 0.1140 _refine_special_details ; 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. Atoms Cl(1') and Cl(2') are disordered between two positions, with occupancies 0.85 and 0.15. Minor positions are labelled Cl(1") and Cl(2"). Atom Cl(1) is disordered between two positions with occupancies 0.9 and 0.1, minor position is labelled Cl(1A). ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups 2. Rigid body (RIGU) restrains C43', Cl1', Cl2', Cl1", Cl2" with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 3. Others Uiso(H39A)=Uiso(H39B)=Uiso(H39C)=FVAR(1) Uiso(H40A)=Uiso(H40B)=Uiso(H40C)=FVAR(2) Uiso(H41A)=Uiso(H41B)=Uiso(H41C)=FVAR(3) Uiso(H42A)=Uiso(H42B)=Uiso(H42C)=FVAR(4) Uiso(H39D)=Uiso(H39E)=Uiso(H39F)=FVAR(5) Uiso(H40D)=Uiso(H40E)=Uiso(H40F)=FVAR(6) Uiso(H41D)=Uiso(H41E)=Uiso(H41F)=FVAR(7) Uiso(H42D)=Uiso(H42E)=Uiso(H42F)=FVAR(8) Fixed Sof: D43A(0.85) D43B(0.85) D43C(0.15) D43D(0.15) Cl1'(0.85) Cl2'(0.85) Cl1"(0.15) Cl2"(0.15) Cl1(0.94) Cl1A(0.06) 4.a Secondary CH2 refined with riding coordinates: C43'(D43A,D43B), C43'(D43C,D43D), C43(D43E,D43F) 4.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C5(H5), C8(H8), C10(H10), C11(H11), C14(H14), C15(H15), C16(H16), C17(H17), C21(H21), C22(H22), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30), C34(H34), C35(H35), C36(H36), C37(H37), C2'(H2'), C3'(H3'), C5'(H5'), C8'(H8'), C10'(H10'), C11'(H11'), C14'(H14'), C15'(H15'), C16'(H16'), C17'(H17'), C21'(H21'), C22'(H22'), C23'(H23'), C24'(H24'), C27'(H27'), C28'(H28'), C29'(H29'), C30'(H30'), C34'(H34'), C35'(H35'), C36'(H36'), C37'(H37') 4.c Idealised Me refined as rotating group: C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B, H42C), C39'(H39D,H39E,H39F), C40'(H40D,H40E,H40F), C41'(H41D,H41E,H41F), C42'(H42D,H42E,H42F) ; _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 0.46554(2) -0.15900(7) 0.57260(2) 0.02077(13) Uani 1 1 d . . . . . N1 N 0.34907(7) 0.3334(2) 0.46575(4) 0.0171(4) Uani 1 1 d . . . . . N2 N 0.41316(7) 0.3647(2) 0.67636(4) 0.0160(4) Uani 1 1 d . . . . . C1 C 0.43218(8) -0.0275(3) 0.53774(6) 0.0172(5) Uani 1 1 d . . . . . C2 C 0.42588(9) -0.0564(3) 0.49982(6) 0.0216(5) Uani 1 1 d . . . . . H2 H 0.440012 -0.155676 0.490450 0.026 Uiso 1 1 calc R . . . . C3 C 0.39859(9) 0.0631(3) 0.47627(6) 0.0223(5) Uani 1 1 d . . . . . H3 H 0.394287 0.046423 0.450377 0.027 Uiso 1 1 calc R . . . . C4 C 0.37718(8) 0.2087(3) 0.49014(6) 0.0172(5) Uani 1 1 d . . . . . C5 C 0.38350(8) 0.2370(3) 0.52754(5) 0.0152(4) Uani 1 1 d . . . . . H5 H 0.368897 0.335951 0.536750 0.018 Uiso 1 1 calc R . . . . C6 C 0.41154(8) 0.1190(3) 0.55175(5) 0.0150(4) Uani 1 1 d . . . . . C7 C 0.42339(8) 0.1242(2) 0.59164(5) 0.0140(4) Uani 1 1 d . . . . . C8 C 0.41105(8) 0.2513(3) 0.61510(5) 0.0147(4) Uani 1 1 d . . . . . H8 H 0.392339 0.349878 0.605258 0.018 Uiso 1 1 calc R . . . . C9 C 0.42618(8) 0.2327(3) 0.65264(5) 0.0152(4) Uani 1 1 d . . . . . C10 C 0.45419(8) 0.0881(3) 0.66740(6) 0.0184(5) Uani 1 1 d . . . . . H10 H 0.464330 0.077330 0.693372 0.022 Uiso 1 1 calc R . . . . C11 C 0.46721(8) -0.0386(3) 0.64474(6) 0.0192(5) Uani 1 1 d . . . . . H11 H 0.486187 -0.136552 0.654762 0.023 Uiso 1 1 calc R . . . . C12 C 0.45179(8) -0.0194(3) 0.60674(6) 0.0162(4) Uani 1 1 d . . . . . C13 C 0.38186(8) 0.4550(3) 0.45138(5) 0.0164(4) Uani 1 1 d . . . . . C14 C 0.44046(8) 0.4489(3) 0.45837(6) 0.0210(5) Uani 1 1 d . . . . . H14 H 0.459057 0.365793 0.474381 0.025 Uiso 1 1 calc R . . . . C15 C 0.47155(9) 0.5642(3) 0.44193(6) 0.0252(5) Uani 1 1 d . . . . . H15 H 0.511463 0.560130 0.446944 0.030 Uiso 1 1 calc R . . . . C16 C 0.44518(9) 0.6847(3) 0.41838(6) 0.0267(5) Uani 1 1 d . . . . . H16 H 0.466579 0.760606 0.406357 0.032 Uiso 1 1 calc R . . . . C17 C 0.38699(9) 0.6932(3) 0.41254(6) 0.0249(5) Uani 1 1 d . . . . . H17 H 0.368735 0.776675 0.396473 0.030 Uiso 1 1 calc R . . . . C18 C 0.35468(8) 0.5835(3) 0.42947(5) 0.0186(5) Uani 1 1 d . . . . . C19 C 0.29138(8) 0.6030(3) 0.42803(6) 0.0213(5) Uani 1 1 d . . . . . C20 C 0.26568(8) 0.4292(3) 0.42535(6) 0.0203(5) Uani 1 1 d . . . . . C21 C 0.21364(9) 0.3919(3) 0.40443(6) 0.0292(6) Uani 1 1 d . . . . . H21 H 0.195246 0.474042 0.388067 0.035 Uiso 1 1 calc R . . . . C22 C 0.18809(10) 0.2384(3) 0.40688(7) 0.0359(6) Uani 1 1 d . . . . . H22 H 0.152724 0.215077 0.392226 0.043 Uiso 1 1 calc R . . . . C23 C 0.21445(10) 0.1198(3) 0.43076(7) 0.0340(6) Uani 1 1 d . . . . . H23 H 0.196218 0.016305 0.433531 0.041 Uiso 1 1 calc R . . . . C24 C 0.26733(9) 0.1498(3) 0.45083(6) 0.0252(5) Uani 1 1 d . . . . . H24 H 0.285467 0.066462 0.466974 0.030 Uiso 1 1 calc R . . . . C25 C 0.29379(8) 0.3025(3) 0.44726(6) 0.0185(5) Uani 1 1 d . . . . . C26 C 0.45743(8) 0.4723(3) 0.69138(5) 0.0163(4) Uani 1 1 d . . . . . C27 C 0.50965(9) 0.4608(3) 0.67957(6) 0.0204(5) Uani 1 1 d . . . . . H27 H 0.514668 0.385130 0.660433 0.024 Uiso 1 1 calc R . . . . C28 C 0.55405(9) 0.5598(3) 0.69579(6) 0.0249(5) Uani 1 1 d . . . . . H28 H 0.589538 0.551254 0.687828 0.030 Uiso 1 1 calc R . . . . C29 C 0.54701(9) 0.6709(3) 0.72349(6) 0.0256(5) Uani 1 1 d . . . . . H29 H 0.577830 0.735580 0.735294 0.031 Uiso 1 1 calc R . . . . C30 C 0.49452(9) 0.6868(3) 0.73383(6) 0.0224(5) Uani 1 1 d . . . . . H30 H 0.489559 0.765975 0.752319 0.027 Uiso 1 1 calc R . . . . C31 C 0.44875(9) 0.5906(3) 0.71799(5) 0.0180(5) Uani 1 1 d . . . . . C32 C 0.38922(9) 0.6199(3) 0.72599(6) 0.0228(5) Uani 1 1 d . . . . . C33 C 0.35774(8) 0.4543(3) 0.72266(5) 0.0168(5) Uani 1 1 d . . . . . C34 C 0.31526(9) 0.4186(3) 0.74291(6) 0.0228(5) Uani 1 1 d . . . . . H34 H 0.308585 0.494414 0.761644 0.027 Uiso 1 1 calc R . . . . C35 C 0.28242(10) 0.2768(3) 0.73673(7) 0.0293(6) Uani 1 1 d . . . . . H35 H 0.254053 0.254686 0.751278 0.035 Uiso 1 1 calc R . . . . C36 C 0.29124(9) 0.1672(3) 0.70915(6) 0.0275(5) Uani 1 1 d . . . . . H36 H 0.267959 0.071307 0.704082 0.033 Uiso 1 1 calc R . . . . C37 C 0.33385(8) 0.1967(3) 0.68894(6) 0.0193(5) Uani 1 1 d . . . . . H37 H 0.339953 0.120694 0.670115 0.023 Uiso 1 1 calc R . . . . C38 C 0.36788(8) 0.3375(3) 0.69605(5) 0.0146(4) Uani 1 1 d . . . . . C39 C 0.28199(9) 0.6782(3) 0.46541(6) 0.0247(5) Uani 1 1 d . . . . . H39A H 0.241634 0.694368 0.465268 0.030(4) Uiso 1 1 calc GR . . . . H39B H 0.301337 0.786174 0.469207 0.030(4) Uiso 1 1 calc GR . . . . H39C H 0.297057 0.601597 0.485413 0.030(4) Uiso 1 1 calc GR . . . . C40 C 0.26514(10) 0.7183(3) 0.39705(7) 0.0328(6) Uani 1 1 d . . . . . H40A H 0.271229 0.671991 0.373322 0.040(4) Uiso 1 1 calc GR . . . . H40B H 0.282610 0.829151 0.400491 0.040(4) Uiso 1 1 calc GR . . . . H40C H 0.224681 0.728142 0.397371 0.040(4) Uiso 1 1 calc GR . . . . C41 C 0.35904(10) 0.7359(3) 0.69548(8) 0.0353(6) Uani 1 1 d . . . . . H41A H 0.359875 0.685059 0.671306 0.046(4) Uiso 1 1 calc GR . . . . H41B H 0.378176 0.844481 0.696789 0.046(4) Uiso 1 1 calc GR . . . . H41C H 0.319911 0.751858 0.698953 0.046(4) Uiso 1 1 calc GR . . . . C42 C 0.38958(11) 0.7031(4) 0.76356(7) 0.0431(7) Uani 1 1 d . . . . . H42A H 0.350803 0.719996 0.767704 0.045(4) Uiso 1 1 calc GR . . . . H42B H 0.408728 0.811445 0.764032 0.045(4) Uiso 1 1 calc GR . . . . H42C H 0.409449 0.631038 0.783002 0.045(4) Uiso 1 1 calc GR . . . . S1' S 0.96256(2) -0.15123(7) 0.56762(2) 0.02072(13) Uani 1 1 d . . . . . N1' N 0.84746(7) 0.3682(2) 0.46736(5) 0.0162(4) Uani 1 1 d . . . . . N2' N 0.91435(7) 0.3432(2) 0.67881(5) 0.0180(4) Uani 1 1 d . . . . . C1' C 0.93009(8) -0.0098(3) 0.53469(6) 0.0170(5) Uani 1 1 d . . . . . C2' C 0.92361(9) -0.0284(3) 0.49635(6) 0.0205(5) Uani 1 1 d . . . . . H2' H 0.937339 -0.125097 0.485660 0.025 Uiso 1 1 calc R . . . . C3' C 0.89683(9) 0.0971(3) 0.47454(6) 0.0205(5) Uani 1 1 d . . . . . H3' H 0.892370 0.087192 0.448466 0.025 Uiso 1 1 calc R . . . . C4' C 0.87608(8) 0.2389(3) 0.49019(6) 0.0165(4) Uani 1 1 d . . . . . C5' C 0.88281(8) 0.2580(3) 0.52798(5) 0.0155(4) Uani 1 1 d . . . . . H5' H 0.868958 0.355080 0.538440 0.019 Uiso 1 1 calc R . . . . C6' C 0.91028(8) 0.1328(3) 0.55070(5) 0.0146(4) Uani 1 1 d . . . . . C7' C 0.92198(8) 0.1276(2) 0.59056(5) 0.0146(4) Uani 1 1 d . . . . . C8' C 0.91043(8) 0.2474(3) 0.61586(5) 0.0156(4) Uani 1 1 d . . . . . H8' H 0.891657 0.348175 0.607507 0.019 Uiso 1 1 calc R . . . . C9' C 0.92640(8) 0.2189(3) 0.65305(6) 0.0169(4) Uani 1 1 d . . . . . C10' C 0.95373(9) 0.0707(3) 0.66566(6) 0.0208(5) Uani 1 1 d . . . . . H10' H 0.964163 0.052579 0.691407 0.025 Uiso 1 1 calc R . . . . C11' C 0.96576(9) -0.0499(3) 0.64114(6) 0.0194(5) Uani 1 1 d . . . . . H11' H 0.984333 -0.150752 0.649694 0.023 Uiso 1 1 calc R . . . . C12' C 0.94992(8) -0.0198(3) 0.60350(6) 0.0165(4) Uani 1 1 d . . . . . C13' C 0.87976(8) 0.4856(3) 0.45114(5) 0.0165(4) Uani 1 1 d . . . . . C14' C 0.93832(8) 0.4741(3) 0.45574(6) 0.0205(5) Uani 1 1 d . . . . . H14' H 0.957339 0.390557 0.471437 0.025 Uiso 1 1 calc R . . . . C15' C 0.96870(9) 0.5839(3) 0.43753(6) 0.0259(5) Uani 1 1 d . . . . . H15' H 1.008535 0.575635 0.440856 0.031 Uiso 1 1 calc R . . . . C16' C 0.94153(9) 0.7053(3) 0.41456(6) 0.0255(5) Uani 1 1 d . . . . . H16' H 0.962337 0.777831 0.401328 0.031 Uiso 1 1 calc R . . . . C17' C 0.88360(9) 0.7204(3) 0.41098(6) 0.0218(5) Uani 1 1 d . . . . . H17' H 0.864990 0.804907 0.395378 0.026 Uiso 1 1 calc R . . . . C18' C 0.85215(8) 0.6148(3) 0.42971(5) 0.0166(4) Uani 1 1 d . . . . . C19' C 0.78943(8) 0.6389(3) 0.43026(6) 0.0200(5) Uani 1 1 d . . . . . C20' C 0.76281(8) 0.4663(3) 0.42862(6) 0.0180(5) Uani 1 1 d . . . . . C21' C 0.70986(9) 0.4294(3) 0.40872(6) 0.0253(5) Uani 1 1 d . . . . . H21' H 0.691137 0.510765 0.392290 0.030 Uiso 1 1 calc R . . . . C22' C 0.68407(9) 0.2775(3) 0.41237(7) 0.0302(6) Uani 1 1 d . . . . . H22' H 0.648048 0.254798 0.398512 0.036 Uiso 1 1 calc R . . . . C23' C 0.71074(9) 0.1591(3) 0.43614(7) 0.0286(6) Uani 1 1 d . . . . . H23' H 0.692279 0.056666 0.439643 0.034 Uiso 1 1 calc R . . . . C24' C 0.76437(9) 0.1885(3) 0.45499(6) 0.0212(5) Uani 1 1 d . . . . . H24' H 0.782894 0.105434 0.471036 0.025 Uiso 1 1 calc R . . . . C25' C 0.79124(8) 0.3395(3) 0.45048(5) 0.0158(4) Uani 1 1 d . . . . . C26' C 0.95441(8) 0.4676(3) 0.69045(5) 0.0163(4) Uani 1 1 d . . . . . C27' C 1.00634(9) 0.4642(3) 0.67783(6) 0.0205(5) Uani 1 1 d . . . . . H27' H 1.013129 0.381965 0.660413 0.025 Uiso 1 1 calc R . . . . C28' C 1.04756(9) 0.5793(3) 0.69048(6) 0.0232(5) Uani 1 1 d . . . . . H28' H 1.082649 0.575333 0.681864 0.028 Uiso 1 1 calc R . . . . C29' C 1.03814(9) 0.7004(3) 0.71565(6) 0.0251(5) Uani 1 1 d . . . . . H29' H 1.066754 0.778539 0.724775 0.030 Uiso 1 1 calc R . . . . C30' C 0.98641(9) 0.7061(3) 0.72734(6) 0.0217(5) Uani 1 1 d . . . . . H30' H 0.979818 0.790614 0.744313 0.026 Uiso 1 1 calc R . . . . C31' C 0.94363(8) 0.5923(3) 0.71512(5) 0.0172(4) Uani 1 1 d . . . . . C32' C 0.88652(9) 0.6115(3) 0.72767(5) 0.0176(5) Uani 1 1 d . . . . . C33' C 0.84820(9) 0.4628(3) 0.71521(5) 0.0172(5) Uani 1 1 d . . . . . C34' C 0.79547(9) 0.4529(3) 0.72601(6) 0.0246(5) Uani 1 1 d . . . . . H34' H 0.784018 0.540407 0.740636 0.030 Uiso 1 1 calc R . . . . C35' C 0.75929(10) 0.3209(3) 0.71628(6) 0.0295(6) Uani 1 1 d . . . . . H35' H 0.723336 0.319010 0.723743 0.035 Uiso 1 1 calc R . . . . C36' C 0.77579(9) 0.1916(3) 0.69562(6) 0.0247(5) Uani 1 1 d . . . . . H36' H 0.751954 0.097442 0.689721 0.030 Uiso 1 1 calc R . . . . C37' C 0.82723(9) 0.1993(3) 0.68348(6) 0.0197(5) Uani 1 1 d . . . . . H37' H 0.838251 0.110949 0.668902 0.024 Uiso 1 1 calc R . . . . C38' C 0.86310(8) 0.3358(3) 0.69246(5) 0.0157(4) Uani 1 1 d . . . . . C39' C 0.78313(9) 0.7163(3) 0.46814(6) 0.0237(5) Uani 1 1 d . . . . . H39D H 0.743186 0.733947 0.469245 0.032(4) Uiso 1 1 calc GR . . . . H39E H 0.802954 0.823748 0.471146 0.032(4) Uiso 1 1 calc GR . . . . H39F H 0.799280 0.640083 0.487945 0.032(4) Uiso 1 1 calc GR . . . . C40' C 0.76168(9) 0.7552(3) 0.39987(7) 0.0290(6) Uani 1 1 d . . . . . H40D H 0.765902 0.708676 0.375794 0.035(4) Uiso 1 1 calc GR . . . . H40E H 0.779651 0.865457 0.402840 0.035(4) Uiso 1 1 calc GR . . . . H40F H 0.721615 0.766371 0.401393 0.035(4) Uiso 1 1 calc GR . . . . C41' C 0.85874(9) 0.7734(3) 0.71068(6) 0.0257(5) Uani 1 1 d . . . . . H41D H 0.853731 0.766008 0.683731 0.026(4) Uiso 1 1 calc GR . . . . H41E H 0.882806 0.869274 0.719034 0.026(4) Uiso 1 1 calc GR . . . . H41F H 0.822013 0.787718 0.718483 0.026(4) Uiso 1 1 calc GR . . . . C42' C 0.89458(10) 0.6248(3) 0.77023(6) 0.0247(5) Uani 1 1 d . . . . . H42D H 0.857735 0.631962 0.778167 0.033(4) Uiso 1 1 calc GR . . . . H42E H 0.916541 0.725177 0.778247 0.033(4) Uiso 1 1 calc GR . . . . H42F H 0.914563 0.525541 0.781201 0.033(4) Uiso 1 1 calc GR . . . . C43' C 0.66928(13) 0.7547(4) 0.64158(8) 0.0562(8) Uani 1 1 d . U . . . D43A D 0.699866 0.797998 0.629147 0.067 Uiso 0.85 1 calc R . P A 1 D43B D 0.662859 0.636018 0.634426 0.067 Uiso 0.85 1 calc R . P A 1 D43C D 0.649014 0.662515 0.627118 0.067 Uiso 0.15 1 calc R . P B 2 D43D D 0.696447 0.799729 0.626539 0.067 Uiso 0.15 1 calc R . P B 2 Cl1' Cl 0.60968(5) 0.8657(2) 0.62727(3) 0.0689(4) Uani 0.85 1 d . U P C 1 Cl2' Cl 0.69043(3) 0.76808(11) 0.69051(2) 0.0407(2) Uani 0.85 1 d . U P C 1 Cl1" Cl 0.6152(3) 0.9276(7) 0.64419(18) 0.0502(18) Uani 0.15 1 d . U P C 2 Cl2" Cl 0.7001(2) 0.6836(9) 0.67164(15) 0.0586(15) Uani 0.15 1 d . U P C 2 Cl1 Cl 0.14141(5) 0.90021(10) 0.65307(2) 0.0627(3) Uani 0.94 1 d . . P D 1 Cl2 Cl 0.20242(3) 0.58794(10) 0.67016(2) 0.0496(2) Uani 1 1 d . . . . . C43 C 0.17179(17) 0.7259(4) 0.63585(9) 0.0717(11) Uani 1 1 d . . . . . D43E D 0.200910 0.763889 0.621540 0.086 Uiso 1 1 calc R . . D 1 D43F D 0.142587 0.665469 0.618755 0.086 Uiso 1 1 calc R . . D 1 Cl1A Cl 0.1226(6) 0.846(2) 0.6306(5) 0.066(4) Uiso 0.06 1 d . . P D 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 0.0254(3) 0.0167(3) 0.0213(3) -0.0012(2) 0.0070(2) 0.0058(2) N1 0.0139(9) 0.0199(10) 0.0169(9) 0.0011(7) 0.0013(7) -0.0023(7) N2 0.0161(9) 0.0166(10) 0.0160(9) -0.0034(7) 0.0045(7) -0.0024(7) C1 0.0142(10) 0.0163(11) 0.0219(11) -0.0004(9) 0.0057(9) -0.0008(9) C2 0.0265(12) 0.0171(12) 0.0231(12) -0.0037(9) 0.0097(10) 0.0015(9) C3 0.0264(12) 0.0252(13) 0.0157(11) -0.0037(9) 0.0049(9) -0.0016(10) C4 0.0147(10) 0.0184(12) 0.0187(11) 0.0003(9) 0.0029(9) -0.0026(9) C5 0.0130(10) 0.0144(11) 0.0191(11) -0.0035(9) 0.0054(8) -0.0026(8) C6 0.0122(10) 0.0158(11) 0.0177(11) -0.0006(9) 0.0047(8) -0.0034(8) C7 0.0109(10) 0.0140(11) 0.0178(11) 0.0010(8) 0.0040(8) -0.0016(8) C8 0.0101(10) 0.0146(11) 0.0195(11) 0.0001(9) 0.0029(8) -0.0011(8) C9 0.0115(10) 0.0159(11) 0.0185(11) -0.0016(9) 0.0036(8) -0.0034(8) C10 0.0186(11) 0.0217(12) 0.0147(11) 0.0011(9) 0.0021(9) -0.0012(9) C11 0.0187(11) 0.0178(12) 0.0218(11) 0.0039(9) 0.0051(9) 0.0018(9) C12 0.0147(10) 0.0136(11) 0.0215(11) -0.0007(9) 0.0065(9) -0.0006(8) C13 0.0173(11) 0.0168(11) 0.0159(10) -0.0057(9) 0.0049(9) -0.0016(9) C14 0.0164(11) 0.0207(12) 0.0258(12) -0.0057(10) 0.0027(9) 0.0007(9) C15 0.0171(11) 0.0237(13) 0.0366(14) -0.0089(11) 0.0097(10) -0.0047(10) C16 0.0265(12) 0.0229(13) 0.0343(13) -0.0048(11) 0.0154(11) -0.0067(10) C17 0.0297(13) 0.0239(13) 0.0226(12) -0.0013(10) 0.0091(10) 0.0005(10) C18 0.0197(11) 0.0218(12) 0.0149(11) -0.0028(9) 0.0044(9) 0.0007(9) C19 0.0164(11) 0.0252(13) 0.0222(12) 0.0003(10) 0.0025(9) 0.0029(9) C20 0.0150(11) 0.0286(13) 0.0178(11) -0.0031(9) 0.0043(9) 0.0012(9) C21 0.0169(12) 0.0387(15) 0.0311(13) -0.0061(11) 0.0010(10) 0.0026(11) C22 0.0152(12) 0.0480(18) 0.0429(16) -0.0146(13) 0.0003(11) -0.0050(12) C23 0.0231(13) 0.0333(15) 0.0470(16) -0.0111(12) 0.0100(12) -0.0113(11) C24 0.0208(12) 0.0249(13) 0.0315(13) -0.0033(10) 0.0086(10) -0.0039(10) C25 0.0143(10) 0.0249(12) 0.0174(11) -0.0059(9) 0.0062(9) -0.0013(9) C26 0.0163(11) 0.0160(11) 0.0158(10) 0.0032(9) -0.0001(9) -0.0028(9) C27 0.0216(11) 0.0195(12) 0.0204(11) 0.0000(9) 0.0044(9) -0.0023(9) C28 0.0165(11) 0.0270(13) 0.0312(13) 0.0048(11) 0.0037(10) -0.0040(10) C29 0.0227(12) 0.0235(13) 0.0269(12) 0.0045(10) -0.0071(10) -0.0103(10) C30 0.0280(12) 0.0194(12) 0.0177(11) -0.0009(9) -0.0029(9) -0.0035(10) C31 0.0216(11) 0.0170(11) 0.0144(10) 0.0024(9) 0.0000(9) 0.0005(9) C32 0.0243(12) 0.0188(12) 0.0248(12) -0.0064(9) 0.0023(10) 0.0008(9) C33 0.0172(11) 0.0174(11) 0.0145(10) 0.0032(9) -0.0010(9) 0.0043(9) C34 0.0225(12) 0.0271(13) 0.0205(11) 0.0016(10) 0.0086(9) 0.0081(10) C35 0.0269(12) 0.0297(14) 0.0354(14) 0.0035(11) 0.0175(11) -0.0007(11) C36 0.0254(12) 0.0213(13) 0.0378(14) 0.0006(11) 0.0111(11) -0.0051(10) C37 0.0197(11) 0.0166(12) 0.0227(11) -0.0014(9) 0.0066(9) 0.0000(9) C38 0.0137(10) 0.0161(11) 0.0139(10) 0.0024(8) 0.0015(8) 0.0028(8) C39 0.0220(12) 0.0221(13) 0.0317(13) -0.0018(10) 0.0091(10) 0.0025(10) C40 0.0254(13) 0.0374(15) 0.0347(14) 0.0079(12) 0.0020(11) 0.0088(11) C41 0.0257(13) 0.0181(13) 0.0617(18) 0.0089(12) 0.0060(12) 0.0016(10) C42 0.0344(15) 0.0498(18) 0.0485(17) -0.0309(14) 0.0167(13) -0.0138(13) S1' 0.0265(3) 0.0156(3) 0.0207(3) 0.0004(2) 0.0057(2) 0.0066(2) N1' 0.0128(9) 0.0164(10) 0.0189(9) 0.0017(7) 0.0008(7) -0.0014(7) N2' 0.0159(9) 0.0186(10) 0.0197(9) -0.0053(8) 0.0038(7) -0.0016(7) C1' 0.0152(11) 0.0144(11) 0.0214(11) 0.0004(9) 0.0030(9) -0.0015(9) C2' 0.0234(12) 0.0176(12) 0.0212(11) -0.0035(9) 0.0061(9) 0.0025(9) C3' 0.0217(11) 0.0236(12) 0.0166(11) -0.0009(9) 0.0042(9) -0.0004(10) C4' 0.0128(10) 0.0156(11) 0.0209(11) 0.0026(9) 0.0021(8) -0.0013(8) C5' 0.0110(10) 0.0143(11) 0.0217(11) -0.0032(9) 0.0040(8) -0.0017(8) C6' 0.0105(10) 0.0149(11) 0.0192(11) 0.0002(9) 0.0050(8) -0.0029(8) C7' 0.0099(10) 0.0138(11) 0.0203(11) 0.0016(8) 0.0033(8) -0.0008(8) C8' 0.0126(10) 0.0138(11) 0.0206(11) -0.0009(9) 0.0034(8) 0.0002(8) C9' 0.0143(10) 0.0183(11) 0.0182(11) -0.0011(9) 0.0025(8) -0.0021(9) C10' 0.0221(12) 0.0218(12) 0.0183(11) 0.0027(9) 0.0030(9) -0.0012(9) C11' 0.0203(11) 0.0156(12) 0.0220(11) 0.0039(9) 0.0023(9) 0.0034(9) C12' 0.0140(10) 0.0135(11) 0.0225(11) -0.0005(9) 0.0046(9) 0.0001(8) C13' 0.0176(11) 0.0162(11) 0.0160(10) -0.0036(9) 0.0039(9) -0.0023(9) C14' 0.0141(11) 0.0192(12) 0.0275(12) -0.0017(10) 0.0014(9) 0.0007(9) C15' 0.0150(11) 0.0258(13) 0.0382(14) -0.0034(11) 0.0081(10) -0.0032(10) C16' 0.0256(12) 0.0215(13) 0.0324(13) -0.0023(10) 0.0135(10) -0.0067(10) C17' 0.0267(12) 0.0167(12) 0.0229(12) 0.0000(9) 0.0060(10) -0.0013(9) C18' 0.0162(11) 0.0157(11) 0.0177(11) -0.0026(9) 0.0018(9) -0.0006(9) C19' 0.0156(11) 0.0199(12) 0.0246(12) 0.0011(9) 0.0041(9) 0.0024(9) C20' 0.0136(10) 0.0218(12) 0.0192(11) -0.0020(9) 0.0049(9) 0.0039(9) C21' 0.0140(11) 0.0312(14) 0.0299(13) -0.0014(11) 0.0010(10) 0.0040(10) C22' 0.0136(11) 0.0369(15) 0.0390(14) -0.0103(12) 0.0012(10) -0.0037(10) C23' 0.0190(12) 0.0274(14) 0.0409(14) -0.0065(11) 0.0097(11) -0.0073(10) C24' 0.0209(11) 0.0186(12) 0.0259(12) -0.0009(10) 0.0094(9) -0.0011(9) C25' 0.0112(10) 0.0194(12) 0.0173(11) -0.0029(9) 0.0041(8) -0.0001(9) C26' 0.0159(11) 0.0162(11) 0.0155(10) 0.0042(9) -0.0018(8) 0.0007(9) C27' 0.0210(11) 0.0184(12) 0.0221(11) 0.0022(9) 0.0034(9) 0.0021(9) C28' 0.0163(11) 0.0243(13) 0.0281(12) 0.0071(10) 0.0009(10) 0.0002(9) C29' 0.0244(12) 0.0222(13) 0.0254(12) 0.0037(10) -0.0063(10) -0.0079(10) C30' 0.0292(12) 0.0185(12) 0.0157(11) -0.0009(9) -0.0013(9) -0.0019(10) C31' 0.0202(11) 0.0163(11) 0.0137(10) 0.0044(9) -0.0011(9) 0.0010(9) C32' 0.0211(11) 0.0151(11) 0.0167(11) 0.0008(9) 0.0035(9) 0.0017(9) C33' 0.0216(11) 0.0159(11) 0.0141(10) 0.0062(9) 0.0032(9) 0.0014(9) C34' 0.0282(13) 0.0238(13) 0.0245(12) -0.0008(10) 0.0121(10) 0.0004(10) C35' 0.0240(12) 0.0337(15) 0.0339(14) 0.0030(11) 0.0142(11) -0.0041(11) C36' 0.0252(12) 0.0238(13) 0.0253(12) 0.0040(10) 0.0045(10) -0.0075(10) C37' 0.0224(11) 0.0182(12) 0.0172(11) 0.0011(9) -0.0005(9) -0.0003(9) C38' 0.0150(10) 0.0197(11) 0.0118(10) 0.0035(9) 0.0007(8) 0.0021(9) C39' 0.0220(12) 0.0176(12) 0.0329(13) -0.0019(10) 0.0086(10) 0.0043(9) C40' 0.0250(12) 0.0270(14) 0.0340(14) 0.0062(11) 0.0018(10) 0.0049(10) C41' 0.0249(12) 0.0192(12) 0.0340(13) 0.0049(10) 0.0074(10) 0.0023(10) C42' 0.0311(13) 0.0244(13) 0.0189(12) -0.0036(10) 0.0051(10) -0.0013(10) C43' 0.064(2) 0.063(2) 0.0476(18) -0.0194(16) 0.0253(15) -0.0024(16) Cl1' 0.0469(6) 0.1091(13) 0.0468(7) 0.0408(7) -0.0047(6) -0.0073(7) Cl2' 0.0283(4) 0.0504(5) 0.0404(5) 0.0066(4) -0.0033(4) -0.0068(4) Cl1" 0.084(5) 0.030(3) 0.047(4) 0.008(3) 0.039(4) 0.019(3) Cl2" 0.038(3) 0.101(5) 0.041(3) 0.012(3) 0.018(2) 0.015(3) Cl1 0.1124(8) 0.0356(5) 0.0494(5) 0.0031(4) 0.0414(5) 0.0036(5) Cl2 0.0420(4) 0.0649(5) 0.0425(4) -0.0025(4) 0.0085(3) 0.0037(4) C43 0.116(3) 0.066(2) 0.0393(18) -0.0008(16) 0.0325(19) 0.022(2) _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 C1 1.749(2) . ? S1 C12 1.750(2) . ? N1 C4 1.435(3) . ? N1 C13 1.408(3) . ? N1 C25 1.416(3) . ? N2 C9 1.435(3) . ? N2 C26 1.411(3) . ? N2 C38 1.420(2) . ? C1 C2 1.396(3) . ? C1 C6 1.402(3) . ? C2 C3 1.382(3) . ? C3 C4 1.401(3) . ? C4 C5 1.377(3) . ? C5 C6 1.394(3) . ? C6 C7 1.448(3) . ? C7 C8 1.395(3) . ? C7 C12 1.404(3) . ? C8 C9 1.377(3) . ? C9 C10 1.402(3) . ? C10 C11 1.380(3) . ? C11 C12 1.394(3) . ? C13 C14 1.394(3) . ? C13 C18 1.401(3) . ? C14 C15 1.386(3) . ? C15 C16 1.379(3) . ? C16 C17 1.385(3) . ? C17 C18 1.385(3) . ? C18 C19 1.525(3) . ? C19 C20 1.517(3) . ? C19 C39 1.549(3) . ? C19 C40 1.521(3) . ? C20 C21 1.393(3) . ? C20 C25 1.398(3) . ? C21 C22 1.382(3) . ? C22 C23 1.375(4) . ? C23 C24 1.386(3) . ? C24 C25 1.393(3) . ? C26 C27 1.399(3) . ? C26 C31 1.400(3) . ? C27 C28 1.386(3) . ? C28 C29 1.382(3) . ? C29 C30 1.384(3) . ? C30 C31 1.392(3) . ? C31 C32 1.528(3) . ? C32 C33 1.521(3) . ? C32 C41 1.543(3) . ? C32 C42 1.531(3) . ? C33 C34 1.389(3) . ? C33 C38 1.401(3) . ? C34 C35 1.380(3) . ? C35 C36 1.382(3) . ? C36 C37 1.381(3) . ? C37 C38 1.392(3) . ? S1' C1' 1.746(2) . ? S1' C12' 1.751(2) . ? N1' C4' 1.435(3) . ? N1' C13' 1.411(3) . ? N1' C25' 1.414(2) . ? N2' C9' 1.434(3) . ? N2' C26' 1.403(3) . ? N2' C38' 1.407(2) . ? C1' C2' 1.400(3) . ? C1' C6' 1.401(3) . ? C2' C3' 1.378(3) . ? C3' C4' 1.400(3) . ? C4' C5' 1.380(3) . ? C5' C6' 1.399(3) . ? C6' C7' 1.447(3) . ? C7' C8' 1.394(3) . ? C7' C12' 1.401(3) . ? C8' C9' 1.378(3) . ? C9' C10' 1.398(3) . ? C10' C11' 1.382(3) . ? C11' C12' 1.395(3) . ? C13' C14' 1.397(3) . ? C13' C18' 1.400(3) . ? C14' C15' 1.383(3) . ? C15' C16' 1.380(3) . ? C16' C17' 1.386(3) . ? C17' C18' 1.389(3) . ? C18' C19' 1.527(3) . ? C19' C20' 1.518(3) . ? C19' C39' 1.553(3) . ? C19' C40' 1.522(3) . ? C20' C21' 1.395(3) . ? C20' C25' 1.401(3) . ? C21' C22' 1.381(3) . ? C22' C23' 1.375(3) . ? C23' C24' 1.384(3) . ? C24' C25' 1.392(3) . ? C26' C27' 1.403(3) . ? C26' C31' 1.400(3) . ? C27' C28' 1.378(3) . ? C28' C29' 1.383(3) . ? C29' C30' 1.383(3) . ? C30' C31' 1.393(3) . ? C31' C32' 1.528(3) . ? C32' C33' 1.529(3) . ? C32' C41' 1.541(3) . ? C32' C42' 1.548(3) . ? C33' C34' 1.393(3) . ? C33' C38' 1.398(3) . ? C34' C35' 1.378(3) . ? C35' C36' 1.379(3) . ? C36' C37' 1.385(3) . ? C37' C38' 1.398(3) . ? C43' Cl1' 1.697(3) . ? C43' Cl2' 1.791(3) . ? C43' Cl1" 1.912(7) . ? C43' Cl2" 1.353(6) . ? Cl1 C43 1.740(3) . ? Cl2 C43 1.746(3) . ? C43 Cl1A 1.513(16) . ? 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 C1 S1 C12 91.38(10) . . ? C13 N1 C4 118.48(16) . . ? C13 N1 C25 118.79(17) . . ? C25 N1 C4 119.42(17) . . ? C26 N2 C9 117.37(16) . . ? C26 N2 C38 119.21(16) . . ? C38 N2 C9 117.33(16) . . ? C2 C1 S1 126.48(17) . . ? C2 C1 C6 121.13(19) . . ? C6 C1 S1 112.39(15) . . ? C3 C2 C1 118.3(2) . . ? C2 C3 C4 120.8(2) . . ? C3 C4 N1 120.91(18) . . ? C5 C4 N1 118.32(18) . . ? C5 C4 C3 120.76(19) . . ? C4 C5 C6 119.35(19) . . ? C1 C6 C7 111.87(18) . . ? C5 C6 C1 119.62(18) . . ? C5 C6 C7 128.51(19) . . ? C8 C7 C6 128.33(19) . . ? C8 C7 C12 119.32(18) . . ? C12 C7 C6 112.35(18) . . ? C9 C8 C7 119.51(19) . . ? C8 C9 N2 118.75(18) . . ? C8 C9 C10 120.64(19) . . ? C10 C9 N2 120.61(18) . . ? C11 C10 C9 120.90(19) . . ? C10 C11 C12 118.3(2) . . ? C7 C12 S1 112.00(15) . . ? C11 C12 S1 126.65(16) . . ? C11 C12 C7 121.34(19) . . ? C14 C13 N1 121.31(19) . . ? C14 C13 C18 119.79(19) . . ? C18 C13 N1 118.90(18) . . ? C15 C14 C13 119.9(2) . . ? C16 C15 C14 120.7(2) . . ? C15 C16 C17 118.9(2) . . ? C18 C17 C16 121.8(2) . . ? C13 C18 C19 117.81(18) . . ? C17 C18 C13 118.56(19) . . ? C17 C18 C19 123.5(2) . . ? C18 C19 C39 107.29(17) . . ? C20 C19 C18 107.72(17) . . ? C20 C19 C39 107.21(17) . . ? C20 C19 C40 112.98(18) . . ? C40 C19 C18 112.33(18) . . ? C40 C19 C39 109.04(19) . . ? C21 C20 C19 123.6(2) . . ? C21 C20 C25 118.1(2) . . ? C25 C20 C19 118.09(18) . . ? C22 C21 C20 121.7(2) . . ? C23 C22 C21 119.3(2) . . ? C22 C23 C24 120.7(2) . . ? C23 C24 C25 119.8(2) . . ? C20 C25 N1 118.73(19) . . ? C24 C25 N1 121.1(2) . . ? C24 C25 C20 120.15(19) . . ? C27 C26 N2 119.97(19) . . ? C27 C26 C31 120.31(19) . . ? C31 C26 N2 119.73(18) . . ? C28 C27 C26 120.0(2) . . ? C29 C28 C27 120.4(2) . . ? C28 C29 C30 119.2(2) . . ? C29 C30 C31 122.1(2) . . ? C26 C31 C32 119.27(18) . . ? C30 C31 C26 117.86(19) . . ? C30 C31 C32 122.64(19) . . ? C31 C32 C41 107.38(18) . . ? C31 C32 C42 111.81(18) . . ? C33 C32 C31 108.80(17) . . ? C33 C32 C41 107.11(17) . . ? C33 C32 C42 112.36(19) . . ? C42 C32 C41 109.2(2) . . ? C34 C33 C32 122.45(19) . . ? C34 C33 C38 117.7(2) . . ? C38 C33 C32 119.65(18) . . ? C35 C34 C33 122.2(2) . . ? C34 C35 C36 119.3(2) . . ? C37 C36 C35 120.1(2) . . ? C36 C37 C38 120.2(2) . . ? C33 C38 N2 119.29(18) . . ? C37 C38 N2 120.35(18) . . ? C37 C38 C33 120.35(18) . . ? C1' S1' C12' 91.18(10) . . ? C13' N1' C4' 118.67(16) . . ? C13' N1' C25' 118.50(16) . . ? C25' N1' C4' 118.35(16) . . ? C26' N2' C9' 119.28(16) . . ? C26' N2' C38' 121.40(17) . . ? C38' N2' C9' 119.30(17) . . ? C2' C1' S1' 126.38(16) . . ? C2' C1' C6' 121.25(19) . . ? C6' C1' S1' 112.37(15) . . ? C3' C2' C1' 118.3(2) . . ? C2' C3' C4' 121.0(2) . . ? C3' C4' N1' 120.85(18) . . ? C5' C4' N1' 118.41(18) . . ? C5' C4' C3' 120.74(19) . . ? C4' C5' C6' 119.26(19) . . ? C1' C6' C7' 112.18(18) . . ? C5' C6' C1' 119.44(18) . . ? C5' C6' C7' 128.37(19) . . ? C8' C7' C6' 128.94(19) . . ? C8' C7' C12' 119.20(18) . . ? C12' C7' C6' 111.84(18) . . ? C9' C8' C7' 119.64(19) . . ? C8' C9' N2' 119.12(18) . . ? C8' C9' C10' 120.67(19) . . ? C10' C9' N2' 120.21(18) . . ? C11' C10' C9' 120.82(19) . . ? C10' C11' C12' 118.3(2) . . ? C7' C12' S1' 112.42(15) . . ? C11' C12' S1' 126.16(16) . . ? C11' C12' C7' 121.40(19) . . ? C14' C13' N1' 121.36(19) . . ? C14' C13' C18' 119.72(19) . . ? C18' C13' N1' 118.91(17) . . ? C15' C14' C13' 120.2(2) . . ? C16' C15' C14' 120.4(2) . . ? C15' C16' C17' 119.3(2) . . ? C16' C17' C18' 121.4(2) . . ? C13' C18' C19' 117.85(18) . . ? C17' C18' C13' 118.64(19) . . ? C17' C18' C19' 123.38(19) . . ? C18' C19' C39' 107.62(17) . . ? C20' C19' C18' 107.30(17) . . ? C20' C19' C39' 107.19(17) . . ? C20' C19' C40' 113.14(18) . . ? C40' C19' C18' 112.68(18) . . ? C40' C19' C39' 108.64(18) . . ? C21' C20' C19' 123.85(19) . . ? C21' C20' C25' 117.9(2) . . ? C25' C20' C19' 118.04(18) . . ? C22' C21' C20' 121.5(2) . . ? C23' C22' C21' 119.7(2) . . ? C22' C23' C24' 120.2(2) . . ? C23' C24' C25' 120.2(2) . . ? C20' C25' N1' 118.60(18) . . ? C24' C25' N1' 121.30(19) . . ? C24' C25' C20' 120.10(19) . . ? N2' C26' C27' 119.46(19) . . ? C31' C26' N2' 120.76(18) . . ? C31' C26' C27' 119.76(19) . . ? C28' C27' C26' 120.5(2) . . ? C27' C28' C29' 120.4(2) . . ? C28' C29' C30' 119.0(2) . . ? C29' C30' C31' 122.4(2) . . ? C26' C31' C32' 122.49(18) . . ? C30' C31' C26' 117.94(19) . . ? C30' C31' C32' 119.52(19) . . ? C31' C32' C33' 111.19(17) . . ? C31' C32' C41' 108.37(17) . . ? C31' C32' C42' 109.87(17) . . ? C33' C32' C41' 109.22(17) . . ? C33' C32' C42' 109.07(17) . . ? C41' C32' C42' 109.08(18) . . ? C34' C33' C32' 119.56(19) . . ? C34' C33' C38' 117.6(2) . . ? C38' C33' C32' 122.83(18) . . ? C35' C34' C33' 122.5(2) . . ? C34' C35' C36' 119.3(2) . . ? C35' C36' C37' 119.8(2) . . ? C36' C37' C38' 120.7(2) . . ? C33' C38' N2' 120.51(18) . . ? C37' C38' N2' 119.56(18) . . ? C37' C38' C33' 119.92(18) . . ? Cl1' C43' Cl2' 111.65(16) . . ? Cl2" C43' Cl1" 123.4(4) . . ? Cl1 C43 Cl2 113.35(17) . . ? Cl1A C43 Cl2 136.3(7) . . ? _shelx_res_file ; TITL 17srv183 in P21/n #14 17srv183.res created by SHELXL-2016/6 at 22:37:52 on 21-Jul-2017 REM reset to P21/n #14 CELL 0.71073 24.0937 7.9916 36.7515 90 99.3094 90 ZERR 8 0.0012 0.0004 0.0018 0 0.0016 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Cl D N S UNIT 344 272 16 16 16 8 RIGU C43' Cl1' > Cl2" L.S. 7 PLAN 7 SIZE 0.062 0.275 0.503 TEMP -153.15 BOND fmap 2 acta REM REM REM WGHT 0.048000 4.683000 FVAR 0.05279 0.02953 0.03991 0.04578 0.04499 0.03152 0.03479 FVAR 0.02599 0.03297 S1 6 0.465542 -0.159002 0.572598 11.00000 0.02540 0.01669 = 0.02128 -0.00123 0.00700 0.00576 N1 5 0.349071 0.333417 0.465751 11.00000 0.01392 0.01993 = 0.01690 0.00110 0.00127 -0.00233 N2 5 0.413159 0.364652 0.676358 11.00000 0.01605 0.01661 = 0.01601 -0.00338 0.00451 -0.00242 C1 1 0.432177 -0.027474 0.537738 11.00000 0.01422 0.01630 = 0.02190 -0.00038 0.00570 -0.00079 C2 1 0.425882 -0.056354 0.499822 11.00000 0.02648 0.01706 = 0.02308 -0.00368 0.00967 0.00147 AFIX 43 H2 2 0.440012 -0.155676 0.490450 11.00000 -1.20000 AFIX 0 C3 1 0.398588 0.063137 0.476274 11.00000 0.02637 0.02522 = 0.01574 -0.00375 0.00492 -0.00155 AFIX 43 H3 2 0.394287 0.046423 0.450377 11.00000 -1.20000 AFIX 0 C4 1 0.377176 0.208692 0.490139 11.00000 0.01468 0.01837 = 0.01875 0.00033 0.00285 -0.00256 C5 1 0.383500 0.236981 0.527539 11.00000 0.01301 0.01436 = 0.01910 -0.00349 0.00544 -0.00256 AFIX 43 H5 2 0.368897 0.335951 0.536750 11.00000 -1.20000 AFIX 0 C6 1 0.411536 0.118992 0.551753 11.00000 0.01215 0.01577 = 0.01774 -0.00063 0.00466 -0.00343 C7 1 0.423392 0.124246 0.591640 11.00000 0.01086 0.01398 = 0.01785 0.00097 0.00399 -0.00160 C8 1 0.411051 0.251265 0.615105 11.00000 0.01009 0.01459 = 0.01949 0.00008 0.00290 -0.00108 AFIX 43 H8 2 0.392339 0.349878 0.605258 11.00000 -1.20000 AFIX 0 C9 1 0.426185 0.232682 0.652637 11.00000 0.01147 0.01587 = 0.01854 -0.00158 0.00359 -0.00341 C10 1 0.454185 0.088127 0.667404 11.00000 0.01864 0.02168 = 0.01468 0.00110 0.00207 -0.00123 AFIX 43 H10 2 0.464330 0.077330 0.693372 11.00000 -1.20000 AFIX 0 C11 1 0.467206 -0.038647 0.644738 11.00000 0.01868 0.01781 = 0.02179 0.00393 0.00515 0.00180 AFIX 43 H11 2 0.486187 -0.136552 0.654762 11.00000 -1.20000 AFIX 0 C12 1 0.451788 -0.019369 0.606739 11.00000 0.01473 0.01356 = 0.02152 -0.00073 0.00651 -0.00064 C13 1 0.381859 0.454976 0.451383 11.00000 0.01730 0.01677 = 0.01585 -0.00572 0.00494 -0.00161 C14 1 0.440461 0.448875 0.458371 11.00000 0.01636 0.02073 = 0.02578 -0.00571 0.00266 0.00068 AFIX 43 H14 2 0.459057 0.365793 0.474381 11.00000 -1.20000 AFIX 0 C15 1 0.471549 0.564168 0.441932 11.00000 0.01714 0.02371 = 0.03664 -0.00891 0.00974 -0.00468 AFIX 43 H15 2 0.511463 0.560130 0.446944 11.00000 -1.20000 AFIX 0 C16 1 0.445183 0.684705 0.418377 11.00000 0.02649 0.02293 = 0.03429 -0.00477 0.01537 -0.00668 AFIX 43 H16 2 0.466579 0.760606 0.406357 11.00000 -1.20000 AFIX 0 C17 1 0.386989 0.693249 0.412537 11.00000 0.02973 0.02392 = 0.02256 -0.00125 0.00909 0.00047 AFIX 43 H17 2 0.368735 0.776675 0.396473 11.00000 -1.20000 AFIX 0 C18 1 0.354678 0.583550 0.429469 11.00000 0.01969 0.02180 = 0.01487 -0.00280 0.00436 0.00066 C19 1 0.291375 0.602997 0.428027 11.00000 0.01636 0.02517 = 0.02217 0.00032 0.00248 0.00289 C20 1 0.265676 0.429238 0.425353 11.00000 0.01503 0.02861 = 0.01775 -0.00311 0.00426 0.00121 C21 1 0.213635 0.391913 0.404429 11.00000 0.01691 0.03868 = 0.03108 -0.00606 0.00105 0.00255 AFIX 43 H21 2 0.195246 0.474042 0.388067 11.00000 -1.20000 AFIX 0 C22 1 0.188093 0.238431 0.406876 11.00000 0.01520 0.04804 = 0.04294 -0.01456 0.00031 -0.00504 AFIX 43 H22 2 0.152724 0.215077 0.392226 11.00000 -1.20000 AFIX 0 C23 1 0.214453 0.119843 0.430763 11.00000 0.02308 0.03335 = 0.04696 -0.01106 0.01002 -0.01134 AFIX 43 H23 2 0.196218 0.016305 0.433531 11.00000 -1.20000 AFIX 0 C24 1 0.267327 0.149791 0.450833 11.00000 0.02075 0.02486 = 0.03154 -0.00328 0.00861 -0.00391 AFIX 43 H24 2 0.285467 0.066462 0.466974 11.00000 -1.20000 AFIX 0 C25 1 0.293790 0.302548 0.447255 11.00000 0.01431 0.02487 = 0.01744 -0.00594 0.00622 -0.00130 C26 1 0.457434 0.472300 0.691376 11.00000 0.01628 0.01599 = 0.01584 0.00315 -0.00005 -0.00282 C27 1 0.509647 0.460800 0.679570 11.00000 0.02165 0.01947 = 0.02038 0.00000 0.00441 -0.00233 AFIX 43 H27 2 0.514668 0.385130 0.660433 11.00000 -1.20000 AFIX 0 C28 1 0.554049 0.559808 0.695793 11.00000 0.01650 0.02697 = 0.03124 0.00476 0.00375 -0.00404 AFIX 43 H28 2 0.589538 0.551254 0.687828 11.00000 -1.20000 AFIX 0 C29 1 0.547011 0.670907 0.723489 11.00000 0.02271 0.02346 = 0.02692 0.00445 -0.00708 -0.01033 AFIX 43 H29 2 0.577830 0.735580 0.735294 11.00000 -1.20000 AFIX 0 C30 1 0.494520 0.686838 0.733826 11.00000 0.02799 0.01941 = 0.01767 -0.00086 -0.00287 -0.00350 AFIX 43 H30 2 0.489559 0.765975 0.752319 11.00000 -1.20000 AFIX 0 C31 1 0.448753 0.590611 0.717991 11.00000 0.02157 0.01699 = 0.01436 0.00239 -0.00005 0.00047 C32 1 0.389215 0.619946 0.725993 11.00000 0.02427 0.01875 = 0.02484 -0.00638 0.00229 0.00076 C33 1 0.357738 0.454262 0.722663 11.00000 0.01722 0.01735 = 0.01451 0.00325 -0.00099 0.00429 C34 1 0.315260 0.418621 0.742912 11.00000 0.02247 0.02706 = 0.02047 0.00158 0.00863 0.00805 AFIX 43 H34 2 0.308585 0.494414 0.761644 11.00000 -1.20000 AFIX 0 C35 1 0.282422 0.276753 0.736727 11.00000 0.02692 0.02974 = 0.03538 0.00350 0.01748 -0.00070 AFIX 43 H35 2 0.254053 0.254686 0.751278 11.00000 -1.20000 AFIX 0 C36 1 0.291241 0.167172 0.709153 11.00000 0.02539 0.02132 = 0.03776 0.00057 0.01113 -0.00513 AFIX 43 H36 2 0.267959 0.071307 0.704082 11.00000 -1.20000 AFIX 0 C37 1 0.333853 0.196743 0.688940 11.00000 0.01973 0.01660 = 0.02266 -0.00141 0.00662 0.00003 AFIX 43 H37 2 0.339953 0.120694 0.670115 11.00000 -1.20000 AFIX 0 C38 1 0.367879 0.337542 0.696053 11.00000 0.01365 0.01608 = 0.01391 0.00244 0.00149 0.00284 C39 1 0.281989 0.678193 0.465414 11.00000 0.02201 0.02205 = 0.03174 -0.00181 0.00907 0.00252 AFIX 137 H39A 2 0.241634 0.694368 0.465268 11.00000 21.00000 H39B 2 0.301337 0.786174 0.469207 11.00000 21.00000 H39C 2 0.297057 0.601597 0.485413 11.00000 21.00000 AFIX 0 C40 1 0.265142 0.718320 0.397049 11.00000 0.02540 0.03741 = 0.03472 0.00795 0.00205 0.00881 AFIX 137 H40A 2 0.271229 0.671991 0.373322 11.00000 31.00000 H40B 2 0.282610 0.829151 0.400491 11.00000 31.00000 H40C 2 0.224681 0.728142 0.397371 11.00000 31.00000 AFIX 0 C41 1 0.359041 0.735918 0.695476 11.00000 0.02571 0.01809 = 0.06166 0.00891 0.00599 0.00157 AFIX 137 H41A 2 0.359875 0.685059 0.671306 11.00000 41.00000 H41B 2 0.378176 0.844481 0.696789 11.00000 41.00000 H41C 2 0.319911 0.751858 0.698953 11.00000 41.00000 AFIX 0 C42 1 0.389582 0.703087 0.763563 11.00000 0.03436 0.04984 = 0.04854 -0.03086 0.01665 -0.01385 AFIX 137 H42A 2 0.350803 0.719996 0.767704 11.00000 51.00000 H42B 2 0.408728 0.811445 0.764032 11.00000 51.00000 H42C 2 0.409449 0.631038 0.783002 11.00000 51.00000 AFIX 0 S1' 6 0.962562 -0.151226 0.567623 11.00000 0.02648 0.01556 = 0.02072 0.00042 0.00568 0.00662 N1' 5 0.847458 0.368236 0.467361 11.00000 0.01283 0.01640 = 0.01890 0.00169 0.00082 -0.00136 N2' 5 0.914346 0.343211 0.678813 11.00000 0.01594 0.01857 = 0.01968 -0.00535 0.00383 -0.00162 C1' 1 0.930086 -0.009798 0.534695 11.00000 0.01524 0.01441 = 0.02145 0.00043 0.00303 -0.00149 C2' 1 0.923615 -0.028430 0.496350 11.00000 0.02340 0.01760 = 0.02121 -0.00351 0.00609 0.00248 AFIX 43 H2' 2 0.937339 -0.125097 0.485660 11.00000 -1.20000 AFIX 0 C3' 1 0.896827 0.097083 0.474537 11.00000 0.02174 0.02357 = 0.01663 -0.00094 0.00420 -0.00039 AFIX 43 H3' 2 0.892370 0.087192 0.448466 11.00000 -1.20000 AFIX 0 C4' 1 0.876077 0.238943 0.490185 11.00000 0.01277 0.01556 = 0.02088 0.00257 0.00212 -0.00127 C5' 1 0.882815 0.258020 0.527977 11.00000 0.01095 0.01430 = 0.02166 -0.00322 0.00400 -0.00172 AFIX 43 H5' 2 0.868958 0.355080 0.538440 11.00000 -1.20000 AFIX 0 C6' 1 0.910276 0.132827 0.550695 11.00000 0.01047 0.01489 = 0.01924 0.00020 0.00495 -0.00286 C7' 1 0.921977 0.127604 0.590559 11.00000 0.00988 0.01376 = 0.02034 0.00157 0.00328 -0.00078 C8' 1 0.910434 0.247405 0.615860 11.00000 0.01261 0.01383 = 0.02059 -0.00086 0.00339 0.00023 AFIX 43 H8' 2 0.891657 0.348175 0.607507 11.00000 -1.20000 AFIX 0 C9' 1 0.926401 0.218900 0.653050 11.00000 0.01429 0.01833 = 0.01815 -0.00106 0.00246 -0.00214 C10' 1 0.953729 0.070658 0.665660 11.00000 0.02210 0.02175 = 0.01833 0.00267 0.00298 -0.00116 AFIX 43 H10' 2 0.964163 0.052579 0.691407 11.00000 -1.20000 AFIX 0 C11' 1 0.965761 -0.049944 0.641144 11.00000 0.02026 0.01565 = 0.02205 0.00393 0.00229 0.00341 AFIX 43 H11' 2 0.984333 -0.150752 0.649694 11.00000 -1.20000 AFIX 0 C12' 1 0.949918 -0.019784 0.603498 11.00000 0.01403 0.01345 = 0.02252 -0.00049 0.00464 0.00009 C13' 1 0.879759 0.485578 0.451137 11.00000 0.01759 0.01619 = 0.01602 -0.00357 0.00390 -0.00233 C14' 1 0.938320 0.474066 0.455744 11.00000 0.01411 0.01920 = 0.02751 -0.00174 0.00139 0.00071 AFIX 43 H14' 2 0.957339 0.390557 0.471437 11.00000 -1.20000 AFIX 0 C15' 1 0.968699 0.583863 0.437532 11.00000 0.01504 0.02575 = 0.03818 -0.00337 0.00805 -0.00320 AFIX 43 H15' 2 1.008535 0.575635 0.440856 11.00000 -1.20000 AFIX 0 C16' 1 0.941533 0.705306 0.414560 11.00000 0.02560 0.02153 = 0.03245 -0.00234 0.01355 -0.00670 AFIX 43 H16' 2 0.962337 0.777831 0.401328 11.00000 -1.20000 AFIX 0 C17' 1 0.883601 0.720429 0.410982 11.00000 0.02666 0.01667 = 0.02285 -0.00004 0.00604 -0.00130 AFIX 43 H17' 2 0.864990 0.804907 0.395378 11.00000 -1.20000 AFIX 0 C18' 1 0.852145 0.614764 0.429712 11.00000 0.01617 0.01572 = 0.01766 -0.00265 0.00182 -0.00059 C19' 1 0.789434 0.638898 0.430264 11.00000 0.01562 0.01995 = 0.02458 0.00106 0.00411 0.00236 C20' 1 0.762807 0.466278 0.428625 11.00000 0.01364 0.02180 = 0.01924 -0.00196 0.00491 0.00392 C21' 1 0.709861 0.429435 0.408722 11.00000 0.01396 0.03124 = 0.02986 -0.00142 0.00099 0.00399 AFIX 43 H21' 2 0.691137 0.510765 0.392290 11.00000 -1.20000 AFIX 0 C22' 1 0.684071 0.277454 0.412371 11.00000 0.01364 0.03689 = 0.03901 -0.01032 0.00122 -0.00375 AFIX 43 H22' 2 0.648048 0.254798 0.398512 11.00000 -1.20000 AFIX 0 C23' 1 0.710735 0.159064 0.436139 11.00000 0.01904 0.02739 = 0.04088 -0.00649 0.00966 -0.00732 AFIX 43 H23' 2 0.692279 0.056666 0.439643 11.00000 -1.20000 AFIX 0 C24' 1 0.764373 0.188491 0.454985 11.00000 0.02093 0.01858 = 0.02589 -0.00087 0.00935 -0.00108 AFIX 43 H24' 2 0.782894 0.105434 0.471036 11.00000 -1.20000 AFIX 0 C25' 1 0.791243 0.339474 0.450479 11.00000 0.01117 0.01940 = 0.01729 -0.00292 0.00408 -0.00013 C26' 1 0.954411 0.467587 0.690454 11.00000 0.01587 0.01625 = 0.01547 0.00423 -0.00178 0.00067 C27' 1 1.006341 0.464233 0.677828 11.00000 0.02102 0.01836 = 0.02211 0.00216 0.00343 0.00209 AFIX 43 H27' 2 1.013129 0.381965 0.660413 11.00000 -1.20000 AFIX 0 C28' 1 1.047562 0.579262 0.690479 11.00000 0.01632 0.02433 = 0.02812 0.00707 0.00088 0.00022 AFIX 43 H28' 2 1.082649 0.575333 0.681864 11.00000 -1.20000 AFIX 0 C29' 1 1.038141 0.700432 0.715654 11.00000 0.02440 0.02218 = 0.02542 0.00369 -0.00625 -0.00785 AFIX 43 H29' 2 1.066754 0.778539 0.724775 11.00000 -1.20000 AFIX 0 C30' 1 0.986413 0.706107 0.727340 11.00000 0.02922 0.01851 = 0.01575 -0.00087 -0.00128 -0.00188 AFIX 43 H30' 2 0.979818 0.790614 0.744313 11.00000 -1.20000 AFIX 0 C31' 1 0.943634 0.592350 0.715116 11.00000 0.02025 0.01626 = 0.01374 0.00441 -0.00105 0.00098 C32' 1 0.886524 0.611489 0.727666 11.00000 0.02114 0.01509 = 0.01671 0.00076 0.00353 0.00173 C33' 1 0.848201 0.462806 0.715207 11.00000 0.02156 0.01595 = 0.01412 0.00616 0.00315 0.00139 C34' 1 0.795470 0.452867 0.726009 11.00000 0.02822 0.02381 = 0.02451 -0.00077 0.01212 0.00045 AFIX 43 H34' 2 0.784018 0.540407 0.740636 11.00000 -1.20000 AFIX 0 C35' 1 0.759286 0.320869 0.716282 11.00000 0.02399 0.03372 = 0.03393 0.00299 0.01422 -0.00405 AFIX 43 H35' 2 0.723336 0.319010 0.723743 11.00000 -1.20000 AFIX 0 C36' 1 0.775793 0.191573 0.695618 11.00000 0.02520 0.02381 = 0.02531 0.00400 0.00451 -0.00754 AFIX 43 H36' 2 0.751954 0.097442 0.689721 11.00000 -1.20000 AFIX 0 C37' 1 0.827230 0.199327 0.683482 11.00000 0.02241 0.01821 = 0.01716 0.00114 -0.00046 -0.00026 AFIX 43 H37' 2 0.838251 0.110949 0.668902 11.00000 -1.20000 AFIX 0 C38' 1 0.863102 0.335821 0.692460 11.00000 0.01505 0.01971 = 0.01181 0.00348 0.00066 0.00213 C39' 1 0.783132 0.716311 0.468145 11.00000 0.02197 0.01763 = 0.03285 -0.00192 0.00857 0.00425 AFIX 137 H39D 2 0.743186 0.733947 0.469245 11.00000 61.00000 H39E 2 0.802954 0.823748 0.471146 11.00000 61.00000 H39F 2 0.799280 0.640083 0.487945 11.00000 61.00000 AFIX 0 C40' 1 0.761678 0.755210 0.399865 11.00000 0.02503 0.02697 = 0.03399 0.00615 0.00182 0.00490 AFIX 137 H40D 2 0.765902 0.708676 0.375794 11.00000 71.00000 H40E 2 0.779651 0.865457 0.402840 11.00000 71.00000 H40F 2 0.721615 0.766371 0.401393 11.00000 71.00000 AFIX 0 C41' 1 0.858738 0.773362 0.710682 11.00000 0.02494 0.01917 = 0.03398 0.00492 0.00737 0.00232 AFIX 137 H41D 2 0.853731 0.766008 0.683731 11.00000 81.00000 H41E 2 0.882806 0.869274 0.719034 11.00000 81.00000 H41F 2 0.822013 0.787718 0.718483 11.00000 81.00000 AFIX 0 C42' 1 0.894580 0.624760 0.770225 11.00000 0.03111 0.02436 = 0.01893 -0.00362 0.00512 -0.00134 AFIX 137 H42D 2 0.857735 0.631962 0.778167 11.00000 91.00000 H42E 2 0.916541 0.725177 0.778247 11.00000 91.00000 H42F 2 0.914563 0.525541 0.781201 11.00000 91.00000 AFIX 0 C43' 1 0.669280 0.754745 0.641577 11.00000 0.06353 0.06278 = 0.04761 -0.01937 0.02528 -0.00243 PART 1 AFIX 23 D43A 4 0.699866 0.797998 0.629147 10.85000 -1.20000 D43B 4 0.662859 0.636018 0.634426 10.85000 -1.20000 AFIX 23 PART 0 PART 2 D43C 4 0.649014 0.662515 0.627118 10.15000 -1.20000 D43D 4 0.696447 0.799729 0.626539 10.15000 -1.20000 AFIX 0 PART 0 PART 1 CL1' 3 0.609682 0.865678 0.627271 10.85000 0.04689 0.10906 = 0.04682 0.04076 -0.00466 -0.00735 CL2' 3 0.690434 0.768075 0.690513 10.85000 0.02829 0.05045 = 0.04036 0.00656 -0.00331 -0.00680 PART 0 PART 2 CL1" 3 0.615161 0.927566 0.644194 10.15000 0.08366 0.02990 = 0.04651 0.00800 0.03870 0.01900 CL2" 3 0.700089 0.683643 0.671642 10.15000 0.03779 0.10101 = 0.04098 0.01175 0.01799 0.01523 PART 0 PART 1 CL1 3 0.141414 0.900209 0.653075 10.94000 0.11239 0.03564 = 0.04945 0.00310 0.04143 0.00364 PART 0 CL2 3 0.202424 0.587940 0.670160 11.00000 0.04195 0.06486 = 0.04253 -0.00245 0.00853 0.00373 C43 1 0.171790 0.725926 0.635847 11.00000 0.11629 0.06614 = 0.03928 -0.00081 0.03249 0.02160 PART 1 AFIX 23 D43E 4 0.200910 0.763889 0.621540 11.00000 -1.20000 D43F 4 0.142587 0.665469 0.618755 11.00000 -1.20000 AFIX 0 PART 0 PART 2 CL1A 3 0.122569 0.846002 0.630603 10.06000 0.06592 HKLF 4 REM 17srv183 in P21/n #14 REM R1 = 0.0467 for 9504 Fo > 4sig(Fo) and 0.0769 for all 13247 data REM 903 parameters refined using 18 restraints END WGHT 0.0478 4.6888 REM Highest difference peak 0.344, deepest hole -0.514, 1-sigma level 0.052 Q1 1 0.1014 0.9029 0.6386 11.00000 0.05 0.34 Q2 1 0.1999 0.7118 0.6731 11.00000 0.05 0.29 Q3 1 0.9527 -0.0881 0.5896 11.00000 0.05 0.29 Q4 1 0.7441 0.4405 0.4121 11.00000 0.05 0.25 Q5 1 0.3199 0.3170 0.4558 11.00000 0.05 0.25 Q6 1 0.8178 0.3574 0.4584 11.00000 0.05 0.25 Q7 1 0.4584 -0.0877 0.5932 11.00000 0.05 0.24 ; _shelx_res_checksum 95679 _olex2_submission_special_instructions 'No special instructions were received' _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_DtBAcDBT_18s436 _database_code_depnum_ccdc_archive 'CCDC 1901570' loop_ _audit_author_name _audit_author_address 'Andrei S. Batsanov' ;Durham University United Kingdom ; _audit_update_record ; 2019-03-06 deposited with the CCDC. 2019-10-14 downloaded from the CCDC. ; _audit_creation_date 2018-10-11 _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 'C58 H66 N2 S' _chemical_formula_sum 'C58 H66 N2 S' _chemical_formula_weight 823.18 _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' 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 9.8347(4) _cell_length_b 12.1070(5) _cell_length_c 21.2839(9) _cell_angle_alpha 83.6588(19) _cell_angle_beta 88.476(2) _cell_angle_gamma 74.8909(19) _cell_volume 2431.67(18) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7666 _cell_measurement_temperature 200 _cell_measurement_theta_max 23.35 _cell_measurement_theta_min 2.35 _shelx_estimated_absorpt_T_max 0.978 _shelx_estimated_absorpt_T_min 0.947 _exptl_absorpt_coefficient_mu 0.105 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.9453 _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 0.0967 before and 0.0452 after correction. The Ratio of minimum to maximum transmission is 0.9453. 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 1.124 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description parallelepiped _exptl_crystal_F_000 888 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 0.00 1.00 0.0840 -1.00 0.00 -1.00 0.1050 0.00 -1.00 0.00 0.1110 0.00 1.00 0.00 0.1170 0.00 2.00 1.00 0.1200 0.00 1.00 -2.00 0.1440 0.00 -1.00 2.00 0.1800 -2.00 -2.00 1.00 0.2060 0.00 -1.00 -1.00 0.0980 0.00 1.00 1.00 0.1380 -1.00 2.00 0.00 0.1310 0.00 0.00 -1.00 0.1420 0.00 0.00 1.00 0.1650 _exptl_crystal_size_max 0.465 _exptl_crystal_size_mid 0.272 _exptl_crystal_size_min 0.21 _exptl_special_details ; Data were collected in shutterless mode. Full sphere of reciprocal space was nominally covered by 2 runs of 340 and 1 run of 303 narrow-frame \w-scans (scan width 0.5\%, 6s exposure), every run at a different \f angle. Two runs of 358 \f-scans (scan width 1\%, 1s 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 0.0377 _diffrn_reflns_av_unetI/netI 0.0471 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 27673 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_min 2.349 _diffrn_ambient_temperature 200 _diffrn_detector_area_resol_mean 10.4 _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 '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 5863 _reflns_number_total 8540 _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 v8.38A (Bruker, 2017)' _computing_data_collection 'APEX3 v.2016.1-0 (Bruker, 2016)' _computing_data_reduction 'SAINT v8.38A (Bruker, 2017)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL 2018/3 multi-CPU (Sheldrick, 2015)' _computing_structure_solution 'ShelXS 2013/1 (Sheldrick, 2008)' _refine_diff_density_max 0.277 _refine_diff_density_min -0.209 _refine_diff_density_rms 0.038 _refine_ls_extinction_coef 0.0073(10) _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, 2015)' _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 628 _refine_ls_number_reflns 8540 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0842 _refine_ls_R_factor_gt 0.0513 _refine_ls_restrained_S_all 1.254 _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^)+(0.0591P)^2^+0.9287P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1233 _refine_ls_wR_factor_ref 0.1372 _refine_special_details ; t-Bu group C(43)Me~3~ is rotationally disordered between two orientations, A and B, with occupancies 0.720(6) and 0.280(6), respectively. The C(43) atom is not disordered. t-Bu group C(47)Me~3~ is disordered [including C(47)] by rotation and tilt, between two orientations, A and B, with occupancies 0.490(9) and 0.510(9), respectively. t-Bu group C(51)Me~3~ is disordered [including C(51)] by rotation and tilt, between two orientations, A and B, with occupancies 0.637(3) and 0.363(3), respectively. All ordered methyl groups were refined as rigid bodies rotating around C---C bonds, with a common refined U for three H atoms. Major components of disordered methyl groups were refined likewise, with U of H atoms fixed to 1.5 U(eq) of the carbon atoms. 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 C49B-C47B \\sim C48B-C47B \\sim C50B-C47B \\sim C48A-C47A \\sim C49A-C47A \\sim C50A-C47A with sigma of 0.02 C54A-C51A \\sim C53B-C51B \\sim C52A-C51A \\sim C54B-C51B \\sim C44A-H44C \\sim C52B-C51B \\sim C53A- C51A with sigma of 0.02 C51A-C31 \\sim C51B-C31 with sigma of 0.02 C47B-C22 \\sim C47A-C22 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(C51A) = Uanis(C51B) Uanis(C52B) = Uanis(C52A) Uanis(C53A) = Uanis(C53B) Uanis(C54A) = Uanis(C54B) Uanis(C47A) = Uanis(C47B) Uanis(C45B) = Uanis(C45A) Uanis(C44A) = Uanis(C44B) Uanis(C46B) = Uanis(C46A) 4. Others Sof(C47B)=Sof(C48B)=Sof(H48D)=Sof(H48E)=Sof(H48F)=Sof(C49B)=Sof(H49D)= Sof(H49E)=Sof(H49F)=Sof(C50B)=Sof(H50D)=Sof(H50E)=Sof(H50F)=1-FVAR(1) Sof(C47A)=Sof(C48A)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C49A)=Sof(H49A)= Sof(H49B)=Sof(H49C)=Sof(C50A)=Sof(H50A)=Sof(H50B)=Sof(H50C)=FVAR(1) Sof(C51B)=Sof(C52B)=Sof(H52D)=Sof(H52E)=Sof(H52F)=Sof(C53B)=Sof(H53D)= Sof(H53E)=Sof(H53F)=Sof(C54B)=Sof(H54D)=Sof(H54E)=Sof(H54F)=1-FVAR(2) Sof(C51A)=Sof(C52A)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C53A)=Sof(H53A)= Sof(H53B)=Sof(H53C)=Sof(C54A)=Sof(H54A)=Sof(H54B)=Sof(H54C)=FVAR(2) Uiso(H26A)=Uiso(H26B)=Uiso(H26C)=FVAR(3) Uiso(H27A)=Uiso(H27B)=Uiso(H27C)=FVAR(4) Uiso(H41A)=Uiso(H41B)=Uiso(H41C)=FVAR(5) Uiso(H42A)=Uiso(H42B)=Uiso(H42C)=FVAR(6) Uiso(H56A)=Uiso(H56B)=Uiso(H56C)=FVAR(7) Uiso(H57A)=Uiso(H57B)=Uiso(H57C)=FVAR(8) Uiso(H58A)=Uiso(H58B)=Uiso(H58C)=FVAR(9) Sof(C44B)=Sof(H44D)=Sof(H44E)=Sof(H44F)=Sof(C46B)=Sof(H46D)=Sof(H46E)= Sof(H46F)=Sof(C45B)=Sof(H45D)=Sof(H45E)=Sof(H45F)=1-FVAR(10) Sof(C44A)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C45A)=Sof(H45A)=Sof(H45B)= Sof(H45C)=Sof(C46A)=Sof(H46A)=Sof(H46B)=Sof(H46C)=FVAR(10) 5.a Me refined with riding coordinates: C48B(H48D,H48E,H48F), C49B(H49D,H49E,H49F), C50B(H50D,H50E,H50F), C52B(H52D, H52E,H52F), C53B(H53D,H53E,H53F), C54B(H54D,H54E,H54F), C44B(H44D,H44E,H44F), C46B(H46D,H46E,H46F), C45B(H45D,H45E,H45F) 5.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C5(H5), C8(H8), C10(H10), C11(H11), C14(H14), C15(H15), C17(H17), C21(H21), C23(H23), C24(H24), C29(H29), C30(H30), C32(H32), C36(H36), C38(H38), C39(H39) 5.c Idealised Me refined as rotating group: C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C41(H41A,H41B,H41C), C42(H42A,H42B, H42C), C44A(H44A,H44B,H44C), C45A(H45A,H45B,H45C), C46A(H46A,H46B,H46C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C48A(H48A,H48B, H48C), C49A(H49A,H49B,H49C), C50A(H50A,H50B,H50C), C52A(H52A,H52B,H52C), C53A(H53A,H53B,H53C), C54A(H54A,H54B,H54C) ; _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 S S 0.13173(6) 0.81595(5) 0.22875(3) 0.04116(18) Uani 1 1 d . . . . . N1 N 0.06634(19) 0.41934(15) 0.10322(8) 0.0385(4) Uani 1 1 d . . . . . N2 N 0.47726(18) 0.43309(15) 0.40091(8) 0.0383(4) Uani 1 1 d . . . . . C1 C 0.0962(2) 0.70817(17) 0.18842(9) 0.0338(5) Uani 1 1 d . . . . . C2 C 0.0080(2) 0.7238(2) 0.13656(10) 0.0434(6) Uani 1 1 d . . . . . H2 H -0.043677 0.798777 0.120158 0.052 Uiso 1 1 calc R . . . . C3 C -0.0032(2) 0.6281(2) 0.10924(10) 0.0438(6) Uani 1 1 d . . . . . H3 H -0.063803 0.637321 0.073934 0.053 Uiso 1 1 calc R . . . . C4 C 0.0730(2) 0.51872(18) 0.13282(9) 0.0348(5) Uani 1 1 d . . . . . C5 C 0.1578(2) 0.50316(17) 0.18502(9) 0.0317(5) Uani 1 1 d . . . . . H5 H 0.207758 0.427806 0.201582 0.038 Uiso 1 1 calc R . . . . C6 C 0.1703(2) 0.59794(16) 0.21359(9) 0.0281(5) Uani 1 1 d . . . . . C7 C 0.2544(2) 0.60062(16) 0.26799(9) 0.0290(5) Uani 1 1 d . . . . . C8 C 0.3335(2) 0.50892(17) 0.30780(9) 0.0318(5) Uani 1 1 d . . . . . H8 H 0.339751 0.432098 0.299779 0.038 Uiso 1 1 calc R . . . . C9 C 0.4027(2) 0.52963(18) 0.35892(10) 0.0353(5) Uani 1 1 d . . . . . C10 C 0.3968(2) 0.64188(19) 0.36989(11) 0.0431(6) Uani 1 1 d . . . . . H10 H 0.447747 0.655034 0.404388 0.052 Uiso 1 1 calc R . . . . C11 C 0.3184(2) 0.73420(19) 0.33156(10) 0.0429(6) Uani 1 1 d . . . . . H11 H 0.314150 0.810708 0.339508 0.052 Uiso 1 1 calc R . . . . C12 C 0.2452(2) 0.71331(17) 0.28078(9) 0.0339(5) Uani 1 1 d . . . . . C13 C 0.1653(2) 0.38021(18) 0.05662(9) 0.0338(5) Uani 1 1 d . . . . . C14 C 0.2403(2) 0.45299(19) 0.02607(10) 0.0422(6) Uani 1 1 d . . . . . H14 H 0.222584 0.529859 0.036320 0.051 Uiso 1 1 calc R . . . . C15 C 0.3398(2) 0.4152(2) -0.01886(11) 0.0456(6) Uani 1 1 d . . . . . H15 H 0.389377 0.466871 -0.039163 0.055 Uiso 1 1 calc R . . . . C16 C 0.3693(2) 0.30459(19) -0.03505(11) 0.0438(6) Uani 1 1 d . . . . . C17 C 0.2919(2) 0.23345(19) -0.00453(11) 0.0409(5) Uani 1 1 d . . . . . H17 H 0.310320 0.156682 -0.015026 0.049 Uiso 1 1 calc R . . . . C18 C 0.1889(2) 0.26843(18) 0.04057(9) 0.0329(5) Uani 1 1 d . . . . . C19 C 0.1133(2) 0.18421(18) 0.07520(10) 0.0350(5) Uani 1 1 d . . . . . C20 C -0.0218(2) 0.25037(18) 0.10581(9) 0.0340(5) Uani 1 1 d . . . . . C21 C -0.1279(2) 0.1969(2) 0.12491(11) 0.0431(6) Uani 1 1 d . . . . . H21 H -0.119387 0.121614 0.113672 0.052 Uiso 1 1 calc R . . . . C22 C -0.2453(2) 0.2472(2) 0.15942(11) 0.0440(6) Uani 1 1 d D . . . . C23 C -0.2540(2) 0.3566(2) 0.17505(11) 0.0457(6) Uani 1 1 d . . . . . H23 H -0.331787 0.393745 0.199194 0.055 Uiso 1 1 calc R . . . . C24 C -0.1525(2) 0.4132(2) 0.15646(10) 0.0422(6) Uani 1 1 d . . . . . H24 H -0.162184 0.488793 0.167438 0.051 Uiso 1 1 calc R . . . . C25 C -0.0362(2) 0.36103(18) 0.12182(9) 0.0339(5) Uani 1 1 d . . . . . C26 C 0.0817(3) 0.1028(2) 0.03129(13) 0.0622(8) Uani 1 1 d . . . . . H26A H 0.042173 0.045158 0.055822 0.074(5) Uiso 1 1 calc GR . . . . H26B H 0.168880 0.064132 0.010796 0.074(5) Uiso 1 1 calc GR . . . . H26C H 0.013672 0.146653 -0.000993 0.074(5) Uiso 1 1 calc GR . . . . C27 C 0.2103(2) 0.1134(2) 0.12896(12) 0.0540(7) Uani 1 1 d . . . . . H27A H 0.228736 0.165031 0.158106 0.067(5) Uiso 1 1 calc GR . . . . H27B H 0.299404 0.071710 0.111158 0.067(5) Uiso 1 1 calc GR . . . . H27C H 0.164352 0.058205 0.151833 0.067(5) Uiso 1 1 calc GR . . . . C28 C 0.6155(2) 0.37539(18) 0.38687(9) 0.0334(5) Uani 1 1 d . . . . . C29 C 0.6942(2) 0.42662(19) 0.34294(10) 0.0395(5) Uani 1 1 d . . . . . H29 H 0.652406 0.500338 0.321491 0.047 Uiso 1 1 calc R . . . . C30 C 0.8322(2) 0.37150(19) 0.33016(10) 0.0411(5) Uani 1 1 d . . . . . H30 H 0.883202 0.408016 0.299695 0.049 Uiso 1 1 calc R . . . . C31 C 0.8979(2) 0.26485(19) 0.36049(10) 0.0404(5) Uani 1 1 d D . . . . C32 C 0.8165(2) 0.21444(19) 0.40345(10) 0.0402(5) Uani 1 1 d . . . . . H32 H 0.858851 0.140587 0.424583 0.048 Uiso 1 1 calc R . . . . C33 C 0.6766(2) 0.26600(18) 0.41719(9) 0.0340(5) Uani 1 1 d . . . . . C34 C 0.5888(2) 0.20007(18) 0.45865(10) 0.0364(5) Uani 1 1 d . . . . . C35 C 0.4585(2) 0.28245(18) 0.48354(10) 0.0349(5) Uani 1 1 d . . . . . C36 C 0.3806(2) 0.2463(2) 0.53358(10) 0.0409(5) Uani 1 1 d . . . . . H36 H 0.413392 0.169776 0.553124 0.049 Uiso 1 1 calc R . . . . C37 C 0.2580(2) 0.3155(2) 0.55666(11) 0.0434(6) Uani 1 1 d . . . . . C38 C 0.2138(2) 0.4262(2) 0.52715(11) 0.0489(6) Uani 1 1 d . . . . . H38 H 0.131463 0.476963 0.541962 0.059 Uiso 1 1 calc R . . . . C39 C 0.2860(2) 0.4649(2) 0.47682(11) 0.0459(6) Uani 1 1 d . . . . . H39 H 0.252333 0.541578 0.457507 0.055 Uiso 1 1 calc R . . . . C40 C 0.4073(2) 0.39379(19) 0.45376(9) 0.0353(5) Uani 1 1 d . . . . . C41 C 0.6780(3) 0.1252(2) 0.51295(12) 0.0558(7) Uani 1 1 d . . . . . H41A H 0.752371 0.065252 0.495917 0.069(5) Uiso 1 1 calc GR . . . . H41B H 0.618117 0.089217 0.541451 0.069(5) Uiso 1 1 calc GR . . . . H41C H 0.720626 0.173035 0.536322 0.069(5) Uiso 1 1 calc GR . . . . C42 C 0.5379(3) 0.1226(2) 0.41680(13) 0.0553(7) Uani 1 1 d . . . . . H42A H 0.480142 0.170501 0.382100 0.066(4) Uiso 1 1 calc GR . . . . H42B H 0.481628 0.078391 0.442273 0.066(4) Uiso 1 1 calc GR . . . . H42C H 0.619476 0.069587 0.399431 0.066(4) Uiso 1 1 calc GR . . . . C43 C 0.4844(3) 0.2603(2) -0.08345(13) 0.0577(7) Uani 1 1 d . . . . . C44A C 0.6070(8) 0.1802(9) -0.0505(3) 0.157(4) Uani 0.720(6) 1 d D . P A 1 H44A H 0.637595 0.217408 -0.016810 0.236 Uiso 0.720(6) 1 calc GR . P A 1 H44B H 0.684099 0.159281 -0.080650 0.236 Uiso 0.720(6) 1 calc GR . P A 1 H44C H 0.580963 0.110767 -0.032132 0.236 Uiso 0.720(6) 1 calc DGR . P A 1 C45A C 0.5312(8) 0.3534(4) -0.1223(3) 0.097(2) Uani 0.720(6) 1 d . . P A 1 H45A H 0.450764 0.404844 -0.145833 0.146 Uiso 0.720(6) 1 calc GR . P A 1 H45B H 0.603867 0.319491 -0.152056 0.146 Uiso 0.720(6) 1 calc GR . P A 1 H45C H 0.569969 0.397232 -0.094607 0.146 Uiso 0.720(6) 1 calc GR . P A 1 C46A C 0.4271(10) 0.1977(11) -0.1307(4) 0.153(4) Uani 0.720(6) 1 d . . P A 1 H46A H 0.396142 0.133504 -0.108057 0.229 Uiso 0.720(6) 1 calc GR . P A 1 H46B H 0.501127 0.168058 -0.160802 0.229 Uiso 0.720(6) 1 calc GR . P A 1 H46C H 0.347028 0.251209 -0.153499 0.229 Uiso 0.720(6) 1 calc GR . P A 1 C55 C 0.1764(3) 0.2682(2) 0.61107(12) 0.0541(7) Uani 1 1 d . . . . . C56 C 0.2780(4) 0.2115(4) 0.66587(16) 0.1127(14) Uani 1 1 d . . . . . H56A H 0.349210 0.145873 0.651933 0.181(12) Uiso 1 1 calc GR . . . . H56B H 0.225241 0.184682 0.701466 0.181(12) Uiso 1 1 calc GR . . . . H56C H 0.324278 0.267591 0.679186 0.181(12) Uiso 1 1 calc GR . . . . C57 C 0.0626(4) 0.3619(3) 0.63688(16) 0.0891(11) Uani 1 1 d . . . . . H57A H 0.104729 0.419611 0.651311 0.148(9) Uiso 1 1 calc GR . . . . H57B H 0.015851 0.328322 0.672466 0.148(9) Uiso 1 1 calc GR . . . . H57C H -0.006686 0.398384 0.603610 0.148(9) Uiso 1 1 calc GR . . . . C58 C 0.1126(4) 0.1792(3) 0.58921(19) 0.1113(15) Uani 1 1 d . . . . . H58A H 0.040625 0.215748 0.557077 0.152(10) Uiso 1 1 calc GR . . . . H58B H 0.069329 0.143472 0.625212 0.152(10) Uiso 1 1 calc GR . . . . H58C H 0.186199 0.120128 0.571068 0.152(10) Uiso 1 1 calc GR . . . . C47A C -0.3661(11) 0.1925(9) 0.1791(5) 0.0545(11) Uani 0.490(9) 1 d D . P B 1 C48A C -0.3660(10) 0.1720(8) 0.2511(3) 0.083(4) Uani 0.490(9) 1 d D . P B 1 H48A H -0.439974 0.134025 0.265034 0.125 Uiso 0.490(9) 1 calc GR . P B 1 H48B H -0.383733 0.245829 0.268781 0.125 Uiso 0.490(9) 1 calc GR . P B 1 H48C H -0.274251 0.122854 0.265859 0.125 Uiso 0.490(9) 1 calc GR . P B 1 C49A C -0.5047(6) 0.2712(6) 0.1532(6) 0.093(3) Uani 0.490(9) 1 d D . P B 1 H49A H -0.582612 0.239320 0.168907 0.140 Uiso 0.490(9) 1 calc GR . P B 1 H49B H -0.503111 0.277308 0.106938 0.140 Uiso 0.490(9) 1 calc GR . P B 1 H49C H -0.517531 0.347766 0.167188 0.140 Uiso 0.490(9) 1 calc GR . P B 1 C50A C -0.3441(12) 0.0762(8) 0.1546(5) 0.085(4) Uani 0.490(9) 1 d D . P B 1 H50A H -0.425205 0.045290 0.166067 0.128 Uiso 0.490(9) 1 calc GR . P B 1 H50B H -0.258493 0.023287 0.173513 0.128 Uiso 0.490(9) 1 calc GR . P B 1 H50C H -0.334361 0.084800 0.108547 0.128 Uiso 0.490(9) 1 calc GR . P B 1 C51A C 1.0489(7) 0.2002(6) 0.3468(4) 0.0463(8) Uani 0.637(3) 1 d D . P C 1 C52A C 1.1298(5) 0.1736(7) 0.4085(3) 0.1021(19) Uani 0.637(3) 1 d D . P C 1 H52A H 1.087551 0.124478 0.438234 0.153 Uiso 0.637(3) 1 calc GR . P C 1 H52B H 1.126283 0.245529 0.426324 0.153 Uiso 0.637(3) 1 calc GR . P C 1 H52C H 1.228113 0.133625 0.400760 0.153 Uiso 0.637(3) 1 calc GR . P C 1 C53A C 1.1249(5) 0.2706(4) 0.3019(3) 0.0712(13) Uani 0.637(3) 1 d D . P C 1 H53A H 1.219735 0.223810 0.293499 0.107 Uiso 0.637(3) 1 calc GR . P C 1 H53B H 1.131738 0.338876 0.321134 0.107 Uiso 0.637(3) 1 calc GR . P C 1 H53C H 1.072278 0.294543 0.262089 0.107 Uiso 0.637(3) 1 calc GR . P C 1 C54A C 1.0546(5) 0.0903(5) 0.3180(4) 0.1037(19) Uani 0.637(3) 1 d D . P C 1 H54A H 1.017639 0.038333 0.348308 0.156 Uiso 0.637(3) 1 calc GR . P C 1 H54B H 1.152313 0.053068 0.307707 0.156 Uiso 0.637(3) 1 calc GR . P C 1 H54C H 0.997354 0.108315 0.279410 0.156 Uiso 0.637(3) 1 calc GR . P C 1 C47B C -0.3487(10) 0.1758(9) 0.1828(5) 0.0545(11) Uani 0.510(9) 1 d D . P B 2 C48B C -0.2797(8) 0.0739(8) 0.2304(5) 0.117(5) Uani 0.510(9) 1 d D . P B 2 H48D H -0.246529 0.102149 0.266986 0.175 Uiso 0.510(9) 1 calc R . P B 2 H48E H -0.348646 0.030683 0.244316 0.175 Uiso 0.510(9) 1 calc R . P B 2 H48F H -0.199759 0.023434 0.210486 0.175 Uiso 0.510(9) 1 calc R . P B 2 C49B C -0.4765(8) 0.2483(7) 0.2153(5) 0.099(4) Uani 0.510(9) 1 d D . P B 2 H49D H -0.445332 0.275814 0.252600 0.148 Uiso 0.510(9) 1 calc R . P B 2 H49E H -0.524070 0.314255 0.185819 0.148 Uiso 0.510(9) 1 calc R . P B 2 H49F H -0.541818 0.201232 0.228233 0.148 Uiso 0.510(9) 1 calc R . P B 2 C50B C -0.4015(13) 0.1349(13) 0.1253(5) 0.122(5) Uani 0.510(9) 1 d D . P B 2 H50D H -0.445247 0.201552 0.095480 0.183 Uiso 0.510(9) 1 calc R . P B 2 H50E H -0.322189 0.084806 0.104845 0.183 Uiso 0.510(9) 1 calc R . P B 2 H50F H -0.471076 0.092054 0.138674 0.183 Uiso 0.510(9) 1 calc R . P B 2 C51B C 1.0565(13) 0.2105(11) 0.3503(6) 0.0463(8) Uani 0.363(3) 1 d D . P C 2 C52B C 1.0742(9) 0.1884(12) 0.2823(4) 0.1021(19) Uani 0.363(3) 1 d D . P C 2 H52D H 1.019625 0.134747 0.273506 0.153 Uiso 0.363(3) 1 calc R . P C 2 H52E H 1.040605 0.261074 0.255323 0.153 Uiso 0.363(3) 1 calc R . P C 2 H52F H 1.174019 0.155040 0.273716 0.153 Uiso 0.363(3) 1 calc R . P C 2 C53B C 1.1089(9) 0.0970(8) 0.3893(5) 0.0712(13) Uani 0.363(3) 1 d D . P C 2 H53D H 1.054476 0.044044 0.379159 0.107 Uiso 0.363(3) 1 calc R . P C 2 H53E H 1.208649 0.064619 0.380103 0.107 Uiso 0.363(3) 1 calc R . P C 2 H53F H 1.097959 0.108037 0.434305 0.107 Uiso 0.363(3) 1 calc R . P C 2 C54B C 1.1388(9) 0.2923(8) 0.3654(7) 0.1037(19) Uani 0.363(3) 1 d D . P C 2 H54D H 1.125759 0.305543 0.410008 0.156 Uiso 0.363(3) 1 calc R . P C 2 H54E H 1.238917 0.259487 0.357201 0.156 Uiso 0.363(3) 1 calc R . P C 2 H54F H 1.105504 0.365521 0.338808 0.156 Uiso 0.363(3) 1 calc R . P C 2 C44B C 0.448(2) 0.333(2) -0.1445(9) 0.157(4) Uani 0.280(6) 1 d . . P A 3 H44D H 0.437184 0.413810 -0.138158 0.236 Uiso 0.280(6) 1 calc R . P A 3 H44E H 0.523130 0.309305 -0.175117 0.236 Uiso 0.280(6) 1 calc R . P A 3 H44F H 0.359311 0.323998 -0.160435 0.236 Uiso 0.280(6) 1 calc R . P A 3 C46B C 0.625(2) 0.278(2) -0.0565(10) 0.153(4) Uani 0.280(6) 1 d . . P A 3 H46D H 0.612436 0.359723 -0.051355 0.229 Uiso 0.280(6) 1 calc R . P A 3 H46E H 0.647750 0.232199 -0.015498 0.229 Uiso 0.280(6) 1 calc R . P A 3 H46F H 0.702556 0.253745 -0.086113 0.229 Uiso 0.280(6) 1 calc R . P A 3 C45B C 0.501(2) 0.1406(11) -0.0915(10) 0.097(2) Uani 0.280(6) 1 d . . P A 3 H45D H 0.524868 0.093803 -0.050765 0.146 Uiso 0.280(6) 1 calc R . P A 3 H45E H 0.412444 0.130686 -0.107232 0.146 Uiso 0.280(6) 1 calc R . P A 3 H45F H 0.576263 0.115993 -0.121914 0.146 Uiso 0.280(6) 1 calc R . P A 3 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 S 0.0547(4) 0.0287(3) 0.0391(3) -0.0040(2) 0.0014(3) -0.0091(3) N1 0.0423(11) 0.0454(11) 0.0352(10) -0.0162(9) 0.0101(8) -0.0205(9) N2 0.0327(10) 0.0453(11) 0.0320(10) 0.0025(8) 0.0020(8) -0.0043(8) C1 0.0383(12) 0.0327(12) 0.0295(11) -0.0039(9) 0.0077(10) -0.0080(10) C2 0.0480(14) 0.0377(13) 0.0378(13) 0.0001(10) -0.0047(11) -0.0007(11) C3 0.0464(14) 0.0513(15) 0.0333(12) -0.0050(11) -0.0060(11) -0.0112(12) C4 0.0367(12) 0.0405(13) 0.0297(11) -0.0075(10) 0.0063(10) -0.0136(10) C5 0.0325(11) 0.0305(11) 0.0329(11) -0.0037(9) 0.0067(9) -0.0097(9) C6 0.0275(11) 0.0297(11) 0.0277(10) -0.0040(9) 0.0070(9) -0.0088(9) C7 0.0287(11) 0.0304(11) 0.0289(11) -0.0054(9) 0.0091(9) -0.0093(9) C8 0.0321(11) 0.0303(11) 0.0336(11) -0.0068(9) 0.0075(9) -0.0083(9) C9 0.0312(12) 0.0410(13) 0.0327(12) -0.0016(10) 0.0035(9) -0.0086(10) C10 0.0461(14) 0.0473(14) 0.0399(13) -0.0103(11) -0.0034(11) -0.0168(11) C11 0.0552(15) 0.0372(13) 0.0410(13) -0.0095(11) -0.0009(11) -0.0179(11) C12 0.0378(12) 0.0332(12) 0.0324(11) -0.0041(9) 0.0069(10) -0.0127(10) C13 0.0318(12) 0.0414(13) 0.0303(11) -0.0072(10) -0.0005(9) -0.0118(10) C14 0.0483(14) 0.0387(13) 0.0436(13) -0.0102(11) 0.0090(11) -0.0171(11) C15 0.0475(14) 0.0438(14) 0.0485(14) -0.0047(11) 0.0142(12) -0.0188(11) C16 0.0408(14) 0.0429(14) 0.0458(14) -0.0036(11) 0.0123(11) -0.0092(11) C17 0.0371(13) 0.0366(13) 0.0482(13) -0.0077(11) 0.0061(11) -0.0077(10) C18 0.0293(11) 0.0387(12) 0.0310(11) -0.0028(9) -0.0009(9) -0.0097(10) C19 0.0336(12) 0.0362(12) 0.0378(12) -0.0072(10) 0.0038(10) -0.0125(10) C20 0.0304(12) 0.0404(13) 0.0321(11) -0.0046(10) -0.0001(9) -0.0102(10) C21 0.0383(13) 0.0446(14) 0.0504(14) -0.0112(11) 0.0035(11) -0.0157(11) C22 0.0352(13) 0.0555(15) 0.0445(13) -0.0087(12) 0.0041(11) -0.0167(11) C23 0.0366(13) 0.0545(15) 0.0463(14) -0.0095(12) 0.0089(11) -0.0114(11) C24 0.0432(14) 0.0418(13) 0.0433(13) -0.0106(11) 0.0085(11) -0.0123(11) C25 0.0324(12) 0.0428(13) 0.0291(11) -0.0047(10) -0.0008(9) -0.0141(10) C26 0.0641(18) 0.0700(18) 0.0683(18) -0.0325(15) 0.0281(14) -0.0381(15) C27 0.0406(14) 0.0545(16) 0.0597(16) 0.0109(13) 0.0083(12) -0.0073(12) C28 0.0322(12) 0.0399(13) 0.0298(11) -0.0053(10) -0.0003(9) -0.0117(10) C29 0.0396(13) 0.0397(13) 0.0383(12) -0.0001(10) 0.0031(10) -0.0106(10) C30 0.0375(13) 0.0459(14) 0.0415(13) 0.0008(11) 0.0055(10) -0.0166(11) C31 0.0354(12) 0.0482(14) 0.0398(13) -0.0038(11) 0.0037(10) -0.0153(11) C32 0.0362(13) 0.0395(13) 0.0429(13) 0.0021(10) 0.0021(10) -0.0094(10) C33 0.0313(12) 0.0406(13) 0.0333(11) -0.0058(10) 0.0019(9) -0.0143(10) C34 0.0331(12) 0.0385(12) 0.0382(12) -0.0026(10) 0.0052(10) -0.0115(10) C35 0.0328(12) 0.0414(13) 0.0336(11) -0.0070(10) 0.0014(9) -0.0143(10) C36 0.0420(13) 0.0419(13) 0.0411(13) -0.0033(10) 0.0058(11) -0.0160(11) C37 0.0420(14) 0.0486(15) 0.0429(13) -0.0116(11) 0.0116(11) -0.0160(11) C38 0.0408(14) 0.0519(15) 0.0516(15) -0.0104(12) 0.0146(12) -0.0071(12) C39 0.0417(14) 0.0461(14) 0.0447(14) -0.0014(11) 0.0068(11) -0.0043(11) C40 0.0308(12) 0.0464(13) 0.0311(11) -0.0060(10) 0.0021(9) -0.0135(10) C41 0.0423(14) 0.0618(17) 0.0536(15) 0.0133(13) 0.0101(12) -0.0052(12) C42 0.0505(15) 0.0549(16) 0.0697(17) -0.0229(14) 0.0217(13) -0.0254(13) C43 0.0534(16) 0.0436(15) 0.0723(18) -0.0084(14) 0.0308(14) -0.0079(13) C44A 0.087(4) 0.189(8) 0.119(5) 0.030(5) 0.057(4) 0.076(5) C45A 0.095(4) 0.066(3) 0.114(4) 0.000(3) 0.082(4) -0.004(3) C46A 0.150(7) 0.239(9) 0.131(5) -0.129(6) 0.106(5) -0.125(7) C55 0.0558(16) 0.0542(16) 0.0559(16) -0.0119(13) 0.0249(13) -0.0208(13) C56 0.097(3) 0.159(4) 0.067(2) 0.032(2) 0.030(2) -0.025(3) C57 0.095(2) 0.077(2) 0.100(3) -0.0209(19) 0.066(2) -0.0325(19) C58 0.140(3) 0.110(3) 0.120(3) -0.048(2) 0.078(3) -0.089(3) C47A 0.040(2) 0.068(3) 0.063(2) -0.0162(19) 0.0126(17) -0.026(2) C48A 0.101(8) 0.114(8) 0.060(4) -0.009(4) 0.023(4) -0.075(7) C49A 0.036(4) 0.102(6) 0.151(9) -0.026(6) -0.004(4) -0.030(4) C50A 0.106(8) 0.088(6) 0.095(8) -0.042(5) 0.054(6) -0.074(6) C51A 0.0333(15) 0.0539(19) 0.0507(17) 0.0043(14) 0.0045(12) -0.0138(13) C52A 0.040(2) 0.166(6) 0.077(3) 0.025(4) 0.000(2) -0.001(3) C53A 0.043(2) 0.070(3) 0.094(4) 0.007(3) 0.023(2) -0.012(2) C54A 0.055(3) 0.084(3) 0.182(6) -0.059(4) 0.049(3) -0.023(2) C47B 0.040(2) 0.068(3) 0.063(2) -0.0162(19) 0.0126(17) -0.026(2) C48B 0.076(5) 0.109(8) 0.157(9) 0.067(7) 0.011(5) -0.045(5) C49B 0.061(5) 0.110(6) 0.138(10) -0.041(7) 0.047(6) -0.038(5) C50B 0.108(10) 0.196(15) 0.110(9) -0.049(8) 0.031(6) -0.117(11) C51B 0.0333(15) 0.0539(19) 0.0507(17) 0.0043(14) 0.0045(12) -0.0138(13) C52B 0.040(2) 0.166(6) 0.077(3) 0.025(4) 0.000(2) -0.001(3) C53B 0.043(2) 0.070(3) 0.094(4) 0.007(3) 0.023(2) -0.012(2) C54B 0.055(3) 0.084(3) 0.182(6) -0.059(4) 0.049(3) -0.023(2) C44B 0.087(4) 0.189(8) 0.119(5) 0.030(5) 0.057(4) 0.076(5) C46B 0.150(7) 0.239(9) 0.131(5) -0.129(6) 0.106(5) -0.125(7) C45B 0.095(4) 0.066(3) 0.114(4) 0.000(3) 0.082(4) -0.004(3) _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 S C1 1.750(2) . ? S C12 1.748(2) . ? N1 C4 1.435(3) . ? N1 C13 1.402(3) . ? N1 C25 1.400(3) . ? N2 C9 1.435(3) . ? N2 C28 1.398(3) . ? N2 C40 1.406(3) . ? C1 C2 1.388(3) . ? C1 C6 1.398(3) . ? C2 C3 1.383(3) . ? C3 C4 1.387(3) . ? C4 C5 1.373(3) . ? C5 C6 1.390(3) . ? C6 C7 1.449(3) . ? C7 C8 1.390(3) . ? C7 C12 1.400(3) . ? C8 C9 1.378(3) . ? C9 C10 1.390(3) . ? C10 C11 1.376(3) . ? C11 C12 1.395(3) . ? C13 C14 1.389(3) . ? C13 C18 1.391(3) . ? C14 C15 1.377(3) . ? C15 C16 1.375(3) . ? C16 C17 1.391(3) . ? C16 C43 1.540(3) . ? C17 C18 1.393(3) . ? C18 C19 1.528(3) . ? C19 C20 1.532(3) . ? C19 C26 1.524(3) . ? C19 C27 1.539(3) . ? C20 C21 1.394(3) . ? C20 C25 1.390(3) . ? C21 C22 1.390(3) . ? C22 C23 1.382(3) . ? C22 C47A 1.533(10) . ? C22 C47B 1.539(10) . ? C23 C24 1.377(3) . ? C24 C25 1.390(3) . ? C28 C29 1.393(3) . ? C28 C33 1.396(3) . ? C29 C30 1.382(3) . ? C30 C31 1.380(3) . ? C31 C32 1.394(3) . ? C31 C51A 1.525(7) . ? C31 C51B 1.546(12) . ? C32 C33 1.392(3) . ? C33 C34 1.524(3) . ? C34 C35 1.528(3) . ? C34 C41 1.528(3) . ? C34 C42 1.542(3) . ? C35 C36 1.393(3) . ? C35 C40 1.395(3) . ? C36 C37 1.389(3) . ? C37 C38 1.380(3) . ? C37 C55 1.535(3) . ? C38 C39 1.376(3) . ? C39 C40 1.390(3) . ? C43 C44A 1.474(6) . ? C43 C45A 1.487(5) . ? C43 C46A 1.525(6) . ? C43 C44B 1.482(18) . ? C43 C46B 1.588(19) . ? C43 C45B 1.445(15) . ? C55 C56 1.536(4) . ? C55 C57 1.511(4) . ? C55 C58 1.500(4) . ? C47A C48A 1.526(11) . ? C47A C49A 1.521(10) . ? C47A C50A 1.516(11) . ? C51A C52A 1.513(8) . ? C51A C53A 1.521(8) . ? C51A C54A 1.513(8) . ? C47B C48B 1.527(10) . ? C47B C49B 1.530(10) . ? C47B C50B 1.520(11) . ? C51B C52B 1.498(12) . ? C51B C53B 1.498(12) . ? C51B C54B 1.497(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 C12 S C1 91.18(10) . . ? C13 N1 C4 119.27(17) . . ? C25 N1 C4 120.09(16) . . ? C25 N1 C13 120.63(17) . . ? C28 N2 C9 119.71(16) . . ? C28 N2 C40 120.84(17) . . ? C40 N2 C9 119.35(17) . . ? C2 C1 S 126.73(17) . . ? C2 C1 C6 120.97(19) . . ? C6 C1 S 112.29(15) . . ? C3 C2 C1 118.6(2) . . ? C2 C3 C4 120.7(2) . . ? C3 C4 N1 121.06(19) . . ? C5 C4 N1 118.38(19) . . ? C5 C4 C3 120.56(19) . . ? C4 C5 C6 119.85(19) . . ? C1 C6 C7 112.15(17) . . ? C5 C6 C1 119.22(18) . . ? C5 C6 C7 128.63(18) . . ? C8 C7 C6 128.69(18) . . ? C8 C7 C12 119.36(18) . . ? C12 C7 C6 111.89(18) . . ? C9 C8 C7 119.89(19) . . ? C8 C9 N2 118.40(19) . . ? C8 C9 C10 120.2(2) . . ? C10 C9 N2 121.34(19) . . ? C11 C10 C9 121.0(2) . . ? C10 C11 C12 118.7(2) . . ? C7 C12 S 112.45(15) . . ? C11 C12 S 126.84(17) . . ? C11 C12 C7 120.7(2) . . ? C14 C13 N1 120.15(19) . . ? C14 C13 C18 119.51(19) . . ? C18 C13 N1 120.34(18) . . ? C15 C14 C13 120.9(2) . . ? C16 C15 C14 121.6(2) . . ? C15 C16 C17 116.7(2) . . ? C15 C16 C43 121.9(2) . . ? C17 C16 C43 121.4(2) . . ? C16 C17 C18 123.7(2) . . ? C13 C18 C17 117.61(19) . . ? C13 C18 C19 120.99(18) . . ? C17 C18 C19 121.21(19) . . ? C18 C19 C20 110.05(17) . . ? C18 C19 C27 107.82(17) . . ? C20 C19 C27 107.19(17) . . ? C26 C19 C18 111.65(18) . . ? C26 C19 C20 110.94(18) . . ? C26 C19 C27 109.0(2) . . ? C21 C20 C19 120.89(19) . . ? C25 C20 C19 121.16(18) . . ? C25 C20 C21 117.58(19) . . ? C22 C21 C20 123.9(2) . . ? C21 C22 C47A 125.1(5) . . ? C21 C22 C47B 119.1(4) . . ? C23 C22 C21 116.5(2) . . ? C23 C22 C47A 118.4(5) . . ? C23 C22 C47B 124.2(4) . . ? C24 C23 C22 121.6(2) . . ? C23 C24 C25 120.8(2) . . ? C20 C25 N1 120.02(18) . . ? C20 C25 C24 119.65(19) . . ? C24 C25 N1 120.34(19) . . ? C29 C28 N2 120.49(19) . . ? C29 C28 C33 119.28(19) . . ? C33 C28 N2 120.23(18) . . ? C30 C29 C28 120.8(2) . . ? C31 C30 C29 121.8(2) . . ? C30 C31 C32 116.4(2) . . ? C30 C31 C51A 123.4(3) . . ? C30 C31 C51B 120.7(5) . . ? C32 C31 C51A 120.2(3) . . ? C32 C31 C51B 122.7(5) . . ? C33 C32 C31 123.8(2) . . ? C28 C33 C34 120.96(18) . . ? C32 C33 C28 117.88(18) . . ? C32 C33 C34 120.86(19) . . ? C33 C34 C35 110.85(17) . . ? C33 C34 C41 110.41(17) . . ? C33 C34 C42 107.50(17) . . ? C35 C34 C41 111.03(18) . . ? C35 C34 C42 107.58(18) . . ? C41 C34 C42 109.4(2) . . ? C36 C35 C34 121.19(19) . . ? C36 C35 C40 117.69(19) . . ? C40 C35 C34 120.95(18) . . ? C37 C36 C35 124.0(2) . . ? C36 C37 C55 120.8(2) . . ? C38 C37 C36 116.3(2) . . ? C38 C37 C55 122.9(2) . . ? C39 C38 C37 121.7(2) . . ? C38 C39 C40 121.1(2) . . ? C35 C40 N2 120.32(19) . . ? C39 C40 N2 120.5(2) . . ? C39 C40 C35 119.13(19) . . ? C16 C43 C46B 105.5(5) . . ? C44A C43 C16 109.7(3) . . ? C44A C43 C45A 109.2(4) . . ? C44A C43 C46A 109.2(5) . . ? C45A C43 C16 113.7(2) . . ? C45A C43 C46A 105.2(4) . . ? C46A C43 C16 109.7(3) . . ? C44B C43 C16 108.3(6) . . ? C44B C43 C46B 109.4(13) . . ? C45B C43 C16 112.5(5) . . ? C45B C43 C44B 110.6(12) . . ? C45B C43 C46B 110.5(11) . . ? C37 C55 C56 109.4(2) . . ? C57 C55 C37 112.3(2) . . ? C57 C55 C56 107.0(3) . . ? C58 C55 C37 109.9(2) . . ? C58 C55 C56 108.5(3) . . ? C58 C55 C57 109.7(3) . . ? C48A C47A C22 107.7(7) . . ? C49A C47A C22 109.6(7) . . ? C49A C47A C48A 112.1(9) . . ? C50A C47A C22 111.4(8) . . ? C50A C47A C48A 107.0(8) . . ? C50A C47A C49A 109.0(8) . . ? C52A C51A C31 107.8(5) . . ? C52A C51A C53A 106.6(5) . . ? C53A C51A C31 113.1(5) . . ? C54A C51A C31 111.5(5) . . ? C54A C51A C52A 110.3(6) . . ? C54A C51A C53A 107.3(5) . . ? C48B C47B C22 111.8(7) . . ? C48B C47B C49B 107.2(8) . . ? C49B C47B C22 111.4(7) . . ? C50B C47B C22 107.7(8) . . ? C50B C47B C48B 110.9(9) . . ? C50B C47B C49B 107.8(9) . . ? C52B C51B C31 106.9(8) . . ? C52B C51B C53B 107.2(10) . . ? C53B C51B C31 112.5(9) . . ? C54B C51B C31 109.3(8) . . ? C54B C51B C52B 110.8(11) . . ? C54B C51B C53B 110.1(10) . . ? _shelx_res_file ; TITL 17srv366 in P-1 #2 18srv436.res created by SHELXL-2018/3 at 23:31:53 on 11-Oct-2018 REM reset to P-1 #2 CELL 0.71073 9.8347 12.107 21.2839 83.6588 88.4755 74.8909 ZERR 2 0.0004 0.0005 0.0009 0.0019 0.002 0.0019 LATT 1 SFAC C H N S UNIT 116 132 4 2 SADI C49B C47B C48B C47B C50B C47B C48A C47A C49A C47A C50A C47A SADI C54A C51A C53B C51B C52A C51A C54B C51B C44A H44c C52B C51B C53A C51A SADI C51A C31 C51B C31 SADI C47B C22 C47A C22 EADP C51A C51B EADP C52B C52A EADP C53A C53B EADP C54A C54B EADP C47A C47B EADP C45B C45A EADP C44A C44B EADP C46B C46A L.S. 7 PLAN 7 SIZE 0.209 0.281 0.523 TEMP -73.15 BOND fmap 2 acta OMIT -3 50 OMIT 1 0 0 REM REM REM WGHT 0.059100 0.928700 EXTI 0.007346 FVAR 0.22738 0.49016 0.63652 0.07406 0.06667 0.06942 0.06596 FVAR 0.18069 0.14842 0.15227 0.72035 S 4 0.131727 0.815954 0.228754 11.00000 0.05472 0.02866 = 0.03913 -0.00400 0.00137 -0.00906 N1 3 0.066342 0.419338 0.103219 11.00000 0.04232 0.04544 = 0.03517 -0.01618 0.01005 -0.02054 N2 3 0.477261 0.433088 0.400908 11.00000 0.03270 0.04529 = 0.03201 0.00255 0.00203 -0.00431 C1 1 0.096162 0.708173 0.188424 11.00000 0.03827 0.03267 = 0.02954 -0.00392 0.00771 -0.00803 C2 1 0.007964 0.723822 0.136561 11.00000 0.04803 0.03772 = 0.03783 0.00009 -0.00474 -0.00067 AFIX 43 H2 2 -0.043677 0.798777 0.120158 11.00000 -1.20000 AFIX 0 C3 1 -0.003226 0.628071 0.109237 11.00000 0.04638 0.05127 = 0.03326 -0.00503 -0.00601 -0.01122 AFIX 43 H3 2 -0.063803 0.637321 0.073934 11.00000 -1.20000 AFIX 0 C4 1 0.073031 0.518718 0.132821 11.00000 0.03671 0.04052 = 0.02966 -0.00755 0.00633 -0.01360 C5 1 0.157788 0.503161 0.185023 11.00000 0.03246 0.03048 = 0.03287 -0.00371 0.00666 -0.00971 AFIX 43 H5 2 0.207758 0.427806 0.201582 11.00000 -1.20000 AFIX 0 C6 1 0.170304 0.597939 0.213586 11.00000 0.02747 0.02971 = 0.02774 -0.00399 0.00699 -0.00877 C7 1 0.254414 0.600621 0.267992 11.00000 0.02868 0.03037 = 0.02888 -0.00536 0.00914 -0.00928 C8 1 0.333469 0.508917 0.307800 11.00000 0.03207 0.03029 = 0.03360 -0.00684 0.00752 -0.00832 AFIX 43 H8 2 0.339751 0.432098 0.299779 11.00000 -1.20000 AFIX 0 C9 1 0.402718 0.529628 0.358920 11.00000 0.03117 0.04098 = 0.03266 -0.00165 0.00349 -0.00858 C10 1 0.396815 0.641882 0.369886 11.00000 0.04608 0.04733 = 0.03991 -0.01029 -0.00343 -0.01678 AFIX 43 H10 2 0.447747 0.655034 0.404388 11.00000 -1.20000 AFIX 0 C11 1 0.318384 0.734199 0.331560 11.00000 0.05516 0.03724 = 0.04100 -0.00946 -0.00087 -0.01795 AFIX 43 H11 2 0.314150 0.810708 0.339508 11.00000 -1.20000 AFIX 0 C12 1 0.245161 0.713314 0.280785 11.00000 0.03781 0.03315 = 0.03242 -0.00408 0.00695 -0.01273 C13 1 0.165273 0.380209 0.056623 11.00000 0.03183 0.04143 = 0.03029 -0.00718 -0.00045 -0.01180 C14 1 0.240258 0.452985 0.026071 11.00000 0.04833 0.03873 = 0.04360 -0.01023 0.00900 -0.01714 AFIX 43 H14 2 0.222584 0.529859 0.036320 11.00000 -1.20000 AFIX 0 C15 1 0.339846 0.415248 -0.018861 11.00000 0.04751 0.04379 = 0.04850 -0.00468 0.01420 -0.01883 AFIX 43 H15 2 0.389377 0.466871 -0.039163 11.00000 -1.20000 AFIX 0 C16 1 0.369324 0.304586 -0.035052 11.00000 0.04083 0.04288 = 0.04582 -0.00365 0.01232 -0.00924 C17 1 0.291918 0.233447 -0.004527 11.00000 0.03714 0.03658 = 0.04820 -0.00771 0.00613 -0.00770 AFIX 43 H17 2 0.310320 0.156682 -0.015026 11.00000 -1.20000 AFIX 0 C18 1 0.188940 0.268431 0.040568 11.00000 0.02933 0.03866 = 0.03104 -0.00282 -0.00090 -0.00970 C19 1 0.113342 0.184210 0.075198 11.00000 0.03356 0.03615 = 0.03780 -0.00716 0.00375 -0.01249 C20 1 -0.021805 0.250366 0.105806 11.00000 0.03038 0.04038 = 0.03207 -0.00461 -0.00015 -0.01019 C21 1 -0.127876 0.196903 0.124911 11.00000 0.03835 0.04463 = 0.05038 -0.01122 0.00350 -0.01570 AFIX 43 H21 2 -0.119387 0.121614 0.113672 11.00000 -1.20000 AFIX 0 C22 1 -0.245288 0.247241 0.159422 11.00000 0.03523 0.05549 = 0.04452 -0.00870 0.00407 -0.01671 C23 1 -0.253965 0.356649 0.175046 11.00000 0.03661 0.05448 = 0.04631 -0.00952 0.00891 -0.01141 AFIX 43 H23 2 -0.331787 0.393745 0.199194 11.00000 -1.20000 AFIX 0 C24 1 -0.152542 0.413178 0.156459 11.00000 0.04325 0.04177 = 0.04327 -0.01058 0.00847 -0.01228 AFIX 43 H24 2 -0.162184 0.488793 0.167438 11.00000 -1.20000 AFIX 0 C25 1 -0.036173 0.361031 0.121823 11.00000 0.03242 0.04282 = 0.02915 -0.00470 -0.00081 -0.01407 C26 1 0.081694 0.102775 0.031289 11.00000 0.06413 0.06996 = 0.06834 -0.03245 0.02805 -0.03808 AFIX 137 H26A 2 0.042173 0.045158 0.055822 11.00000 41.00000 H26B 2 0.168880 0.064132 0.010796 11.00000 41.00000 H26C 2 0.013672 0.146653 -0.000993 11.00000 41.00000 AFIX 0 C27 1 0.210259 0.113355 0.128955 11.00000 0.04057 0.05448 = 0.05967 0.01092 0.00828 -0.00729 AFIX 137 H27A 2 0.228736 0.165031 0.158106 11.00000 51.00000 H27B 2 0.299404 0.071710 0.111158 11.00000 51.00000 H27C 2 0.164352 0.058205 0.151833 11.00000 51.00000 AFIX 0 C28 1 0.615537 0.375394 0.386871 11.00000 0.03220 0.03993 = 0.02977 -0.00534 -0.00031 -0.01167 C29 1 0.694170 0.426619 0.342937 11.00000 0.03956 0.03973 = 0.03832 -0.00011 0.00312 -0.01055 AFIX 43 H29 2 0.652406 0.500338 0.321491 11.00000 -1.20000 AFIX 0 C30 1 0.832204 0.371503 0.330165 11.00000 0.03750 0.04592 = 0.04145 0.00081 0.00546 -0.01663 AFIX 43 H30 2 0.883202 0.408016 0.299695 11.00000 -1.20000 AFIX 0 C31 1 0.897946 0.264848 0.360488 11.00000 0.03540 0.04819 = 0.03982 -0.00379 0.00367 -0.01526 C32 1 0.816466 0.214444 0.403446 11.00000 0.03617 0.03951 = 0.04294 0.00213 0.00209 -0.00943 AFIX 43 H32 2 0.858851 0.140587 0.424583 11.00000 -1.20000 AFIX 0 C33 1 0.676601 0.266004 0.417190 11.00000 0.03130 0.04056 = 0.03326 -0.00577 0.00194 -0.01425 C34 1 0.588845 0.200072 0.458646 11.00000 0.03313 0.03845 = 0.03824 -0.00264 0.00516 -0.01153 C35 1 0.458470 0.282454 0.483545 11.00000 0.03283 0.04141 = 0.03358 -0.00700 0.00143 -0.01427 C36 1 0.380617 0.246349 0.533584 11.00000 0.04197 0.04192 = 0.04106 -0.00326 0.00581 -0.01604 AFIX 43 H36 2 0.413392 0.169776 0.553124 11.00000 -1.20000 AFIX 0 C37 1 0.257965 0.315477 0.556663 11.00000 0.04197 0.04860 = 0.04294 -0.01162 0.01160 -0.01601 C38 1 0.213795 0.426203 0.527150 11.00000 0.04076 0.05190 = 0.05159 -0.01044 0.01459 -0.00713 AFIX 43 H38 2 0.131463 0.476963 0.541962 11.00000 -1.20000 AFIX 0 C39 1 0.285972 0.464932 0.476823 11.00000 0.04174 0.04615 = 0.04472 -0.00141 0.00676 -0.00427 AFIX 43 H39 2 0.252333 0.541578 0.457507 11.00000 -1.20000 AFIX 0 C40 1 0.407299 0.393795 0.453759 11.00000 0.03076 0.04644 = 0.03111 -0.00596 0.00206 -0.01351 C41 1 0.677981 0.125180 0.512953 11.00000 0.04234 0.06177 = 0.05363 0.01334 0.01006 -0.00519 AFIX 137 H41A 2 0.752371 0.065252 0.495917 11.00000 61.00000 H41B 2 0.618117 0.089217 0.541451 11.00000 61.00000 H41C 2 0.720626 0.173035 0.536322 11.00000 61.00000 AFIX 0 C42 1 0.537878 0.122575 0.416799 11.00000 0.05048 0.05488 = 0.06971 -0.02286 0.02170 -0.02540 AFIX 137 H42A 2 0.480142 0.170501 0.382100 11.00000 71.00000 H42B 2 0.481628 0.078391 0.442273 11.00000 71.00000 H42C 2 0.619476 0.069587 0.399431 11.00000 71.00000 AFIX 0 C43 1 0.484387 0.260309 -0.083454 11.00000 0.05341 0.04361 = 0.07226 -0.00840 0.03080 -0.00786 PART 1 C44A 1 0.607033 0.180235 -0.050502 111.00000 0.08711 0.18911 = 0.11919 0.02989 0.05651 0.07558 AFIX 137 H44A 2 0.637595 0.217408 -0.016810 111.00000 -1.50000 H44B 2 0.684099 0.159281 -0.080650 111.00000 -1.50000 H44C 2 0.580963 0.110767 -0.032132 111.00000 -1.50000 AFIX 0 C45A 1 0.531240 0.353403 -0.122298 111.00000 0.09511 0.06609 = 0.11361 0.00013 0.08183 -0.00371 AFIX 137 H45A 2 0.450764 0.404844 -0.145833 111.00000 -1.50000 H45B 2 0.603867 0.319491 -0.152056 111.00000 -1.50000 H45C 2 0.569969 0.397232 -0.094607 111.00000 -1.50000 AFIX 0 C46A 1 0.427051 0.197677 -0.130669 111.00000 0.14997 0.23930 = 0.13061 -0.12903 0.10624 -0.12512 AFIX 137 H46A 2 0.396142 0.133504 -0.108057 111.00000 -1.50000 H46B 2 0.501127 0.168058 -0.160802 111.00000 -1.50000 H46C 2 0.347028 0.251209 -0.153499 111.00000 -1.50000 AFIX 0 PART 0 C55 1 0.176371 0.268229 0.611072 11.00000 0.05578 0.05417 = 0.05593 -0.01185 0.02490 -0.02082 C56 1 0.277964 0.211459 0.665871 11.00000 0.09665 0.15850 = 0.06697 0.03159 0.03001 -0.02546 AFIX 137 H56A 2 0.349210 0.145873 0.651933 11.00000 81.00000 H56B 2 0.225241 0.184682 0.701466 11.00000 81.00000 H56C 2 0.324278 0.267591 0.679186 11.00000 81.00000 AFIX 0 C57 1 0.062569 0.361862 0.636882 11.00000 0.09516 0.07683 = 0.10008 -0.02090 0.06606 -0.03249 AFIX 137 H57A 2 0.104729 0.419611 0.651311 11.00000 91.00000 H57B 2 0.015851 0.328322 0.672466 11.00000 91.00000 H57C 2 -0.006686 0.398384 0.603610 11.00000 91.00000 AFIX 0 C58 1 0.112602 0.179172 0.589212 11.00000 0.13987 0.10995 = 0.12003 -0.04834 0.07754 -0.08896 AFIX 137 H58A 2 0.040625 0.215748 0.557077 11.00000 101.00000 H58B 2 0.069329 0.143472 0.625212 11.00000 101.00000 H58C 2 0.186199 0.120128 0.571068 11.00000 101.00000 AFIX 0 PART 1 C47A 1 -0.366149 0.192542 0.179117 21.00000 0.04040 0.06788 = 0.06326 -0.01617 0.01265 -0.02554 C48A 1 -0.366015 0.171974 0.251137 21.00000 0.10079 0.11442 = 0.05981 -0.00857 0.02281 -0.07450 AFIX 137 H48A 2 -0.439974 0.134025 0.265034 21.00000 -1.50000 H48B 2 -0.383733 0.245829 0.268781 21.00000 -1.50000 H48C 2 -0.274251 0.122854 0.265859 21.00000 -1.50000 AFIX 0 C49A 1 -0.504674 0.271234 0.153235 21.00000 0.03623 0.10218 = 0.15111 -0.02610 -0.00402 -0.02996 AFIX 137 H49A 2 -0.582612 0.239320 0.168907 21.00000 -1.50000 H49B 2 -0.503111 0.277308 0.106938 21.00000 -1.50000 H49C 2 -0.517531 0.347766 0.167188 21.00000 -1.50000 AFIX 0 C50A 1 -0.344102 0.076190 0.154647 21.00000 0.10595 0.08754 = 0.09493 -0.04211 0.05364 -0.07426 AFIX 137 H50A 2 -0.425205 0.045290 0.166067 21.00000 -1.50000 H50B 2 -0.258493 0.023287 0.173513 21.00000 -1.50000 H50C 2 -0.334361 0.084800 0.108547 21.00000 -1.50000 AFIX 0 C51A 1 1.048947 0.200203 0.346780 31.00000 0.03332 0.05388 = 0.05066 0.00431 0.00454 -0.01375 C52A 1 1.129846 0.173618 0.408455 31.00000 0.04009 0.16556 = 0.07736 0.02491 -0.00049 -0.00083 AFIX 137 H52A 2 1.087551 0.124478 0.438234 31.00000 -1.50000 H52B 2 1.126283 0.245529 0.426324 31.00000 -1.50000 H52C 2 1.228113 0.133625 0.400760 31.00000 -1.50000 AFIX 0 C53A 1 1.124928 0.270617 0.301885 31.00000 0.04317 0.07000 = 0.09421 0.00662 0.02267 -0.01216 AFIX 137 H53A 2 1.219735 0.223810 0.293499 31.00000 -1.50000 H53B 2 1.131738 0.338876 0.321134 31.00000 -1.50000 H53C 2 1.072278 0.294543 0.262089 31.00000 -1.50000 AFIX 0 C54A 1 1.054557 0.090306 0.318019 31.00000 0.05516 0.08436 = 0.18179 -0.05859 0.04855 -0.02271 AFIX 137 H54A 2 1.017639 0.038333 0.348308 31.00000 -1.50000 H54B 2 1.152313 0.053068 0.307707 31.00000 -1.50000 H54C 2 0.997354 0.108315 0.279410 31.00000 -1.50000 AFIX 0 PART 0 PART 2 C47B 1 -0.348692 0.175757 0.182786 -21.00000 0.04040 0.06788 = 0.06326 -0.01617 0.01265 -0.02554 C48B 1 -0.279727 0.073877 0.230411 -21.00000 0.07610 0.10894 = 0.15678 0.06671 0.01087 -0.04456 AFIX 33 H48D 2 -0.246529 0.102149 0.266986 -21.00000 -1.50000 H48E 2 -0.348646 0.030683 0.244316 -21.00000 -1.50000 H48F 2 -0.199759 0.023434 0.210486 -21.00000 -1.50000 AFIX 0 C49B 1 -0.476461 0.248283 0.215280 -21.00000 0.06059 0.10992 = 0.13841 -0.04053 0.04706 -0.03765 AFIX 33 H49D 2 -0.445332 0.275814 0.252600 -21.00000 -1.50000 H49E 2 -0.524070 0.314255 0.185819 -21.00000 -1.50000 H49F 2 -0.541818 0.201232 0.228233 -21.00000 -1.50000 AFIX 0 C50B 1 -0.401489 0.134915 0.125346 -21.00000 0.10808 0.19643 = 0.11003 -0.04925 0.03142 -0.11701 AFIX 33 H50D 2 -0.445247 0.201552 0.095480 -21.00000 -1.50000 H50E 2 -0.322189 0.084806 0.104845 -21.00000 -1.50000 H50F 2 -0.471076 0.092054 0.138674 -21.00000 -1.50000 AFIX 0 C51B 1 1.056517 0.210473 0.350331 -31.00000 0.03332 0.05388 = 0.05066 0.00431 0.00454 -0.01375 C52B 1 1.074222 0.188428 0.282344 -31.00000 0.04009 0.16556 = 0.07736 0.02491 -0.00049 -0.00083 AFIX 33 H52D 2 1.019625 0.134747 0.273506 -31.00000 -1.50000 H52E 2 1.040605 0.261074 0.255323 -31.00000 -1.50000 H52F 2 1.174019 0.155040 0.273716 -31.00000 -1.50000 AFIX 0 C53B 1 1.108934 0.096978 0.389349 -31.00000 0.04317 0.07000 = 0.09421 0.00662 0.02267 -0.01216 AFIX 33 H53D 2 1.054476 0.044044 0.379159 -31.00000 -1.50000 H53E 2 1.208649 0.064619 0.380103 -31.00000 -1.50000 H53F 2 1.097959 0.108037 0.434305 -31.00000 -1.50000 AFIX 0 C54B 1 1.138777 0.292323 0.365387 -31.00000 0.05516 0.08436 = 0.18179 -0.05859 0.04855 -0.02271 AFIX 33 H54D 2 1.125759 0.305543 0.410008 -31.00000 -1.50000 H54E 2 1.238917 0.259487 0.357201 -31.00000 -1.50000 H54F 2 1.105504 0.365521 0.338808 -31.00000 -1.50000 AFIX 0 PART 0 PART 3 C44B 1 0.447913 0.333015 -0.144459 -111.00000 0.08711 0.18911 = 0.11919 0.02989 0.05651 0.07558 AFIX 33 H44D 2 0.437184 0.413810 -0.138158 -111.00000 -1.50000 H44E 2 0.523130 0.309305 -0.175117 -111.00000 -1.50000 H44F 2 0.359311 0.323998 -0.160435 -111.00000 -1.50000 AFIX 0 C46B 1 0.625264 0.278207 -0.056528 -111.00000 0.14997 0.23930 = 0.13061 -0.12903 0.10624 -0.12512 AFIX 33 H46D 2 0.612436 0.359723 -0.051355 -111.00000 -1.50000 H46E 2 0.647750 0.232199 -0.015498 -111.00000 -1.50000 H46F 2 0.702556 0.253745 -0.086113 -111.00000 -1.50000 AFIX 0 C45B 1 0.500812 0.140563 -0.091487 -111.00000 0.09511 0.06609 = 0.11361 0.00013 0.08183 -0.00371 AFIX 33 H45D 2 0.524868 0.093803 -0.050765 -111.00000 -1.50000 H45E 2 0.412444 0.130686 -0.107232 -111.00000 -1.50000 H45F 2 0.576263 0.115993 -0.121914 -111.00000 -1.50000 AFIX 0 HKLF 4 REM 17srv366 in P-1 #2 REM wR2 = 0.1372, GooF = S = 1.030, Restrained GooF = 1.254 for all data REM R1 = 0.0513 for 5863 Fo > 4sig(Fo) and 0.0842 for all 8540 data REM 628 parameters refined using 38 restraints END WGHT 0.0591 0.9287 REM Highest difference peak 0.277, deepest hole -0.209, 1-sigma level 0.038 Q1 1 0.0020 0.2826 0.5721 11.00000 0.05 0.28 Q2 1 1.2049 0.2024 0.2838 11.00000 0.05 0.25 Q3 1 1.1674 0.2740 0.3486 11.00000 0.05 0.23 Q4 1 0.6418 0.2324 -0.0740 11.00000 0.05 0.23 Q5 1 0.2297 0.1418 0.6288 11.00000 0.05 0.22 Q6 1 0.5015 0.0825 -0.0705 11.00000 0.05 0.20 Q7 1 0.1750 0.3281 0.6674 11.00000 0.05 0.20 ; _shelx_res_checksum 40776 _olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems' _olex2_submission_special_instructions 'No special instructions were received' #===END _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_DtBuAcDBT_17s366 _database_code_depnum_ccdc_archive 'CCDC 1901571' loop_ _audit_author_name _audit_author_address 'Andrei S. Batsanov' ;Durham University United Kingdom ; _audit_update_record ; 2019-03-06 deposited with the CCDC. 2019-10-14 downloaded from the CCDC. ; _audit_creation_date 2018-10-11 _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 'C58 H66 N2 S' _chemical_formula_sum 'C58 H66 N2 S' _chemical_formula_weight 823.18 _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' 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 9.7054(5) _cell_length_b 12.0521(6) _cell_length_c 21.3945(10) _cell_angle_alpha 83.6147(19) _cell_angle_beta 88.817(2) _cell_angle_gamma 74.1306(18) _cell_volume 2392.1(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9991 _cell_measurement_temperature 120 _cell_measurement_theta_max 27.21 _cell_measurement_theta_min 2.37 _shelx_estimated_absorpt_T_max 0.978 _shelx_estimated_absorpt_T_min 0.946 _exptl_absorpt_coefficient_mu 0.107 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.9573 _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 0.1108 before and 0.0453 after correction. The Ratio of minimum to maximum transmission is 0.9573. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.143 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description parallelepiped _exptl_crystal_F_000 888 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 0.00 1.00 0.0650 -1.00 0.00 -1.00 0.1250 -2.00 -1.00 2.00 0.2200 0.00 1.00 -2.00 0.1520 0.00 -1.00 2.00 0.1800 0.00 -2.00 -1.00 0.1050 0.00 2.00 1.00 0.0990 -1.00 2.00 -1.00 0.1220 0.00 -1.00 -1.00 0.0990 0.00 1.00 2.00 0.1550 0.00 -2.00 1.00 0.1440 _exptl_crystal_size_max 0.523 _exptl_crystal_size_mid 0.281 _exptl_crystal_size_min 0.209 _exptl_special_details ; Data were collected in shutterless mode. Full sphere of reciprocal space was nominally covered by 4 runs of 340 narrow-frame \w-scans (scan width 0.5\%, 5s exposure), every run at a different \f angle. Two runs of 358 \f-scans (scan width 1\%, 1s 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 0.0377 _diffrn_reflns_av_unetI/netI 0.0386 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 37697 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_min 2.374 _diffrn_ambient_temperature 120 _diffrn_detector_area_resol_mean 10.4 _diffrn_detector_type 'Bruker PHOTON 100 CMOS' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 '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 6465 _reflns_number_total 8436 _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 v8.38A (Bruker, 2017)' _computing_data_collection 'APEX3 v.2016.1-0 (Bruker, 2016)' _computing_data_reduction 'SAINT v8.38A (Bruker, 2017)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL 2018/2 multi-CPU (Sheldrick, 2015)' _computing_structure_solution 'ShelXS 2013/1 (Sheldrick, 2008)' _refine_diff_density_max 0.340 _refine_diff_density_min -0.247 _refine_diff_density_rms 0.038 _refine_ls_extinction_coef 0.0053(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, 2015)' _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 631 _refine_ls_number_reflns 8436 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0652 _refine_ls_R_factor_gt 0.0444 _refine_ls_restrained_S_all 1.256 _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^)+(0.0460P)^2^+1.2212P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1053 _refine_ls_wR_factor_ref 0.1145 _refine_special_details ; t-Bu group C(43)Me~3~ is rotationally disordered between two orientations, A and B, with occupancies 0.886(5) and 0.114(5), respectively. The C(43) atom is not disordered. t-Bu group C(47)Me~3~ is disordered [including C(47)] by rotation and tilt, between two orientations, A and B, with occupancies 0.729(5) and 0.271(5), respectively. t-Bu group C(51)Me~3~ is disordered [including C(51)] by rotation and tilt, between two orientations, A and B, with occupancies 0.708(2) and 0.292(2), respectively. All ordered methyl groups were refined as rigid bodies rotating around C---C bonds, with a common refined U for three H atoms. Major components of disordered methyl groups were refined likewise, with U of H atoms fixed to 1.5 U(eq) of the carbon atoms. 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 C49B-C47B \\sim C48B-C47B \\sim C50B-C47B \\sim C48A-C47A \\sim C49A-C47A \\sim C50A-C47A with sigma of 0.02 C54A-C51A \\sim C53B-C51B \\sim C52A-C51A \\sim C54B-C51B \\sim C44A-H44C \\sim C52B-C51B \\sim C53A- C51A with sigma of 0.02 C51A-C31 \\sim C51B-C31 with sigma of 0.02 C47B-C22 \\sim C47A-C22 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(C51A) = Uanis(C51B) Uanis(C52B) = Uanis(C52A) Uanis(C53A) = Uanis(C53B) Uanis(C54A) = Uanis(C54B) Uanis(C47A) = Uanis(C47B) 4. Others Sof(C44B)=Sof(H44D)=Sof(H44E)=Sof(H44F)=Sof(C46B)=Sof(H46D)=Sof(H46E)= Sof(H46F)=Sof(C45B)=Sof(H45D)=Sof(H45E)=Sof(H45F)=1-FVAR(1) Sof(C44A)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C45A)=Sof(H45A)=Sof(H45B)= Sof(H45C)=Sof(C46A)=Sof(H46A)=Sof(H46B)=Sof(H46C)=FVAR(1) Sof(C47B)=Sof(C48B)=Sof(H48D)=Sof(H48E)=Sof(H48F)=Sof(C49B)=Sof(H49D)= Sof(H49E)=Sof(H49F)=Sof(C50B)=Sof(H50D)=Sof(H50E)=Sof(H50F)=1-FVAR(2) Sof(C47A)=Sof(C48A)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C49A)=Sof(H49A)= Sof(H49B)=Sof(H49C)=Sof(C50A)=Sof(H50A)=Sof(H50B)=Sof(H50C)=FVAR(2) Sof(C51B)=Sof(C52B)=Sof(H52D)=Sof(H52E)=Sof(H52F)=Sof(C53B)=Sof(H53D)= Sof(H53E)=Sof(H53F)=Sof(C54B)=Sof(H54D)=Sof(H54E)=Sof(H54F)=1-FVAR(3) Sof(C51A)=Sof(C52A)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C53A)=Sof(H53A)= Sof(H53B)=Sof(H53C)=Sof(C54A)=Sof(H54A)=Sof(H54B)=Sof(H54C)=FVAR(3) Uiso(H26A)=Uiso(H26B)=Uiso(H26C)=FVAR(4) Uiso(H27A)=Uiso(H27B)=Uiso(H27C)=FVAR(5) Uiso(H41A)=Uiso(H41B)=Uiso(H41C)=FVAR(6) Uiso(H42A)=Uiso(H42B)=Uiso(H42C)=FVAR(7) Uiso(H56A)=Uiso(H56B)=Uiso(H56C)=FVAR(8) Uiso(H57A)=Uiso(H57B)=Uiso(H57C)=FVAR(9) Uiso(H58A)=Uiso(H58B)=Uiso(H58C)=FVAR(10) 5.a Me refined with riding coordinates: C48B(H48D,H48E,H48F), C49B(H49D,H49E,H49F), C50B(H50D,H50E,H50F), C52B(H52D, H52E,H52F), C53B(H53D,H53E,H53F), C54B(H54D,H54E,H54F), C44B(H44D,H44E,H44F), C46B(H46D,H46E,H46F), C45B(H45D,H45E,H45F) 5.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C5(H5), C8(H8), C10(H10), C11(H11), C14(H14), C15(H15), C17(H17), C21(H21), C23(H23), C24(H24), C29(H29), C30(H30), C32(H32), C36(H36), C38(H38), C39(H39) 5.c Idealised Me refined as rotating group: C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C41(H41A,H41B,H41C), C42(H42A,H42B, H42C), C44A(H44A,H44B,H44C), C45A(H45A,H45B,H45C), C46A(H46A,H46B,H46C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C48A(H48A,H48B, H48C), C49A(H49A,H49B,H49C), C50A(H50A,H50B,H50C), C52A(H52A,H52B,H52C), C53A(H53A,H53B,H53C), C54A(H54A,H54B,H54C) ; _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 S S 0.12008(5) 0.82251(4) 0.22903(2) 0.02879(14) Uani 1 1 d . . . . . N1 N 0.05728(16) 0.42509(13) 0.10262(7) 0.0260(4) Uani 1 1 d . . . . . N2 N 0.47910(16) 0.43537(13) 0.40031(7) 0.0282(4) Uani 1 1 d . . . . . C1 C 0.08495(19) 0.71434(15) 0.18857(8) 0.0242(4) Uani 1 1 d . . . . . C2 C -0.0059(2) 0.73112(16) 0.13721(9) 0.0294(4) Uani 1 1 d . . . . . H2 H -0.059896 0.806979 0.121316 0.035 Uiso 1 1 calc R . . . . C3 C -0.0165(2) 0.63534(16) 0.10947(9) 0.0294(4) Uani 1 1 d . . . . . H3 H -0.078795 0.645428 0.074372 0.035 Uiso 1 1 calc R . . . . C4 C 0.06343(19) 0.52436(15) 0.13261(8) 0.0241(4) Uani 1 1 d . . . . . C5 C 0.15168(18) 0.50765(15) 0.18450(8) 0.0217(4) Uani 1 1 d . . . . . H5 H 0.204319 0.431452 0.200526 0.026 Uiso 1 1 calc R . . . . C6 C 0.16343(18) 0.60261(14) 0.21329(8) 0.0208(4) Uani 1 1 d . . . . . C7 C 0.24944(18) 0.60479(15) 0.26745(8) 0.0209(4) Uani 1 1 d . . . . . C8 C 0.33163(18) 0.51188(15) 0.30705(8) 0.0226(4) Uani 1 1 d . . . . . H8 H 0.339996 0.434474 0.298806 0.027 Uiso 1 1 calc R . . . . C9 C 0.40099(19) 0.53275(16) 0.35838(8) 0.0258(4) Uani 1 1 d . . . . . C10 C 0.3933(2) 0.64552(17) 0.36951(9) 0.0315(4) Uani 1 1 d . . . . . H10 H 0.444955 0.658398 0.403984 0.038 Uiso 1 1 calc R . . . . C11 C 0.3117(2) 0.73939(17) 0.33118(9) 0.0311(4) Uani 1 1 d . . . . . H11 H 0.305818 0.816495 0.339217 0.037 Uiso 1 1 calc R . . . . C12 C 0.23830(19) 0.71841(15) 0.28061(8) 0.0244(4) Uani 1 1 d . . . . . C13 C 0.16087(18) 0.38397(15) 0.05798(8) 0.0234(4) Uani 1 1 d . . . . . C14 C 0.2354(2) 0.45744(16) 0.02740(9) 0.0275(4) Uani 1 1 d . . . . . H14 H 0.213459 0.535821 0.036325 0.033 Uiso 1 1 calc R . . . . C15 C 0.3404(2) 0.41872(16) -0.01554(9) 0.0295(4) Uani 1 1 d . . . . . H15 H 0.388946 0.471045 -0.035913 0.035 Uiso 1 1 calc R . . . . C16 C 0.37668(19) 0.30458(16) -0.02962(9) 0.0281(4) Uani 1 1 d . . . . . C17 C 0.29902(19) 0.23314(15) 0.00080(9) 0.0260(4) Uani 1 1 d . . . . . H17 H 0.321964 0.154692 -0.008071 0.031 Uiso 1 1 calc R . . . . C18 C 0.18979(18) 0.26961(15) 0.04344(8) 0.0228(4) Uani 1 1 d . . . . . C19 C 0.11106(19) 0.18527(15) 0.07569(8) 0.0247(4) Uani 1 1 d . . . . . C20 C -0.02457(19) 0.25136(15) 0.10761(8) 0.0244(4) Uani 1 1 d . . . . . C21 C -0.12847(19) 0.19559(16) 0.12809(9) 0.0287(4) Uani 1 1 d . . . . . H21 H -0.116978 0.118800 0.118006 0.034 Uiso 1 1 calc R . . . . C22 C -0.24797(19) 0.24627(17) 0.16245(9) 0.0288(4) Uani 1 1 d D . . . . C23 C -0.2605(2) 0.35794(17) 0.17683(9) 0.0300(4) Uani 1 1 d . . . . . H23 H -0.339681 0.395055 0.200883 0.036 Uiso 1 1 calc R . . . . C24 C -0.16123(19) 0.41627(16) 0.15717(9) 0.0289(4) Uani 1 1 d . . . . . H24 H -0.173470 0.493088 0.167369 0.035 Uiso 1 1 calc R . . . . C25 C -0.04271(19) 0.36408(15) 0.12242(8) 0.0240(4) Uani 1 1 d . . . . . C26 C 0.0720(2) 0.11267(18) 0.02795(10) 0.0386(5) Uani 1 1 d . . . . . H26A H 0.030551 0.053852 0.049984 0.045(4) Uiso 1 1 calc GR . . . . H26B H 0.158406 0.074409 0.005833 0.045(4) Uiso 1 1 calc GR . . . . H26C H 0.002097 0.163321 -0.002483 0.045(4) Uiso 1 1 calc GR . . . . C27 C 0.2099(2) 0.10449(18) 0.12674(10) 0.0371(5) Uani 1 1 d . . . . . H27A H 0.229827 0.150274 0.158801 0.045(4) Uiso 1 1 calc GR . . . . H27B H 0.299998 0.064541 0.107726 0.045(4) Uiso 1 1 calc GR . . . . H27C H 0.162999 0.047102 0.146270 0.045(4) Uiso 1 1 calc GR . . . . C28 C 0.61940(19) 0.37668(15) 0.38577(8) 0.0243(4) Uani 1 1 d . . . . . C29 C 0.6965(2) 0.42837(16) 0.34164(9) 0.0276(4) Uani 1 1 d . . . . . H29 H 0.652487 0.503119 0.320704 0.033 Uiso 1 1 calc R . . . . C30 C 0.8361(2) 0.37259(16) 0.32786(9) 0.0277(4) Uani 1 1 d . . . . . H30 H 0.886042 0.409337 0.297121 0.033 Uiso 1 1 calc R . . . . C31 C 0.90518(19) 0.26419(16) 0.35783(9) 0.0281(4) Uani 1 1 d D . . . . C32 C 0.82515(19) 0.21341(16) 0.40116(9) 0.0291(4) Uani 1 1 d . . . . . H32 H 0.869752 0.138563 0.421847 0.035 Uiso 1 1 calc R . . . . C33 C 0.68381(19) 0.26591(15) 0.41589(8) 0.0247(4) Uani 1 1 d . . . . . C34 C 0.59834(19) 0.19964(16) 0.45885(9) 0.0270(4) Uani 1 1 d . . . . . C35 C 0.46352(19) 0.28302(16) 0.48252(9) 0.0257(4) Uani 1 1 d . . . . . C36 C 0.3855(2) 0.24607(17) 0.53190(9) 0.0298(4) Uani 1 1 d . . . . . H36 H 0.419883 0.168557 0.551092 0.036 Uiso 1 1 calc R . . . . C37 C 0.2599(2) 0.31588(17) 0.55494(9) 0.0315(5) Uani 1 1 d . . . . . C38 C 0.2129(2) 0.42820(18) 0.52580(10) 0.0350(5) Uani 1 1 d . . . . . H38 H 0.129167 0.479478 0.540675 0.042 Uiso 1 1 calc R . . . . C39 C 0.2853(2) 0.46735(17) 0.47553(9) 0.0333(5) Uani 1 1 d . . . . . H39 H 0.249716 0.544644 0.456199 0.040 Uiso 1 1 calc R . . . . C40 C 0.40941(19) 0.39553(16) 0.45272(8) 0.0264(4) Uani 1 1 d . . . . . C41 C 0.6920(2) 0.12893(19) 0.51384(10) 0.0391(5) Uani 1 1 d . . . . . H41A H 0.772705 0.071153 0.497756 0.044(3) Uiso 1 1 calc GR . . . . H41B H 0.635024 0.089459 0.541946 0.044(3) Uiso 1 1 calc GR . . . . H41C H 0.728420 0.180811 0.537083 0.044(3) Uiso 1 1 calc GR . . . . C42 C 0.5508(2) 0.11674(17) 0.41941(10) 0.0372(5) Uani 1 1 d . . . . . H42A H 0.490509 0.161915 0.384167 0.050(4) Uiso 1 1 calc GR . . . . H42B H 0.496317 0.072404 0.445838 0.050(4) Uiso 1 1 calc GR . . . . H42C H 0.635521 0.063235 0.403159 0.050(4) Uiso 1 1 calc GR . . . . C43 C 0.4971(2) 0.25783(17) -0.07512(10) 0.0347(5) Uani 1 1 d . . . . . C44A C 0.6256(3) 0.1795(3) -0.03737(15) 0.0735(12) Uani 0.886(5) 1 d D . P A 1 H44A H 0.657640 0.224062 -0.007805 0.110 Uiso 0.886(5) 1 calc GR . P A 1 H44B H 0.703612 0.149785 -0.066068 0.110 Uiso 0.886(5) 1 calc GR . P A 1 H44C H 0.597970 0.114380 -0.013990 0.110 Uiso 0.886(5) 1 calc DGR . P A 1 C45A C 0.5447(3) 0.3543(2) -0.11344(15) 0.0562(10) Uani 0.886(5) 1 d . . P A 1 H45A H 0.462009 0.408350 -0.135943 0.084 Uiso 0.886(5) 1 calc GR . P A 1 H45B H 0.616936 0.320982 -0.143812 0.084 Uiso 0.886(5) 1 calc GR . P A 1 H45C H 0.585883 0.395943 -0.085302 0.084 Uiso 0.886(5) 1 calc GR . P A 1 C46A C 0.4484(4) 0.1883(3) -0.12088(16) 0.0703(12) Uani 0.886(5) 1 d . . P A 1 H46A H 0.420435 0.123406 -0.097456 0.105 Uiso 0.886(5) 1 calc GR . P A 1 H46B H 0.527065 0.158224 -0.149236 0.105 Uiso 0.886(5) 1 calc GR . P A 1 H46C H 0.366347 0.238416 -0.145505 0.105 Uiso 0.886(5) 1 calc GR . P A 1 C55 C 0.1785(2) 0.26689(18) 0.60884(10) 0.0385(5) Uani 1 1 d . . . . . C56 C 0.2817(3) 0.2025(2) 0.66207(11) 0.0606(7) Uani 1 1 d . . . . . H56A H 0.352355 0.136767 0.646547 0.073(5) Uiso 1 1 calc GR . . . . H56B H 0.228039 0.174023 0.696593 0.073(5) Uiso 1 1 calc GR . . . . H56C H 0.331004 0.255425 0.677258 0.073(5) Uiso 1 1 calc GR . . . . C57 C 0.0641(3) 0.3629(2) 0.63584(12) 0.0554(7) Uani 1 1 d . . . . . H57A H 0.108808 0.419045 0.650656 0.074(5) Uiso 1 1 calc GR . . . . H57B H 0.017187 0.329150 0.671088 0.074(5) Uiso 1 1 calc GR . . . . H57C H -0.007221 0.402227 0.603129 0.074(5) Uiso 1 1 calc GR . . . . C58 C 0.1050(3) 0.1836(2) 0.58395(13) 0.0573(7) Uani 1 1 d . . . . . H58A H 0.035450 0.225773 0.551103 0.070(5) Uiso 1 1 calc GR . . . . H58B H 0.055426 0.150412 0.618420 0.070(5) Uiso 1 1 calc GR . . . . H58C H 0.176884 0.121145 0.566344 0.070(5) Uiso 1 1 calc GR . . . . C47A C -0.3646(6) 0.1874(5) 0.1835(3) 0.0345(8) Uani 0.729(5) 1 d D . P B 1 C48A C -0.3659(4) 0.1705(3) 0.25568(14) 0.0480(11) Uani 0.729(5) 1 d D . P B 1 H48A H -0.442521 0.135188 0.269802 0.072 Uiso 0.729(5) 1 calc GR . P B 1 H48B H -0.382654 0.245982 0.271866 0.072 Uiso 0.729(5) 1 calc GR . P B 1 H48C H -0.273474 0.119665 0.271436 0.072 Uiso 0.729(5) 1 calc GR . P B 1 C49A C -0.5095(3) 0.2640(3) 0.15859(19) 0.0532(11) Uani 0.729(5) 1 d D . P B 1 H49A H -0.584968 0.227845 0.173408 0.080 Uiso 0.729(5) 1 calc GR . P B 1 H49B H -0.508972 0.273061 0.112502 0.080 Uiso 0.729(5) 1 calc GR . P B 1 H49C H -0.527811 0.340353 0.173875 0.080 Uiso 0.729(5) 1 calc GR . P B 1 C50A C -0.3380(5) 0.0684(4) 0.1604(2) 0.0508(12) Uani 0.729(5) 1 d D . P B 1 H50A H -0.416937 0.035086 0.173502 0.076 Uiso 0.729(5) 1 calc GR . P B 1 H50B H -0.247799 0.017285 0.178368 0.076 Uiso 0.729(5) 1 calc GR . P B 1 H50C H -0.332218 0.076125 0.114378 0.076 Uiso 0.729(5) 1 calc GR . P B 1 C51A C 1.0588(6) 0.1987(5) 0.3440(3) 0.0327(7) Uani 0.708(2) 1 d D . P C 1 C52A C 1.1452(4) 0.1742(4) 0.40505(17) 0.0672(11) Uani 0.708(2) 1 d D . P C 1 H52A H 1.104304 0.126259 0.436024 0.101 Uiso 0.708(2) 1 calc GR . P C 1 H52B H 1.142075 0.247689 0.421371 0.101 Uiso 0.708(2) 1 calc GR . P C 1 H52C H 1.244838 0.132996 0.397040 0.101 Uiso 0.708(2) 1 calc GR . P C 1 C53A C 1.1301(3) 0.2695(3) 0.29671(16) 0.0428(7) Uani 0.708(2) 1 d D . P C 1 H53A H 1.227174 0.223261 0.288169 0.064 Uiso 0.708(2) 1 calc GR . P C 1 H53B H 1.134789 0.340219 0.314107 0.064 Uiso 0.708(2) 1 calc GR . P C 1 H53C H 1.073939 0.290399 0.257503 0.064 Uiso 0.708(2) 1 calc GR . P C 1 C54A C 1.0639(4) 0.0856(3) 0.3172(2) 0.0676(11) Uani 0.708(2) 1 d D . P C 1 H54A H 1.027010 0.035128 0.348252 0.101 Uiso 0.708(2) 1 calc GR . P C 1 H54B H 1.163139 0.046517 0.307175 0.101 Uiso 0.708(2) 1 calc GR . P C 1 H54C H 1.004952 0.102490 0.278825 0.101 Uiso 0.708(2) 1 calc GR . P C 1 C47B C -0.3474(15) 0.1705(13) 0.1882(7) 0.0345(8) Uani 0.271(5) 1 d D . P B 2 C48B C -0.2701(11) 0.0722(11) 0.2384(6) 0.083(5) Uani 0.271(5) 1 d D . P B 2 H48D H -0.238378 0.105797 0.273267 0.125 Uiso 0.271(5) 1 calc R . P B 2 H48E H -0.336039 0.027044 0.254142 0.125 Uiso 0.271(5) 1 calc R . P B 2 H48F H -0.186842 0.021419 0.219589 0.125 Uiso 0.271(5) 1 calc R . P B 2 C49B C -0.4818(10) 0.2433(9) 0.2193(6) 0.067(4) Uani 0.271(5) 1 d D . P B 2 H49D H -0.452893 0.276360 0.255022 0.101 Uiso 0.271(5) 1 calc R . P B 2 H49E H -0.534516 0.306144 0.188472 0.101 Uiso 0.271(5) 1 calc R . P B 2 H49F H -0.543365 0.193658 0.234014 0.101 Uiso 0.271(5) 1 calc R . P B 2 C50B C -0.3988(18) 0.1209(17) 0.1327(8) 0.093(6) Uani 0.271(5) 1 d D . P B 2 H50D H -0.315785 0.073986 0.111769 0.139 Uiso 0.271(5) 1 calc R . P B 2 H50E H -0.461058 0.072336 0.148161 0.139 Uiso 0.271(5) 1 calc R . P B 2 H50F H -0.452210 0.184821 0.102618 0.139 Uiso 0.271(5) 1 calc R . P B 2 C51B C 1.0679(14) 0.2095(11) 0.3461(6) 0.0327(7) Uani 0.292(2) 1 d D . P C 2 C52B C 1.0796(9) 0.1863(10) 0.2788(4) 0.0672(11) Uani 0.292(2) 1 d D . P C 2 H52D H 1.023947 0.132192 0.271637 0.101 Uiso 0.292(2) 1 calc R . P C 2 H52E H 1.042321 0.259319 0.251799 0.101 Uiso 0.292(2) 1 calc R . P C 2 H52F H 1.180344 0.152337 0.268861 0.101 Uiso 0.292(2) 1 calc R . P C 2 C53B C 1.1252(8) 0.0962(7) 0.3863(4) 0.0428(7) Uani 0.292(2) 1 d D . P C 2 H53D H 1.118429 0.109610 0.430745 0.064 Uiso 0.292(2) 1 calc R . P C 2 H53E H 1.068969 0.042761 0.378535 0.064 Uiso 0.292(2) 1 calc R . P C 2 H53F H 1.225653 0.062339 0.375848 0.064 Uiso 0.292(2) 1 calc R . P C 2 C54B C 1.1520(9) 0.2920(7) 0.3585(6) 0.0676(11) Uani 0.292(2) 1 d D . P C 2 H54D H 1.143025 0.306050 0.402822 0.101 Uiso 0.292(2) 1 calc R . P C 2 H54E H 1.253059 0.258473 0.348908 0.101 Uiso 0.292(2) 1 calc R . P C 2 H54F H 1.115036 0.365456 0.331846 0.101 Uiso 0.292(2) 1 calc R . P C 2 C44B C 0.468(3) 0.331(2) -0.1385(12) 0.059(7) Uiso 0.114(5) 1 d . . P A 3 H44D H 0.450049 0.413410 -0.132355 0.089 Uiso 0.114(5) 1 calc R . P A 3 H44E H 0.551360 0.308549 -0.165592 0.089 Uiso 0.114(5) 1 calc R . P A 3 H44F H 0.383912 0.319280 -0.158330 0.089 Uiso 0.114(5) 1 calc R . P A 3 C46B C 0.643(2) 0.269(2) -0.0448(11) 0.058(7) Uiso 0.114(5) 1 d . . P A 3 H46D H 0.634954 0.351342 -0.041356 0.086 Uiso 0.114(5) 1 calc R . P A 3 H46E H 0.658517 0.225779 -0.002892 0.086 Uiso 0.114(5) 1 calc R . P A 3 H46F H 0.724004 0.238125 -0.071757 0.086 Uiso 0.114(5) 1 calc R . P A 3 C45B C 0.526(3) 0.132(2) -0.0770(15) 0.078(9) Uiso 0.114(5) 1 d . . P A 3 H45D H 0.543378 0.092649 -0.034215 0.116 Uiso 0.114(5) 1 calc R . P A 3 H45E H 0.443308 0.115490 -0.095442 0.116 Uiso 0.114(5) 1 calc R . P A 3 H45F H 0.610756 0.104759 -0.102704 0.116 Uiso 0.114(5) 1 calc R . P A 3 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 S 0.0392(3) 0.0201(2) 0.0274(3) -0.00363(19) 0.0033(2) -0.0085(2) N1 0.0280(8) 0.0302(8) 0.0250(8) -0.0110(7) 0.0091(7) -0.0144(7) N2 0.0226(8) 0.0338(9) 0.0252(8) -0.0006(7) 0.0028(7) -0.0038(7) C1 0.0284(10) 0.0230(9) 0.0220(9) -0.0046(8) 0.0092(8) -0.0083(8) C2 0.0328(11) 0.0258(10) 0.0264(10) -0.0011(8) 0.0007(8) -0.0030(8) C3 0.0304(10) 0.0349(11) 0.0224(10) -0.0028(8) -0.0003(8) -0.0079(9) C4 0.0262(10) 0.0265(10) 0.0229(10) -0.0074(8) 0.0081(8) -0.0115(8) C5 0.0218(9) 0.0207(9) 0.0231(9) -0.0028(7) 0.0084(7) -0.0071(7) C6 0.0205(9) 0.0224(9) 0.0199(9) -0.0026(7) 0.0081(7) -0.0071(7) C7 0.0192(9) 0.0238(9) 0.0213(9) -0.0048(7) 0.0081(7) -0.0082(7) C8 0.0207(9) 0.0225(9) 0.0261(10) -0.0065(8) 0.0081(8) -0.0076(7) C9 0.0213(9) 0.0310(10) 0.0245(10) -0.0027(8) 0.0044(8) -0.0065(8) C10 0.0303(11) 0.0374(11) 0.0305(11) -0.0100(9) 0.0004(9) -0.0133(9) C11 0.0366(11) 0.0281(10) 0.0327(11) -0.0082(9) 0.0031(9) -0.0141(9) C12 0.0275(10) 0.0236(9) 0.0240(10) -0.0031(8) 0.0079(8) -0.0107(8) C13 0.0208(9) 0.0292(10) 0.0214(9) -0.0051(8) 0.0006(7) -0.0078(8) C14 0.0323(10) 0.0262(10) 0.0277(10) -0.0065(8) 0.0048(8) -0.0130(8) C15 0.0300(10) 0.0310(10) 0.0311(11) -0.0032(8) 0.0076(8) -0.0152(9) C16 0.0238(10) 0.0313(10) 0.0299(10) -0.0042(8) 0.0042(8) -0.0085(8) C17 0.0228(10) 0.0228(9) 0.0320(10) -0.0043(8) 0.0035(8) -0.0054(8) C18 0.0195(9) 0.0269(10) 0.0226(9) -0.0030(8) -0.0007(7) -0.0074(8) C19 0.0242(10) 0.0266(10) 0.0257(10) -0.0044(8) 0.0047(8) -0.0106(8) C20 0.0235(9) 0.0294(10) 0.0219(9) -0.0038(8) 0.0020(7) -0.0100(8) C21 0.0285(10) 0.0302(10) 0.0317(11) -0.0073(8) 0.0031(8) -0.0137(8) C22 0.0245(10) 0.0384(11) 0.0267(10) -0.0059(9) 0.0026(8) -0.0135(9) C23 0.0252(10) 0.0368(11) 0.0292(10) -0.0082(9) 0.0073(8) -0.0094(8) C24 0.0287(10) 0.0293(10) 0.0299(10) -0.0068(8) 0.0068(8) -0.0090(8) C25 0.0245(10) 0.0294(10) 0.0200(9) -0.0021(8) 0.0004(7) -0.0112(8) C26 0.0390(12) 0.0441(12) 0.0428(12) -0.0186(10) 0.0174(10) -0.0242(10) C27 0.0279(11) 0.0369(11) 0.0427(12) 0.0071(10) 0.0056(9) -0.0075(9) C28 0.0233(9) 0.0289(10) 0.0231(9) -0.0078(8) 0.0005(8) -0.0092(8) C29 0.0287(10) 0.0270(10) 0.0273(10) -0.0015(8) 0.0015(8) -0.0087(8) C30 0.0284(10) 0.0302(10) 0.0274(10) -0.0031(8) 0.0051(8) -0.0132(8) C31 0.0249(10) 0.0311(10) 0.0304(10) -0.0033(8) 0.0032(8) -0.0113(8) C32 0.0259(10) 0.0274(10) 0.0332(11) -0.0005(8) 0.0038(8) -0.0075(8) C33 0.0236(10) 0.0277(10) 0.0251(10) -0.0048(8) 0.0023(8) -0.0106(8) C34 0.0248(10) 0.0283(10) 0.0289(10) -0.0033(8) 0.0064(8) -0.0094(8) C35 0.0221(9) 0.0312(10) 0.0276(10) -0.0076(8) 0.0027(8) -0.0119(8) C36 0.0291(10) 0.0312(10) 0.0328(11) -0.0061(9) 0.0058(8) -0.0139(9) C37 0.0290(11) 0.0374(11) 0.0331(11) -0.0111(9) 0.0087(9) -0.0155(9) C38 0.0269(11) 0.0395(12) 0.0386(12) -0.0108(10) 0.0111(9) -0.0073(9) C39 0.0296(11) 0.0343(11) 0.0343(11) -0.0032(9) 0.0061(9) -0.0066(9) C40 0.0243(10) 0.0347(11) 0.0230(10) -0.0057(8) 0.0014(8) -0.0119(8) C41 0.0293(11) 0.0471(13) 0.0354(12) 0.0043(10) 0.0100(9) -0.0051(10) C42 0.0367(12) 0.0345(11) 0.0466(13) -0.0124(10) 0.0188(10) -0.0180(9) C43 0.0306(11) 0.0315(11) 0.0430(12) -0.0079(9) 0.0164(9) -0.0100(9) C44A 0.0410(17) 0.086(3) 0.070(2) -0.0012(18) 0.0225(15) 0.0181(17) C45A 0.0562(19) 0.0443(16) 0.068(2) -0.0105(14) 0.0456(17) -0.0160(14) C46A 0.070(2) 0.099(3) 0.068(2) -0.055(2) 0.0501(18) -0.051(2) C55 0.0370(12) 0.0398(12) 0.0434(13) -0.0104(10) 0.0177(10) -0.0172(10) C56 0.0590(16) 0.0813(19) 0.0414(14) 0.0029(13) 0.0210(12) -0.0245(14) C57 0.0591(16) 0.0481(14) 0.0656(17) -0.0179(12) 0.0404(14) -0.0239(12) C58 0.0588(16) 0.0573(15) 0.0686(17) -0.0190(13) 0.0296(13) -0.0349(13) C47A 0.0283(17) 0.045(2) 0.0373(15) -0.0114(13) 0.0099(12) -0.0190(15) C48A 0.059(3) 0.065(2) 0.0362(18) -0.0095(16) 0.0151(16) -0.044(2) C49A 0.0289(17) 0.069(2) 0.070(3) -0.015(2) 0.0027(16) -0.0253(16) C50A 0.057(3) 0.059(3) 0.056(3) -0.026(2) 0.028(2) -0.043(2) C51A 0.0243(12) 0.0338(15) 0.0394(13) 0.0023(11) 0.0070(10) -0.0100(10) C52A 0.0286(17) 0.103(3) 0.055(2) 0.021(2) 0.0020(15) -0.0041(18) C53A 0.0291(15) 0.0466(17) 0.0519(19) 0.0012(15) 0.0134(13) -0.0126(13) C54A 0.0400(18) 0.049(2) 0.119(3) -0.032(2) 0.040(2) -0.0142(16) C47B 0.0283(17) 0.045(2) 0.0373(15) -0.0114(13) 0.0099(12) -0.0190(15) C48B 0.050(6) 0.089(9) 0.107(10) 0.046(8) 0.007(6) -0.036(6) C49B 0.046(6) 0.075(7) 0.090(10) -0.036(7) 0.020(6) -0.024(5) C50B 0.077(12) 0.137(17) 0.105(14) -0.050(11) 0.040(9) -0.086(12) C51B 0.0243(12) 0.0338(15) 0.0394(13) 0.0023(11) 0.0070(10) -0.0100(10) C52B 0.0286(17) 0.103(3) 0.055(2) 0.021(2) 0.0020(15) -0.0041(18) C53B 0.0291(15) 0.0466(17) 0.0519(19) 0.0012(15) 0.0134(13) -0.0126(13) C54B 0.0400(18) 0.049(2) 0.119(3) -0.032(2) 0.040(2) -0.0142(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S C1 1.7525(18) . ? S C12 1.7508(19) . ? N1 C4 1.435(2) . ? N1 C13 1.401(2) . ? N1 C25 1.402(2) . ? N2 C9 1.437(2) . ? N2 C28 1.399(2) . ? N2 C40 1.404(2) . ? C1 C2 1.385(3) . ? C1 C6 1.404(2) . ? C2 C3 1.384(3) . ? C3 C4 1.392(3) . ? C4 C5 1.379(2) . ? C5 C6 1.390(2) . ? C6 C7 1.449(2) . ? C7 C8 1.391(2) . ? C7 C12 1.403(2) . ? C8 C9 1.381(3) . ? C9 C10 1.388(3) . ? C10 C11 1.382(3) . ? C11 C12 1.390(3) . ? C13 C14 1.392(2) . ? C13 C18 1.398(2) . ? C14 C15 1.377(3) . ? C15 C16 1.389(3) . ? C16 C17 1.394(2) . ? C16 C43 1.532(3) . ? C17 C18 1.394(2) . ? C18 C19 1.530(2) . ? C19 C20 1.531(2) . ? C19 C26 1.532(3) . ? C19 C27 1.535(3) . ? C20 C21 1.395(2) . ? C20 C25 1.393(2) . ? C21 C22 1.391(3) . ? C22 C23 1.386(3) . ? C22 C47A 1.528(5) . ? C22 C47B 1.555(14) . ? C23 C24 1.374(3) . ? C24 C25 1.394(2) . ? C28 C29 1.391(2) . ? C28 C33 1.399(3) . ? C29 C30 1.380(3) . ? C30 C31 1.385(3) . ? C31 C32 1.393(3) . ? C31 C51A 1.525(6) . ? C31 C51B 1.563(13) . ? C32 C33 1.390(2) . ? C33 C34 1.529(2) . ? C34 C35 1.531(2) . ? C34 C41 1.528(3) . ? C34 C42 1.542(3) . ? C35 C36 1.391(3) . ? C35 C40 1.397(3) . ? C36 C37 1.394(3) . ? C37 C38 1.384(3) . ? C37 C55 1.539(3) . ? C38 C39 1.382(3) . ? C39 C40 1.392(3) . ? C43 C44A 1.525(4) . ? C43 C45A 1.518(3) . ? C43 C46A 1.517(3) . ? C43 C44B 1.52(2) . ? C43 C46B 1.62(2) . ? C43 C45B 1.47(3) . ? C55 C56 1.525(3) . ? C55 C57 1.525(3) . ? C55 C58 1.525(3) . ? C47A C48A 1.536(6) . ? C47A C49A 1.525(6) . ? C47A C50A 1.522(6) . ? C51A C52A 1.524(6) . ? C51A C53A 1.527(6) . ? C51A C54A 1.524(6) . ? C47B C48B 1.543(13) . ? C47B C49B 1.543(13) . ? C47B C50B 1.538(13) . ? C51B C52B 1.492(13) . ? C51B C53B 1.502(12) . ? C51B C54B 1.495(13) . ? 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 C12 S C1 91.31(8) . . ? C13 N1 C4 119.03(14) . . ? C13 N1 C25 120.75(14) . . ? C25 N1 C4 119.93(14) . . ? C28 N2 C9 119.53(14) . . ? C28 N2 C40 121.08(15) . . ? C40 N2 C9 119.22(14) . . ? C2 C1 S 126.59(14) . . ? C2 C1 C6 121.25(16) . . ? C6 C1 S 112.15(13) . . ? C3 C2 C1 118.79(17) . . ? C2 C3 C4 120.49(17) . . ? C3 C4 N1 120.82(16) . . ? C5 C4 N1 118.55(16) . . ? C5 C4 C3 120.63(16) . . ? C4 C5 C6 119.83(16) . . ? C1 C6 C7 112.15(15) . . ? C5 C6 C1 118.99(16) . . ? C5 C6 C7 128.86(16) . . ? C8 C7 C6 128.68(16) . . ? C8 C7 C12 119.20(16) . . ? C12 C7 C6 112.05(15) . . ? C9 C8 C7 119.67(16) . . ? C8 C9 N2 118.53(16) . . ? C8 C9 C10 120.50(17) . . ? C10 C9 N2 120.96(16) . . ? C11 C10 C9 120.98(18) . . ? C10 C11 C12 118.49(17) . . ? C7 C12 S 112.28(13) . . ? C11 C12 S 126.58(14) . . ? C11 C12 C7 121.09(17) . . ? C14 C13 N1 119.94(16) . . ? C14 C13 C18 119.46(16) . . ? C18 C13 N1 120.60(15) . . ? C15 C14 C13 121.28(17) . . ? C14 C15 C16 121.24(17) . . ? C15 C16 C17 116.45(16) . . ? C15 C16 C43 122.37(16) . . ? C17 C16 C43 121.18(16) . . ? C16 C17 C18 124.09(17) . . ? C13 C18 C19 121.58(15) . . ? C17 C18 C13 117.39(16) . . ? C17 C18 C19 120.94(16) . . ? C18 C19 C20 110.53(14) . . ? C18 C19 C26 110.52(15) . . ? C18 C19 C27 108.50(14) . . ? C20 C19 C26 109.87(15) . . ? C20 C19 C27 108.00(15) . . ? C26 C19 C27 109.37(16) . . ? C21 C20 C19 120.21(16) . . ? C25 C20 C19 121.78(15) . . ? C25 C20 C21 117.74(16) . . ? C22 C21 C20 123.61(17) . . ? C21 C22 C47A 124.0(3) . . ? C21 C22 C47B 118.4(6) . . ? C23 C22 C21 116.60(17) . . ? C23 C22 C47A 119.3(3) . . ? C23 C22 C47B 124.6(6) . . ? C24 C23 C22 121.64(17) . . ? C23 C24 C25 120.79(17) . . ? C20 C25 N1 120.42(16) . . ? C20 C25 C24 119.61(16) . . ? C24 C25 N1 119.98(16) . . ? N2 C28 C33 120.29(16) . . ? C29 C28 N2 120.28(16) . . ? C29 C28 C33 119.43(16) . . ? C30 C29 C28 120.92(17) . . ? C29 C30 C31 121.49(17) . . ? C30 C31 C32 116.56(17) . . ? C30 C31 C51A 123.5(3) . . ? C30 C31 C51B 119.9(5) . . ? C32 C31 C51A 119.9(3) . . ? C32 C31 C51B 123.3(5) . . ? C33 C32 C31 123.81(17) . . ? C28 C33 C34 121.36(15) . . ? C32 C33 C28 117.76(16) . . ? C32 C33 C34 120.63(16) . . ? C33 C34 C35 110.76(15) . . ? C33 C34 C42 107.54(15) . . ? C35 C34 C42 108.01(15) . . ? C41 C34 C33 110.23(15) . . ? C41 C34 C35 110.90(15) . . ? C41 C34 C42 109.31(16) . . ? C36 C35 C34 120.65(16) . . ? C36 C35 C40 117.82(17) . . ? C40 C35 C34 121.39(16) . . ? C35 C36 C37 123.97(18) . . ? C36 C37 C55 120.47(18) . . ? C38 C37 C36 116.41(17) . . ? C38 C37 C55 123.10(17) . . ? C39 C38 C37 121.41(18) . . ? C38 C39 C40 121.17(18) . . ? C35 C40 N2 120.38(16) . . ? C39 C40 N2 120.48(17) . . ? C39 C40 C35 119.13(17) . . ? C16 C43 C46B 106.5(9) . . ? C44A C43 C16 108.86(18) . . ? C45A C43 C16 112.23(17) . . ? C45A C43 C44A 108.4(2) . . ? C46A C43 C16 110.54(17) . . ? C46A C43 C44A 109.1(2) . . ? C46A C43 C45A 107.6(2) . . ? C44B C43 C16 109.5(9) . . ? C44B C43 C46B 109.6(14) . . ? C45B C43 C16 112.3(11) . . ? C45B C43 C44B 115.6(16) . . ? C45B C43 C46B 102.7(15) . . ? C56 C55 C37 110.38(17) . . ? C57 C55 C37 111.60(17) . . ? C57 C55 C56 108.0(2) . . ? C57 C55 C58 108.21(19) . . ? C58 C55 C37 109.20(17) . . ? C58 C55 C56 109.5(2) . . ? C22 C47A C48A 108.6(4) . . ? C49A C47A C22 109.3(3) . . ? C49A C47A C48A 109.7(4) . . ? C50A C47A C22 112.2(4) . . ? C50A C47A C48A 107.7(4) . . ? C50A C47A C49A 109.2(4) . . ? C31 C51A C53A 112.2(4) . . ? C52A C51A C31 108.2(4) . . ? C52A C51A C53A 107.4(4) . . ? C52A C51A C54A 110.4(4) . . ? C54A C51A C31 111.0(4) . . ? C54A C51A C53A 107.6(4) . . ? C48B C47B C22 111.5(9) . . ? C49B C47B C22 111.4(10) . . ? C49B C47B C48B 107.2(11) . . ? C50B C47B C22 108.4(10) . . ? C50B C47B C48B 110.9(13) . . ? C50B C47B C49B 107.3(12) . . ? C52B C51B C31 106.2(9) . . ? C52B C51B C53B 108.2(10) . . ? C52B C51B C54B 110.7(11) . . ? C53B C51B C31 111.8(9) . . ? C54B C51B C31 110.2(9) . . ? C54B C51B C53B 109.7(10) . . ? _shelx_res_file ; TITL 17srv366 in P-1 #2 17srv366.res created by SHELXL-2018/3 at 22:21:01 on 11-Oct-2018 REM reset to P-1 #2 CELL 0.71073 9.7054 12.0521 21.3945 83.6147 88.8165 74.1306 ZERR 2 0.0005 0.0006 0.001 0.0019 0.002 0.0018 LATT 1 SFAC C H N S UNIT 116 132 4 2 SADI C49B C47B C48B C47B C50B C47B C48A C47A C49A C47A C50A C47A SADI C54A C51A C53B C51B C52A C51A C54B C51B C44A H44c C52B C51B C53A C51A SADI C51A C31 C51B C31 SADI C47B C22 C47A C22 EADP C51A C51B EADP C52B C52A EADP C53A C53B EADP C54A C54B EADP C47A C47B L.S. 7 PLAN 7 SIZE 0.209 0.281 0.523 TEMP -153.15 BOND fmap 2 acta OMIT -3 50 OMIT 0 -1 1 OMIT 1 0 0 REM REM REM WGHT 0.046000 1.221200 EXTI 0.005273 FVAR 0.20033 0.88582 0.72866 0.70817 0.04536 0.04546 0.04409 FVAR 0.04967 0.07349 0.07395 0.07027 S 4 0.120082 0.822509 0.229027 11.00000 0.03918 0.02009 = 0.02744 -0.00363 0.00330 -0.00848 N1 3 0.057277 0.425086 0.102620 11.00000 0.02803 0.03022 = 0.02504 -0.01103 0.00911 -0.01439 N2 3 0.479097 0.435368 0.400306 11.00000 0.02258 0.03384 = 0.02520 -0.00060 0.00282 -0.00383 C1 1 0.084955 0.714342 0.188571 11.00000 0.02838 0.02296 = 0.02203 -0.00461 0.00916 -0.00830 C2 1 -0.005877 0.731116 0.137209 11.00000 0.03277 0.02576 = 0.02643 -0.00106 0.00072 -0.00302 AFIX 43 H2 2 -0.059896 0.806979 0.121316 11.00000 -1.20000 AFIX 0 C3 1 -0.016495 0.635345 0.109470 11.00000 0.03043 0.03489 = 0.02238 -0.00285 -0.00030 -0.00790 AFIX 43 H3 2 -0.078795 0.645428 0.074372 11.00000 -1.20000 AFIX 0 C4 1 0.063426 0.524360 0.132613 11.00000 0.02616 0.02650 = 0.02291 -0.00737 0.00811 -0.01152 C5 1 0.151682 0.507647 0.184498 11.00000 0.02181 0.02068 = 0.02313 -0.00284 0.00839 -0.00707 AFIX 43 H5 2 0.204319 0.431452 0.200526 11.00000 -1.20000 AFIX 0 C6 1 0.163432 0.602606 0.213294 11.00000 0.02055 0.02244 = 0.01991 -0.00257 0.00810 -0.00708 C7 1 0.249441 0.604790 0.267452 11.00000 0.01921 0.02379 = 0.02133 -0.00478 0.00808 -0.00824 C8 1 0.331634 0.511877 0.307046 11.00000 0.02074 0.02252 = 0.02607 -0.00653 0.00806 -0.00758 AFIX 43 H8 2 0.339996 0.434474 0.298806 11.00000 -1.20000 AFIX 0 C9 1 0.400986 0.532748 0.358379 11.00000 0.02125 0.03105 = 0.02447 -0.00268 0.00441 -0.00650 C10 1 0.393320 0.645520 0.369510 11.00000 0.03034 0.03738 = 0.03055 -0.01005 0.00036 -0.01332 AFIX 43 H10 2 0.444955 0.658398 0.403984 11.00000 -1.20000 AFIX 0 C11 1 0.311671 0.739394 0.331183 11.00000 0.03663 0.02811 = 0.03268 -0.00821 0.00313 -0.01413 AFIX 43 H11 2 0.305818 0.816495 0.339217 11.00000 -1.20000 AFIX 0 C12 1 0.238304 0.718411 0.280607 11.00000 0.02750 0.02359 = 0.02399 -0.00313 0.00786 -0.01069 C13 1 0.160866 0.383973 0.057983 11.00000 0.02076 0.02917 = 0.02142 -0.00512 0.00058 -0.00783 C14 1 0.235425 0.457443 0.027402 11.00000 0.03234 0.02618 = 0.02769 -0.00648 0.00478 -0.01298 AFIX 43 H14 2 0.213459 0.535821 0.036325 11.00000 -1.20000 AFIX 0 C15 1 0.340410 0.418718 -0.015536 11.00000 0.03000 0.03096 = 0.03114 -0.00323 0.00762 -0.01517 AFIX 43 H15 2 0.388946 0.471045 -0.035913 11.00000 -1.20000 AFIX 0 C16 1 0.376678 0.304576 -0.029615 11.00000 0.02382 0.03134 = 0.02987 -0.00424 0.00420 -0.00855 C17 1 0.299024 0.233136 0.000805 11.00000 0.02284 0.02276 = 0.03199 -0.00434 0.00350 -0.00542 AFIX 43 H17 2 0.321964 0.154692 -0.008071 11.00000 -1.20000 AFIX 0 C18 1 0.189793 0.269610 0.043442 11.00000 0.01951 0.02690 = 0.02265 -0.00297 -0.00066 -0.00741 C19 1 0.111063 0.185268 0.075689 11.00000 0.02417 0.02659 = 0.02568 -0.00443 0.00473 -0.01058 C20 1 -0.024572 0.251361 0.107613 11.00000 0.02350 0.02944 = 0.02193 -0.00379 0.00202 -0.00995 C21 1 -0.128471 0.195594 0.128086 11.00000 0.02847 0.03017 = 0.03175 -0.00726 0.00313 -0.01373 AFIX 43 H21 2 -0.116978 0.118800 0.118006 11.00000 -1.20000 AFIX 0 C22 1 -0.247970 0.246274 0.162448 11.00000 0.02453 0.03841 = 0.02672 -0.00587 0.00257 -0.01353 C23 1 -0.260484 0.357945 0.176831 11.00000 0.02521 0.03680 = 0.02919 -0.00823 0.00731 -0.00936 AFIX 43 H23 2 -0.339681 0.395055 0.200883 11.00000 -1.20000 AFIX 0 C24 1 -0.161226 0.416273 0.157171 11.00000 0.02872 0.02935 = 0.02992 -0.00683 0.00682 -0.00901 AFIX 43 H24 2 -0.173470 0.493088 0.167369 11.00000 -1.20000 AFIX 0 C25 1 -0.042714 0.364078 0.122425 11.00000 0.02451 0.02945 = 0.02005 -0.00213 0.00043 -0.01119 C26 1 0.072010 0.112670 0.027954 11.00000 0.03898 0.04408 = 0.04281 -0.01863 0.01742 -0.02419 AFIX 137 H26A 2 0.030551 0.053852 0.049984 11.00000 51.00000 H26B 2 0.158406 0.074409 0.005833 11.00000 51.00000 H26C 2 0.002097 0.163321 -0.002483 11.00000 51.00000 AFIX 0 C27 1 0.209909 0.104493 0.126737 11.00000 0.02785 0.03687 = 0.04272 0.00710 0.00560 -0.00747 AFIX 137 H27A 2 0.229827 0.150274 0.158801 11.00000 61.00000 H27B 2 0.299998 0.064541 0.107726 11.00000 61.00000 H27C 2 0.162999 0.047102 0.146270 11.00000 61.00000 AFIX 0 C28 1 0.619395 0.376676 0.385768 11.00000 0.02333 0.02888 = 0.02310 -0.00780 0.00053 -0.00916 C29 1 0.696530 0.428371 0.341642 11.00000 0.02867 0.02703 = 0.02726 -0.00147 0.00146 -0.00867 AFIX 43 H29 2 0.652487 0.503119 0.320704 11.00000 -1.20000 AFIX 0 C30 1 0.836143 0.372585 0.327857 11.00000 0.02843 0.03019 = 0.02741 -0.00305 0.00513 -0.01321 AFIX 43 H30 2 0.886042 0.409337 0.297121 11.00000 -1.20000 AFIX 0 C31 1 0.905177 0.264194 0.357830 11.00000 0.02491 0.03108 = 0.03037 -0.00329 0.00321 -0.01130 C32 1 0.825151 0.213410 0.401162 11.00000 0.02590 0.02745 = 0.03316 -0.00053 0.00382 -0.00745 AFIX 43 H32 2 0.869752 0.138563 0.421847 11.00000 -1.20000 AFIX 0 C33 1 0.683806 0.265912 0.415890 11.00000 0.02363 0.02775 = 0.02510 -0.00477 0.00233 -0.01058 C34 1 0.598336 0.199635 0.458853 11.00000 0.02476 0.02835 = 0.02892 -0.00334 0.00636 -0.00941 C35 1 0.463524 0.283022 0.482520 11.00000 0.02210 0.03118 = 0.02758 -0.00765 0.00272 -0.01188 C36 1 0.385498 0.246070 0.531901 11.00000 0.02914 0.03123 = 0.03282 -0.00605 0.00585 -0.01390 AFIX 43 H36 2 0.419883 0.168557 0.551092 11.00000 -1.20000 AFIX 0 C37 1 0.259902 0.315883 0.554937 11.00000 0.02899 0.03743 = 0.03312 -0.01111 0.00870 -0.01548 C38 1 0.212938 0.428199 0.525801 11.00000 0.02690 0.03946 = 0.03860 -0.01079 0.01108 -0.00727 AFIX 43 H38 2 0.129167 0.479478 0.540675 11.00000 -1.20000 AFIX 0 C39 1 0.285301 0.467346 0.475533 11.00000 0.02961 0.03427 = 0.03426 -0.00318 0.00606 -0.00659 AFIX 43 H39 2 0.249716 0.544644 0.456199 11.00000 -1.20000 AFIX 0 C40 1 0.409407 0.395532 0.452724 11.00000 0.02431 0.03472 = 0.02295 -0.00569 0.00136 -0.01189 C41 1 0.692019 0.128926 0.513839 11.00000 0.02927 0.04706 = 0.03540 0.00429 0.01004 -0.00506 AFIX 137 H41A 2 0.772705 0.071153 0.497756 11.00000 71.00000 H41B 2 0.635024 0.089459 0.541946 11.00000 71.00000 H41C 2 0.728420 0.180811 0.537083 11.00000 71.00000 AFIX 0 C42 1 0.550843 0.116744 0.419410 11.00000 0.03666 0.03447 = 0.04662 -0.01244 0.01882 -0.01804 AFIX 137 H42A 2 0.490509 0.161915 0.384167 11.00000 81.00000 H42B 2 0.496317 0.072404 0.445838 11.00000 81.00000 H42C 2 0.635521 0.063235 0.403159 11.00000 81.00000 AFIX 0 C43 1 0.497141 0.257828 -0.075116 11.00000 0.03058 0.03155 = 0.04299 -0.00792 0.01644 -0.00997 PART 1 C44A 1 0.625561 0.179519 -0.037374 21.00000 0.04098 0.08593 = 0.07000 -0.00118 0.02253 0.01807 AFIX 137 H44A 2 0.657640 0.224062 -0.007805 21.00000 -1.50000 H44B 2 0.703612 0.149785 -0.066068 21.00000 -1.50000 H44C 2 0.597970 0.114380 -0.013990 21.00000 -1.50000 AFIX 0 C45A 1 0.544705 0.354324 -0.113438 21.00000 0.05620 0.04432 = 0.06844 -0.01051 0.04562 -0.01596 AFIX 137 H45A 2 0.462009 0.408350 -0.135943 21.00000 -1.50000 H45B 2 0.616936 0.320982 -0.143812 21.00000 -1.50000 H45C 2 0.585883 0.395943 -0.085302 21.00000 -1.50000 AFIX 0 C46A 1 0.448435 0.188315 -0.120879 21.00000 0.06961 0.09860 = 0.06774 -0.05550 0.05013 -0.05056 AFIX 137 H46A 2 0.420435 0.123406 -0.097456 21.00000 -1.50000 H46B 2 0.527065 0.158224 -0.149236 21.00000 -1.50000 H46C 2 0.366347 0.238416 -0.145505 21.00000 -1.50000 AFIX 0 PART 0 C55 1 0.178539 0.266886 0.608842 11.00000 0.03697 0.03976 = 0.04339 -0.01037 0.01771 -0.01724 C56 1 0.281706 0.202522 0.662068 11.00000 0.05903 0.08135 = 0.04135 0.00287 0.02097 -0.02455 AFIX 137 H56A 2 0.352355 0.136767 0.646547 11.00000 91.00000 H56B 2 0.228039 0.174023 0.696593 11.00000 91.00000 H56C 2 0.331004 0.255425 0.677258 11.00000 91.00000 AFIX 0 C57 1 0.064104 0.362906 0.635841 11.00000 0.05908 0.04805 = 0.06560 -0.01792 0.04045 -0.02392 AFIX 137 H57A 2 0.108808 0.419045 0.650656 11.00000 101.00000 H57B 2 0.017187 0.329150 0.671088 11.00000 101.00000 H57C 2 -0.007221 0.402227 0.603129 11.00000 101.00000 AFIX 0 C58 1 0.105003 0.183611 0.583953 11.00000 0.05879 0.05729 = 0.06863 -0.01901 0.02963 -0.03487 AFIX 137 H58A 2 0.035450 0.225773 0.551103 11.00000 111.00000 H58B 2 0.055426 0.150412 0.618420 11.00000 111.00000 H58C 2 0.176884 0.121145 0.566344 11.00000 111.00000 AFIX 0 PART 1 C47A 1 -0.364616 0.187352 0.183474 31.00000 0.02826 0.04451 = 0.03733 -0.01136 0.00989 -0.01898 C48A 1 -0.365936 0.170525 0.255676 31.00000 0.05930 0.06495 = 0.03623 -0.00950 0.01509 -0.04427 AFIX 137 H48A 2 -0.442521 0.135188 0.269802 31.00000 -1.50000 H48B 2 -0.382654 0.245982 0.271866 31.00000 -1.50000 H48C 2 -0.273474 0.119665 0.271436 31.00000 -1.50000 AFIX 0 C49A 1 -0.509543 0.264002 0.158591 31.00000 0.02894 0.06930 = 0.07022 -0.01502 0.00271 -0.02534 AFIX 137 H49A 2 -0.584968 0.227845 0.173408 31.00000 -1.50000 H49B 2 -0.508972 0.273061 0.112502 31.00000 -1.50000 H49C 2 -0.527811 0.340353 0.173875 31.00000 -1.50000 AFIX 0 C50A 1 -0.338024 0.068365 0.160373 31.00000 0.05739 0.05893 = 0.05598 -0.02649 0.02843 -0.04325 AFIX 137 H50A 2 -0.416937 0.035086 0.173502 31.00000 -1.50000 H50B 2 -0.247799 0.017285 0.178368 31.00000 -1.50000 H50C 2 -0.332218 0.076125 0.114378 31.00000 -1.50000 AFIX 0 C51A 1 1.058819 0.198666 0.343964 41.00000 0.02433 0.03379 = 0.03941 0.00230 0.00705 -0.00999 C52A 1 1.145219 0.174221 0.405051 41.00000 0.02863 0.10285 = 0.05481 0.02137 0.00200 -0.00408 AFIX 137 H52A 2 1.104304 0.126259 0.436024 41.00000 -1.50000 H52B 2 1.142075 0.247689 0.421371 41.00000 -1.50000 H52C 2 1.244838 0.132996 0.397040 41.00000 -1.50000 AFIX 0 C53A 1 1.130057 0.269475 0.296705 41.00000 0.02914 0.04658 = 0.05191 0.00123 0.01338 -0.01260 AFIX 137 H53A 2 1.227174 0.223261 0.288169 41.00000 -1.50000 H53B 2 1.134789 0.340219 0.314107 41.00000 -1.50000 H53C 2 1.073939 0.290399 0.257503 41.00000 -1.50000 AFIX 0 C54A 1 1.063937 0.085607 0.317161 41.00000 0.04002 0.04916 = 0.11854 -0.03193 0.03982 -0.01417 AFIX 137 H54A 2 1.027010 0.035128 0.348252 41.00000 -1.50000 H54B 2 1.163139 0.046517 0.307175 41.00000 -1.50000 H54C 2 1.004952 0.102490 0.278825 41.00000 -1.50000 AFIX 0 PART 0 PART 2 C47B 1 -0.347375 0.170499 0.188229 -31.00000 0.02826 0.04451 = 0.03733 -0.01136 0.00989 -0.01898 C48B 1 -0.270109 0.072223 0.238383 -31.00000 0.05028 0.08889 = 0.10675 0.04643 0.00668 -0.03570 AFIX 33 H48D 2 -0.238378 0.105797 0.273267 -31.00000 -1.50000 H48E 2 -0.336039 0.027044 0.254142 -31.00000 -1.50000 H48F 2 -0.186842 0.021419 0.219589 -31.00000 -1.50000 AFIX 0 C49B 1 -0.481798 0.243306 0.219265 -31.00000 0.04583 0.07492 = 0.09033 -0.03578 0.01975 -0.02363 AFIX 33 H49D 2 -0.452893 0.276360 0.255022 -31.00000 -1.50000 H49E 2 -0.534516 0.306144 0.188472 -31.00000 -1.50000 H49F 2 -0.543365 0.193658 0.234014 -31.00000 -1.50000 AFIX 0 C50B 1 -0.398768 0.120913 0.132654 -31.00000 0.07668 0.13694 = 0.10530 -0.05014 0.04023 -0.08626 AFIX 33 H50D 2 -0.315785 0.073986 0.111769 -31.00000 -1.50000 H50E 2 -0.461058 0.072336 0.148161 -31.00000 -1.50000 H50F 2 -0.452210 0.184821 0.102618 -31.00000 -1.50000 AFIX 0 C51B 1 1.067932 0.209455 0.346104 -41.00000 0.02433 0.03379 = 0.03941 0.00230 0.00705 -0.00999 C52B 1 1.079641 0.186341 0.278825 -41.00000 0.02863 0.10285 = 0.05481 0.02137 0.00200 -0.00408 AFIX 33 H52D 2 1.023947 0.132192 0.271637 -41.00000 -1.50000 H52E 2 1.042321 0.259319 0.251799 -41.00000 -1.50000 H52F 2 1.180344 0.152337 0.268861 -41.00000 -1.50000 AFIX 0 C53B 1 1.125222 0.096204 0.386299 -41.00000 0.02914 0.04658 = 0.05191 0.00123 0.01338 -0.01260 AFIX 33 H53D 2 1.118429 0.109610 0.430745 -41.00000 -1.50000 H53E 2 1.068969 0.042761 0.378535 -41.00000 -1.50000 H53F 2 1.225653 0.062339 0.375848 -41.00000 -1.50000 AFIX 0 C54B 1 1.152008 0.291968 0.358487 -41.00000 0.04002 0.04916 = 0.11854 -0.03193 0.03982 -0.01417 AFIX 33 H54D 2 1.143025 0.306050 0.402822 -41.00000 -1.50000 H54E 2 1.253059 0.258473 0.348908 -41.00000 -1.50000 H54F 2 1.115036 0.365456 0.331846 -41.00000 -1.50000 AFIX 0 PART 0 PART 3 C44B 1 0.468026 0.331301 -0.138484 -21.00000 0.05911 AFIX 33 H44D 2 0.450049 0.413410 -0.132355 -21.00000 -1.50000 H44E 2 0.551360 0.308549 -0.165592 -21.00000 -1.50000 H44F 2 0.383912 0.319280 -0.158330 -21.00000 -1.50000 AFIX 0 C46B 1 0.643000 0.269408 -0.044798 -21.00000 0.05765 AFIX 33 H46D 2 0.634954 0.351342 -0.041356 -21.00000 -1.50000 H46E 2 0.658517 0.225779 -0.002892 -21.00000 -1.50000 H46F 2 0.724004 0.238125 -0.071757 -21.00000 -1.50000 AFIX 0 C45B 1 0.526044 0.132262 -0.077028 -21.00000 0.07754 AFIX 33 H45D 2 0.543378 0.092649 -0.034215 -21.00000 -1.50000 H45E 2 0.443308 0.115490 -0.095442 -21.00000 -1.50000 H45F 2 0.610756 0.104759 -0.102704 -21.00000 -1.50000 AFIX 0 HKLF 4 REM 17srv366 in P-1 #2 REM wR2 = 0.1145, GooF = S = 1.027, Restrained GooF = 1.256 for all data REM R1 = 0.0444 for 6465 Fo > 4sig(Fo) and 0.0652 for all 8436 data REM 631 parameters refined using 38 restraints END WGHT 0.0458 1.2241 REM Highest difference peak 0.340, deepest hole -0.247, 1-sigma level 0.038 Q1 1 0.2063 0.7738 0.2519 11.00000 0.05 0.30 Q2 1 -0.5077 0.1736 0.2494 11.00000 0.05 0.23 Q3 1 1.1786 0.2691 0.3421 11.00000 0.05 0.22 Q4 1 0.1506 0.2297 0.0644 11.00000 0.05 0.21 Q5 1 0.6411 0.2396 0.4430 11.00000 0.05 0.21 Q6 1 0.0428 0.2177 0.0925 11.00000 0.05 0.21 Q7 1 1.1203 0.3376 0.3730 11.00000 0.05 0.20 ; _shelx_res_checksum 15491 _olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems' _olex2_submission_special_instructions 'No special instructions were received' #===END _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_DAcDBT_17s188 _database_code_depnum_ccdc_archive 'CCDC 1901569' loop_ _audit_author_name _audit_author_address 'Andrei S. Batsanov' ;Durham University United Kingdom ; _audit_update_record ; 2019-03-06 deposited with the CCDC. 2019-10-14 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT201_DAcDBT_17s188 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 3 Report RESPONSE: extensive disorder in the main molecule ; # Added during the CSD deposition process: Wednesday 06 March 2019 11:39 PM # end Validation Reply Form _audit_creation_date 2019-03-06 _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 'C42 H34 N2 S, C Cl2 D2' _chemical_formula_sum 'C43 H34 Cl2 D2 N2 S' _chemical_formula_weight 685.71 _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' Cl Cl 0.1484 0.1585 '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 0.0061 0.0033 '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 monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.1029(6) _cell_length_b 8.0200(4) _cell_length_c 36.8781(19) _cell_angle_alpha 90 _cell_angle_beta 99.1232(15) _cell_angle_gamma 90 _cell_volume 3534.3(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9934 _cell_measurement_temperature 200 _cell_measurement_theta_max 24.00 _cell_measurement_theta_min 2.24 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.277 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.9452 _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 0.1591 before and 0.0580 after correction. The Ratio of minimum to maximum transmission is 0.9452. 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 1.289 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description tablet _exptl_crystal_F_000 1432 _exptl_crystal_size_max 0.503 _exptl_crystal_size_mid 0.275 _exptl_crystal_size_min 0.062 _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 (340, 340, 189 and 127 scans of 0.5\% width, 10s exposure), every run at a different \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. ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_unetI/netI 0.0434 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_number 34143 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 24.996 _diffrn_reflns_theta_max 24.996 _diffrn_reflns_theta_min 2.194 _diffrn_ambient_temperature 200 _diffrn_detector 'Bruker PHOTON 100 CMOS' _diffrn_detector_area_resol_mean 10.4 _diffrn_detector_type 'CMOS sensor' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device '3-circle area detector diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method \w-scan _diffrn_measurement_specimen_support 'MiTeGen loop' _diffrn_radiation_monochromator 'focusing mirrors' _diffrn_radiation_probe X-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\mS microsource' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 4363 _reflns_number_total 6222 _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 v8.38A (Bruker, 2017)' _computing_data_collection 'APEX3 v.2016.1-0 (Bruker, 2016)' _computing_data_reduction 'SAINT v8.38A (Bruker, 2017)' _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, 2015)' _computing_structure_solution 'SHELXS 2013/1 (Sheldrick, 2008)' _refine_diff_density_max 0.248 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.041 _refine_ls_extinction_coef 0.0032(3) _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, 2015)' _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 465 _refine_ls_number_reflns 6222 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0495 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+2.1131P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1025 _refine_ls_wR_factor_ref 0.1158 _refine_special_details ; C(27), C(28), C(29), C(30), C(32), C(41) and C(42) with the attached hydrogens, are disordered between two positions, A and B, with occupancies 0.572(9) and 0.428(9), respectively. The CD~2~Cl~2~ molecule is disordered between two orientations, A and B, pivoting around the C atom, with occupancies 0.7 and 0.3. Methyl groups C(39)H~3~ and C(40)H~3~ 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, All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C32B-C31 \\sim C32A-C31 \\sim C33-C32A \\sim C33-C32B with sigma of 0.02 C42A-C32A \\sim C41B-C32B \\sim C42B-C32B \\sim C41A-C32A with sigma of 0.02 C30B-C29B \\sim C30A-C29A with sigma of 0.02 C29B-C28B \\sim C29A-C28A with sigma of 0.02 C28A-C27A \\sim C28B-C27B with sigma of 0.02 C27A-C26 \\sim C27B-C26 with sigma of 0.02 C31-C30B \\sim C31-C30A with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uiso(C32A) = Uiso(C32B) Uiso(C27A) = Uiso(C27B) Uanis(C29A) = Uanis(C29B) Uanis(C30A) = Uanis(C30B) Uiso(C28A) = Uiso(C28B) 4. Others Sof(C27B)=Sof(H27B)=Sof(C28B)=Sof(H28B)=Sof(C29B)=Sof(H29B)=Sof(C30B)= Sof(H30B)=Sof(C32B)=Sof(C41B)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C42B)= Sof(H42A)=Sof(H42B)=Sof(H42C)=Sof(D43D)=Sof(D43C)=1-FVAR(1) Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)= Sof(H30A)=Sof(C32A)=Sof(C41A)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42A)= Sof(H42D)=Sof(H42E)=Sof(H42F)=Sof(D43B)=Sof(D43A)=FVAR(1) Uiso(H39A)=Uiso(H39B)=Uiso(H39C)=FVAR(2) Uiso(H40A)=Uiso(H40B)=Uiso(H40C)=FVAR(3) Fixed Sof: Cl1A(0.7) Cl2A(0.7) Cl1B(0.3) Cl2B(0.3) 5.a Secondary CH2 refined with riding coordinates: C43(D43B,D43A), C43(D43D,D43C) 5.b Me refined with riding coordinates: C41A(H41A,H41B,H41C), C42A(H42D,H42E,H42F), C41B(H41D,H41E,H41F), C42B(H42A, H42B,H42C) 5.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C5(H5), C8(H8), C10(H10), C11(H11), C14(H14), C15(H15), C16(H16), C17(H17), C21(H21), C22(H22), C23(H23), C24(H24), C34(H34), C35(H35), C36(H36), C37(H37), C27A(H27A), C28A(H28A), C29A(H29A), C30A(H30A), C27B(H27B), C28B(H28B), C29B(H29B), C30B(H30B) 5.d Idealised Me refined as rotating group: C39(H39A,H39B,H39C), C40(H40A,H40B,H40C) ; _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 0.14099(5) -0.15327(8) 0.57069(2) 0.03961(19) Uani 1 1 d . . . . . N1 N 0.26922(14) 0.3474(2) 0.46665(5) 0.0311(5) Uani 1 1 d . . . . . N2 N 0.34965(15) 0.3542(2) 0.67671(5) 0.0337(5) Uani 1 1 d . . . . . C1 C 0.17295(18) -0.0179(3) 0.53678(6) 0.0316(5) Uani 1 1 d . . . . . C2 C 0.1479(2) -0.0422(3) 0.49889(6) 0.0383(6) Uani 1 1 d . . . . . H2 H 0.110119 -0.139877 0.489039 0.046 Uiso 1 1 calc R . . . . C3 C 0.17923(19) 0.0788(3) 0.47621(6) 0.0380(6) Uani 1 1 d . . . . . H3 H 0.162212 0.064886 0.450345 0.046 Uiso 1 1 calc R . . . . C4 C 0.23568(18) 0.2219(3) 0.49053(6) 0.0308(5) Uani 1 1 d . . . . . C5 C 0.26006(17) 0.2457(3) 0.52765(6) 0.0274(5) Uani 1 1 d . . . . . H5 H 0.298356 0.343416 0.537257 0.033 Uiso 1 1 calc R . . . . C6 C 0.22831(17) 0.1256(3) 0.55127(6) 0.0256(5) Uani 1 1 d . . . . . C7 C 0.24507(17) 0.1261(3) 0.59108(6) 0.0266(5) Uani 1 1 d . . . . . C8 C 0.29342(17) 0.2487(3) 0.61510(6) 0.0285(5) Uani 1 1 d . . . . . H8 H 0.321474 0.348017 0.605841 0.034 Uiso 1 1 calc R . . . . C9 C 0.30043(18) 0.2257(3) 0.65225(6) 0.0309(5) Uani 1 1 d . . . . . C10 C 0.25886(19) 0.0806(3) 0.66598(6) 0.0376(6) Uani 1 1 d . . . . . H10 H 0.264518 0.066404 0.691790 0.045 Uiso 1 1 calc R . . . . C11 C 0.20995(19) -0.0421(3) 0.64294(6) 0.0370(6) Uani 1 1 d . . . . . H11 H 0.181868 -0.140790 0.652428 0.044 Uiso 1 1 calc R . . . . C12 C 0.20261(18) -0.0180(3) 0.60527(6) 0.0306(5) Uani 1 1 d . . . . . C13 C 0.36353(18) 0.3177(3) 0.44951(6) 0.0317(5) Uani 1 1 d . . . . . C14 C 0.4208(2) 0.1667(3) 0.45394(7) 0.0434(6) Uani 1 1 d . . . . . H14 H 0.399377 0.084129 0.469937 0.052 Uiso 1 1 calc R . . . . C15 C 0.5088(2) 0.1367(4) 0.43509(8) 0.0565(8) Uani 1 1 d . . . . . H15 H 0.548583 0.034303 0.438529 0.068 Uiso 1 1 calc R . . . . C16 C 0.5389(2) 0.2537(4) 0.41153(9) 0.0618(9) Uani 1 1 d . . . . . H16 H 0.596896 0.230510 0.397652 0.074 Uiso 1 1 calc R . . . . C17 C 0.4848(2) 0.4058(4) 0.40799(8) 0.0516(7) Uani 1 1 d . . . . . H17 H 0.506698 0.487000 0.391774 0.062 Uiso 1 1 calc R . . . . C18 C 0.39901(19) 0.4427(3) 0.42760(6) 0.0354(6) Uani 1 1 d . . . . . C19 C 0.34910(19) 0.6155(3) 0.42941(7) 0.0375(6) Uani 1 1 d . . . . . C20 C 0.22393(19) 0.5947(3) 0.42990(6) 0.0329(6) Uani 1 1 d . . . . . C21 C 0.1432(2) 0.7025(3) 0.41240(7) 0.0411(6) Uani 1 1 d . . . . . H21 H 0.164475 0.786295 0.396639 0.049 Uiso 1 1 calc R . . . . C22 C 0.0326(2) 0.6914(3) 0.41729(8) 0.0478(7) Uani 1 1 d . . . . . H22 H -0.021598 0.766033 0.404866 0.057 Uiso 1 1 calc R . . . . C23 C 0.0018(2) 0.5715(3) 0.44025(8) 0.0461(7) Uani 1 1 d . . . . . H23 H -0.073444 0.565980 0.444509 0.055 Uiso 1 1 calc R . . . . C24 C 0.07957(19) 0.4588(3) 0.45723(7) 0.0380(6) Uani 1 1 d . . . . . H24 H 0.057333 0.375518 0.472922 0.046 Uiso 1 1 calc R . . . . C25 C 0.19003(18) 0.4666(3) 0.45147(6) 0.0299(5) Uani 1 1 d . . . . . C26 C 0.46050(18) 0.3343(3) 0.69404(6) 0.0293(5) Uani 1 1 d D . . . . C31 C 0.5088(2) 0.4547(3) 0.71916(6) 0.0365(6) Uani 1 1 d D . . . . C33 C 0.3221(2) 0.5886(3) 0.71601(6) 0.0338(6) Uani 1 1 d D . . . . C34 C 0.2471(2) 0.6925(3) 0.72988(7) 0.0462(7) Uani 1 1 d . . . . . H34 H 0.275492 0.773559 0.747727 0.055 Uiso 1 1 calc R . . . . C35 C 0.1333(3) 0.6824(4) 0.71876(8) 0.0556(8) Uani 1 1 d . . . . . H35 H 0.084032 0.753681 0.729180 0.067 Uiso 1 1 calc R . . . . C36 C 0.0919(2) 0.5679(3) 0.69239(8) 0.0494(7) Uani 1 1 d . . . . . H36 H 0.013687 0.562253 0.683966 0.059 Uiso 1 1 calc R . . . . C37 C 0.1632(2) 0.4610(3) 0.67805(7) 0.0392(6) Uani 1 1 d . . . . . H37 H 0.133994 0.382251 0.659786 0.047 Uiso 1 1 calc R . . . . C38 C 0.27801(19) 0.4686(3) 0.69031(6) 0.0323(6) Uani 1 1 d . . . . . C39 C 0.4009(2) 0.6944(3) 0.46633(7) 0.0462(7) Uani 1 1 d . . . . . H39A H 0.389133 0.620250 0.486490 0.056(4) Uiso 1 1 calc GR . . . . H39B H 0.365272 0.802227 0.469211 0.056(4) Uiso 1 1 calc GR . . . . H39C H 0.481374 0.710780 0.466751 0.056(4) Uiso 1 1 calc GR . . . . C40 C 0.3730(2) 0.7295(4) 0.39838(8) 0.0579(8) Uani 1 1 d . . . . . H40A H 0.454098 0.739351 0.399190 0.072(5) Uiso 1 1 calc GR . . . . H40B H 0.341141 0.840019 0.401321 0.072(5) Uiso 1 1 calc GR . . . . H40C H 0.339222 0.682074 0.374708 0.072(5) Uiso 1 1 calc GR . . . . C27A C 0.5204(6) 0.1958(10) 0.6881(2) 0.0355(9) Uiso 0.572(9) 1 d D . P A 1 H27A H 0.489326 0.116073 0.670291 0.043 Uiso 0.572(9) 1 calc R . P A 1 C28A C 0.6252(4) 0.1708(7) 0.70771(17) 0.0421(10) Uiso 0.572(9) 1 d D . P A 1 H28A H 0.667249 0.075623 0.702867 0.050 Uiso 0.572(9) 1 calc R . P A 1 C29A C 0.6696(8) 0.2821(11) 0.7342(3) 0.059(2) Uani 0.572(9) 1 d D . P A 1 H29A H 0.741839 0.262205 0.747816 0.071 Uiso 0.572(9) 1 calc R . P A 1 C30A C 0.6112(6) 0.4222(12) 0.7414(2) 0.0416(16) Uani 0.572(9) 1 d D . P A 1 H30A H 0.639858 0.495122 0.760907 0.050 Uiso 0.572(9) 1 calc R . P A 1 C32A C 0.4475(6) 0.6154(9) 0.7246(2) 0.0383(8) Uiso 0.572(9) 1 d D . P A 1 C41A C 0.4787(8) 0.7380(9) 0.6952(3) 0.071(2) Uani 0.572(9) 1 d D . P A 1 H41A H 0.441368 0.845149 0.697353 0.106 Uiso 0.572(9) 1 calc R . P A 1 H41B H 0.559941 0.754642 0.699106 0.106 Uiso 0.572(9) 1 calc R . P A 1 H41C H 0.454461 0.691496 0.670675 0.106 Uiso 0.572(9) 1 calc R . P A 1 C42A C 0.4740(9) 0.6880(15) 0.7638(3) 0.107(5) Uani 0.572(9) 1 d D . P A 1 H42D H 0.431448 0.791182 0.765126 0.160 Uiso 0.572(9) 1 calc R . P A 1 H42E H 0.452968 0.606970 0.781399 0.160 Uiso 0.572(9) 1 calc R . P A 1 H42F H 0.554198 0.711824 0.769720 0.160 Uiso 0.572(9) 1 calc R . P A 1 C27B C 0.5251(8) 0.1979(14) 0.6831(3) 0.0355(9) Uiso 0.428(9) 1 d D . P A 2 H27B H 0.488953 0.116435 0.666645 0.043 Uiso 0.428(9) 1 calc R . P A 2 C28B C 0.6384(6) 0.1820(9) 0.6959(2) 0.0421(10) Uiso 0.428(9) 1 d D . P A 2 H28B H 0.679814 0.090400 0.688758 0.050 Uiso 0.428(9) 1 calc R . P A 2 C29B C 0.6896(11) 0.3033(15) 0.7193(3) 0.059(2) Uani 0.428(9) 1 d D . P A 2 H29B H 0.766788 0.295372 0.729216 0.071 Uiso 0.428(9) 1 calc R . P A 2 C30B C 0.6264(8) 0.4363(17) 0.7282(3) 0.0416(16) Uani 0.428(9) 1 d D . P A 2 H30B H 0.665838 0.524582 0.741705 0.050 Uiso 0.428(9) 1 calc R . P A 2 C32B C 0.4484(7) 0.6064(12) 0.7287(3) 0.0383(8) Uiso 0.428(9) 1 d D . P A 2 C41B C 0.4877(11) 0.7614(14) 0.7094(2) 0.047(3) Uiso 0.428(9) 1 d D . P A 2 H41D H 0.447215 0.859949 0.715998 0.071 Uiso 0.428(9) 1 calc R . P A 2 H41E H 0.568202 0.777461 0.717356 0.071 Uiso 0.428(9) 1 calc R . P A 2 H41F H 0.472706 0.745330 0.682776 0.071 Uiso 0.428(9) 1 calc R . P A 2 C42B C 0.4850(13) 0.6372(16) 0.7697(3) 0.055(3) Uiso 0.428(9) 1 d D . P A 2 H42A H 0.447068 0.736402 0.777142 0.082 Uiso 0.428(9) 1 calc R . P A 2 H42B H 0.465417 0.540362 0.783591 0.082 Uiso 0.428(9) 1 calc R . P A 2 H42C H 0.566199 0.654459 0.774658 0.082 Uiso 0.428(9) 1 calc R . P A 2 C43 C 0.8013(4) 0.7549(6) 0.63689(11) 0.1317(19) Uani 1 1 d . . . . . D43B D 0.730441 0.802086 0.623800 0.158 Uiso 0.572(9) 1 calc R . P A 1 D43A D 0.833674 0.685953 0.618942 0.158 Uiso 0.572(9) 1 calc R . P A 1 D43D D 0.804780 0.640471 0.627088 0.158 Uiso 0.428(9) 1 calc R . P A 2 D43C D 0.730658 0.806421 0.624762 0.158 Uiso 0.428(9) 1 calc R . P A 2 Cl1A Cl 0.76843(13) 0.6259(3) 0.66962(5) 0.1081(6) Uani 0.7 1 d . . P B 1 Cl2A Cl 0.8896(2) 0.9157(2) 0.64881(6) 0.1289(9) Uani 0.7 1 d . . P B 1 Cl1B Cl 0.7996(3) 0.7435(6) 0.68641(12) 0.1070(13) Uani 0.3 1 d . . P B 2 Cl2B Cl 0.9026(4) 0.8584(7) 0.62707(11) 0.1037(15) Uani 0.3 1 d . . P B 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 0.0435(4) 0.0297(3) 0.0433(4) -0.0005(3) -0.0001(3) -0.0115(3) N1 0.0261(10) 0.0341(11) 0.0341(11) 0.0022(9) 0.0080(8) 0.0036(9) N2 0.0290(11) 0.0357(12) 0.0356(11) -0.0113(9) 0.0032(8) 0.0027(9) C1 0.0259(12) 0.0293(13) 0.0381(14) -0.0029(11) 0.0007(10) 0.0002(10) C2 0.0372(14) 0.0341(14) 0.0419(15) -0.0099(12) 0.0010(11) -0.0068(11) C3 0.0384(14) 0.0420(15) 0.0318(13) -0.0052(12) 0.0004(11) -0.0012(12) C4 0.0268(12) 0.0321(14) 0.0337(13) 0.0006(11) 0.0054(10) 0.0030(11) C5 0.0207(12) 0.0269(12) 0.0343(13) -0.0038(10) 0.0029(9) 0.0018(10) C6 0.0209(11) 0.0235(12) 0.0320(12) -0.0026(10) 0.0028(9) 0.0028(10) C7 0.0192(11) 0.0255(13) 0.0349(13) -0.0012(10) 0.0034(9) 0.0013(9) C8 0.0224(12) 0.0275(13) 0.0358(13) -0.0006(10) 0.0051(9) 0.0002(10) C9 0.0267(12) 0.0309(13) 0.0350(13) -0.0046(11) 0.0047(10) 0.0023(10) C10 0.0386(14) 0.0440(16) 0.0293(13) 0.0022(12) 0.0024(11) 0.0029(12) C11 0.0366(14) 0.0343(14) 0.0399(14) 0.0067(12) 0.0052(11) -0.0032(11) C12 0.0258(12) 0.0277(13) 0.0374(13) -0.0003(11) 0.0022(10) -0.0005(10) C13 0.0224(12) 0.0381(14) 0.0336(13) -0.0044(11) 0.0018(9) 0.0004(11) C14 0.0324(14) 0.0418(16) 0.0555(16) -0.0011(13) 0.0057(12) 0.0060(12) C15 0.0342(16) 0.0534(19) 0.083(2) -0.0080(17) 0.0133(15) 0.0114(14) C16 0.0384(17) 0.069(2) 0.084(2) -0.0125(19) 0.0291(15) 0.0070(16) C17 0.0360(15) 0.0596(19) 0.0633(18) -0.0008(15) 0.0207(13) -0.0027(14) C18 0.0263(13) 0.0417(15) 0.0388(14) -0.0008(12) 0.0068(10) -0.0017(11) C19 0.0299(13) 0.0387(15) 0.0445(14) 0.0036(12) 0.0082(11) -0.0013(11) C20 0.0313(13) 0.0336(14) 0.0329(13) -0.0037(11) 0.0027(10) 0.0015(11) C21 0.0434(16) 0.0350(15) 0.0432(15) 0.0022(12) 0.0013(12) 0.0049(12) C22 0.0345(15) 0.0400(16) 0.0644(18) -0.0057(14) -0.0056(13) 0.0104(13) C23 0.0271(14) 0.0421(16) 0.0688(18) -0.0107(15) 0.0067(12) 0.0036(12) C24 0.0307(14) 0.0353(14) 0.0494(15) -0.0049(12) 0.0105(11) 0.0006(12) C25 0.0267(13) 0.0317(13) 0.0309(12) -0.0067(11) 0.0035(10) 0.0018(10) C26 0.0306(13) 0.0302(13) 0.0269(12) 0.0050(10) 0.0033(9) -0.0008(10) C31 0.0387(14) 0.0300(14) 0.0380(14) 0.0036(11) -0.0029(11) -0.0032(11) C33 0.0472(15) 0.0281(13) 0.0273(12) 0.0032(11) 0.0096(10) 0.0017(11) C34 0.0629(19) 0.0385(16) 0.0383(15) -0.0026(12) 0.0118(13) 0.0112(14) C35 0.063(2) 0.0512(18) 0.0565(18) 0.0017(15) 0.0226(15) 0.0256(16) C36 0.0388(16) 0.0501(18) 0.0609(18) 0.0084(15) 0.0133(13) 0.0108(14) C37 0.0363(15) 0.0374(15) 0.0441(15) 0.0015(12) 0.0070(11) 0.0053(12) C38 0.0365(14) 0.0326(13) 0.0296(12) 0.0049(11) 0.0104(10) 0.0024(11) C39 0.0359(15) 0.0422(16) 0.0588(17) -0.0050(14) 0.0021(12) -0.0071(12) C40 0.0501(18) 0.060(2) 0.0660(19) 0.0159(16) 0.0174(14) -0.0021(15) C29A 0.042(4) 0.057(3) 0.072(6) 0.002(4) -0.015(4) 0.009(2) C30A 0.047(3) 0.044(2) 0.029(4) 0.003(4) -0.007(3) -0.004(2) C41A 0.071(5) 0.027(4) 0.124(8) 0.018(5) 0.044(6) 0.008(3) C42A 0.062(5) 0.144(11) 0.100(7) -0.091(7) -0.031(5) 0.028(6) C29B 0.042(4) 0.057(3) 0.072(6) 0.002(4) -0.015(4) 0.009(2) C30B 0.047(3) 0.044(2) 0.029(4) 0.003(4) -0.007(3) -0.004(2) C43 0.160(5) 0.137(4) 0.080(3) -0.002(3) -0.037(3) -0.047(4) Cl1A 0.0711(10) 0.169(2) 0.0833(11) -0.0026(12) 0.0097(8) -0.0106(11) Cl2A 0.168(2) 0.0742(12) 0.1177(16) 0.0073(12) -0.0585(15) 0.0017(12) Cl1B 0.087(3) 0.144(4) 0.100(3) 0.018(3) 0.044(2) 0.025(3) Cl2B 0.097(3) 0.144(5) 0.073(3) 0.045(3) 0.019(2) 0.015(3) _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 C1 1.745(2) . ? S1 C12 1.749(2) . ? N1 C4 1.438(3) . ? N1 C13 1.410(3) . ? N1 C25 1.406(3) . ? N2 C9 1.435(3) . ? N2 C26 1.401(3) . ? N2 C38 1.408(3) . ? C1 C2 1.396(3) . ? C1 C6 1.395(3) . ? C2 C3 1.373(3) . ? C3 C4 1.396(3) . ? C4 C5 1.367(3) . ? C5 C6 1.393(3) . ? C6 C7 1.450(3) . ? C7 C8 1.389(3) . ? C7 C12 1.399(3) . ? C8 C9 1.372(3) . ? C9 C10 1.395(3) . ? C10 C11 1.371(3) . ? C11 C12 1.391(3) . ? C13 C14 1.392(3) . ? C13 C18 1.398(3) . ? C14 C15 1.382(4) . ? C15 C16 1.367(4) . ? C16 C17 1.381(4) . ? C17 C18 1.388(3) . ? C18 C19 1.518(3) . ? C19 C20 1.527(3) . ? C19 C39 1.541(3) . ? C19 C40 1.528(3) . ? C20 C21 1.385(3) . ? C20 C25 1.400(3) . ? C21 C22 1.382(3) . ? C22 C23 1.371(4) . ? C23 C24 1.381(3) . ? C24 C25 1.388(3) . ? C26 C31 1.400(3) . ? C26 C27A 1.363(7) . ? C26 C27B 1.439(9) . ? C31 C30A 1.398(7) . ? C31 C32A 1.516(7) . ? C31 C30B 1.417(10) . ? C31 C32B 1.490(9) . ? C33 C34 1.388(3) . ? C33 C38 1.396(3) . ? C33 C32A 1.516(7) . ? C33 C32B 1.532(9) . ? C34 C35 1.376(4) . ? C35 C36 1.373(4) . ? C36 C37 1.380(3) . ? C37 C38 1.392(3) . ? C27A C28A 1.372(7) . ? C28A C29A 1.368(8) . ? C29A C30A 1.375(9) . ? C32A C41A 1.553(8) . ? C32A C42A 1.544(8) . ? C27B C28B 1.383(9) . ? C28B C29B 1.381(11) . ? C29B C30B 1.381(11) . ? C32B C41B 1.544(11) . ? C32B C42B 1.527(11) . ? C43 Cl1A 1.684(5) . ? C43 Cl2A 1.688(5) . ? C43 Cl1B 1.832(6) . ? C43 Cl2B 1.570(6) . ? 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 C1 S1 C12 91.10(11) . . ? C13 N1 C4 118.89(18) . . ? C25 N1 C4 118.64(17) . . ? C25 N1 C13 119.07(18) . . ? C26 N2 C9 118.51(18) . . ? C26 N2 C38 120.71(18) . . ? C38 N2 C9 118.30(18) . . ? C2 C1 S1 126.37(18) . . ? C6 C1 S1 112.73(16) . . ? C6 C1 C2 120.9(2) . . ? C3 C2 C1 118.3(2) . . ? C2 C3 C4 121.1(2) . . ? C3 C4 N1 120.9(2) . . ? C5 C4 N1 118.6(2) . . ? C5 C4 C3 120.6(2) . . ? C4 C5 C6 119.5(2) . . ? C1 C6 C7 111.82(19) . . ? C5 C6 C1 119.6(2) . . ? C5 C6 C7 128.5(2) . . ? C8 C7 C6 128.7(2) . . ? C8 C7 C12 119.3(2) . . ? C12 C7 C6 112.08(19) . . ? C9 C8 C7 119.6(2) . . ? C8 C9 N2 119.0(2) . . ? C8 C9 C10 120.4(2) . . ? C10 C9 N2 120.6(2) . . ? C11 C10 C9 121.2(2) . . ? C10 C11 C12 118.2(2) . . ? C7 C12 S1 112.27(16) . . ? C11 C12 S1 126.45(18) . . ? C11 C12 C7 121.3(2) . . ? C14 C13 N1 121.2(2) . . ? C14 C13 C18 119.9(2) . . ? C18 C13 N1 118.8(2) . . ? C15 C14 C13 120.1(3) . . ? C16 C15 C14 120.3(3) . . ? C15 C16 C17 119.7(3) . . ? C16 C17 C18 121.5(3) . . ? C13 C18 C19 118.0(2) . . ? C17 C18 C13 118.2(2) . . ? C17 C18 C19 123.6(2) . . ? C18 C19 C20 107.65(19) . . ? C18 C19 C39 107.7(2) . . ? C18 C19 C40 112.9(2) . . ? C20 C19 C39 107.47(19) . . ? C20 C19 C40 112.4(2) . . ? C40 C19 C39 108.5(2) . . ? C21 C20 C19 123.6(2) . . ? C21 C20 C25 118.3(2) . . ? C25 C20 C19 117.9(2) . . ? C22 C21 C20 121.7(2) . . ? C23 C22 C21 119.3(2) . . ? C22 C23 C24 120.5(2) . . ? C23 C24 C25 120.3(2) . . ? C20 C25 N1 118.85(19) . . ? C24 C25 N1 121.4(2) . . ? C24 C25 C20 119.8(2) . . ? N2 C26 C27B 118.8(5) . . ? C31 C26 N2 119.5(2) . . ? C31 C26 C27B 121.4(5) . . ? C27A C26 N2 120.9(4) . . ? C27A C26 C31 119.5(4) . . ? C26 C31 C32A 120.8(3) . . ? C26 C31 C30B 112.4(6) . . ? C26 C31 C32B 123.4(4) . . ? C30A C31 C26 119.8(4) . . ? C30A C31 C32A 119.2(5) . . ? C30B C31 C32B 122.8(7) . . ? C34 C33 C38 117.5(2) . . ? C34 C33 C32A 122.0(4) . . ? C34 C33 C32B 120.7(4) . . ? C38 C33 C32A 120.1(3) . . ? C38 C33 C32B 121.8(4) . . ? C35 C34 C33 122.5(3) . . ? C36 C35 C34 119.0(2) . . ? C35 C36 C37 120.5(3) . . ? C36 C37 C38 120.0(2) . . ? C33 C38 N2 120.0(2) . . ? C37 C38 N2 119.7(2) . . ? C37 C38 C33 120.3(2) . . ? C26 C27A C28A 120.3(7) . . ? C29A C28A C27A 120.5(7) . . ? C28A C29A C30A 121.0(8) . . ? C29A C30A C31 118.3(8) . . ? C31 C32A C33 110.3(5) . . ? C31 C32A C41A 105.5(6) . . ? C31 C32A C42A 114.3(6) . . ? C33 C32A C41A 106.8(6) . . ? C33 C32A C42A 107.5(6) . . ? C42A C32A C41A 112.1(8) . . ? C28B C27B C26 121.8(9) . . ? C29B C28B C27B 118.1(9) . . ? C30B C29B C28B 118.8(12) . . ? C29B C30B C31 126.7(12) . . ? C31 C32B C33 110.8(6) . . ? C31 C32B C41B 110.5(8) . . ? C31 C32B C42B 106.8(8) . . ? C33 C32B C41B 107.5(7) . . ? C42B C32B C33 115.9(9) . . ? C42B C32B C41B 105.2(8) . . ? Cl1A C43 Cl2A 119.6(3) . . ? Cl2B C43 Cl1B 112.9(3) . . ? _shelx_res_file ; TITL 17srv188.res created by SHELXL-2018/3 at 21:57:22 on 06-Mar-2019 CELL 0.71073 12.1029 8.02 36.8781 90 99.1232 90 ZERR 4 0.0006 0.0004 0.0019 0 0.0015 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Cl D N S UNIT 172 136 8 8 8 4 SADI C32B C31 C32A C31 C33 C32A C33 C32B SADI C42A C32A C41B C32B C42B C32B C41A C32A SADI C30B C29B C30A C29A SADI C29B C28B C29A C28A SADI C28A C27A C28B C27B SADI C27A C26 C27B C26 SADI C31 C30B C31 C30A EADP C32A C32B EADP C27A C27B EADP C29A C29B EADP C30A C30B EADP C28A C28B L.S. 7 PLAN 10 TEMP -73.15 fmap 2 acta OMIT -3 50 REM REM REM WGHT 0.040300 2.113100 EXTI 0.003170 FVAR 0.11106 0.57212 0.05612 0.07246 S1 6 0.140991 -0.153273 0.570690 11.00000 0.04352 0.02971 = 0.04331 -0.00050 -0.00012 -0.01150 N1 5 0.269225 0.347439 0.466654 11.00000 0.02608 0.03409 = 0.03414 0.00216 0.00804 0.00364 N2 5 0.349647 0.354175 0.676707 11.00000 0.02901 0.03574 = 0.03558 -0.01132 0.00319 0.00270 C1 1 0.172947 -0.017888 0.536778 11.00000 0.02594 0.02928 = 0.03810 -0.00295 0.00070 0.00023 C2 1 0.147893 -0.042155 0.498887 11.00000 0.03719 0.03406 = 0.04194 -0.00988 0.00102 -0.00681 AFIX 43 H2 2 0.110119 -0.139877 0.489039 11.00000 -1.20000 AFIX 0 C3 1 0.179233 0.078812 0.476211 11.00000 0.03842 0.04199 = 0.03182 -0.00520 0.00036 -0.00119 AFIX 43 H3 2 0.162212 0.064886 0.450345 11.00000 -1.20000 AFIX 0 C4 1 0.235679 0.221899 0.490526 11.00000 0.02677 0.03214 = 0.03370 0.00055 0.00536 0.00295 C5 1 0.260058 0.245703 0.527645 11.00000 0.02069 0.02689 = 0.03426 -0.00382 0.00287 0.00179 AFIX 43 H5 2 0.298356 0.343416 0.537257 11.00000 -1.20000 AFIX 0 C6 1 0.228307 0.125573 0.551265 11.00000 0.02086 0.02346 = 0.03196 -0.00256 0.00281 0.00284 C7 1 0.245069 0.126063 0.591079 11.00000 0.01924 0.02551 = 0.03493 -0.00118 0.00343 0.00134 C8 1 0.293424 0.248736 0.615097 11.00000 0.02236 0.02749 = 0.03576 -0.00062 0.00506 0.00018 AFIX 43 H8 2 0.321474 0.348017 0.605841 11.00000 -1.20000 AFIX 0 C9 1 0.300434 0.225685 0.652249 11.00000 0.02667 0.03091 = 0.03500 -0.00458 0.00473 0.00231 C10 1 0.258855 0.080559 0.665985 11.00000 0.03865 0.04396 = 0.02926 0.00216 0.00244 0.00287 AFIX 43 H10 2 0.264518 0.066404 0.691790 11.00000 -1.20000 AFIX 0 C11 1 0.209953 -0.042079 0.642937 11.00000 0.03659 0.03432 = 0.03988 0.00672 0.00515 -0.00321 AFIX 43 H11 2 0.181868 -0.140790 0.652428 11.00000 -1.20000 AFIX 0 C12 1 0.202606 -0.017953 0.605272 11.00000 0.02585 0.02770 = 0.03737 -0.00025 0.00218 -0.00048 C13 1 0.363529 0.317656 0.449510 11.00000 0.02241 0.03810 = 0.03362 -0.00443 0.00180 0.00035 C14 1 0.420814 0.166692 0.453937 11.00000 0.03242 0.04175 = 0.05549 -0.00110 0.00569 0.00604 AFIX 43 H14 2 0.399377 0.084129 0.469937 11.00000 -1.20000 AFIX 0 C15 1 0.508833 0.136694 0.435093 11.00000 0.03418 0.05341 = 0.08314 -0.00801 0.01333 0.01144 AFIX 43 H15 2 0.548583 0.034303 0.438529 11.00000 -1.20000 AFIX 0 C16 1 0.538945 0.253710 0.411534 11.00000 0.03841 0.06895 = 0.08431 -0.01252 0.02915 0.00695 AFIX 43 H16 2 0.596896 0.230510 0.397652 11.00000 -1.20000 AFIX 0 C17 1 0.484763 0.405825 0.407995 11.00000 0.03601 0.05957 = 0.06327 -0.00083 0.02074 -0.00275 AFIX 43 H17 2 0.506698 0.487000 0.391774 11.00000 -1.20000 AFIX 0 C18 1 0.399015 0.442706 0.427603 11.00000 0.02625 0.04169 = 0.03878 -0.00079 0.00684 -0.00166 C19 1 0.349101 0.615526 0.429411 11.00000 0.02995 0.03869 = 0.04452 0.00358 0.00816 -0.00132 C20 1 0.223935 0.594717 0.429895 11.00000 0.03128 0.03365 = 0.03290 -0.00368 0.00275 0.00146 C21 1 0.143232 0.702543 0.412400 11.00000 0.04339 0.03502 = 0.04316 0.00221 0.00133 0.00488 AFIX 43 H21 2 0.164475 0.786295 0.396639 11.00000 -1.20000 AFIX 0 C22 1 0.032576 0.691421 0.417285 11.00000 0.03453 0.04000 = 0.06440 -0.00569 -0.00563 0.01041 AFIX 43 H22 2 -0.021598 0.766033 0.404866 11.00000 -1.20000 AFIX 0 C23 1 0.001849 0.571541 0.440248 11.00000 0.02707 0.04209 = 0.06878 -0.01066 0.00667 0.00360 AFIX 43 H23 2 -0.073444 0.565980 0.444509 11.00000 -1.20000 AFIX 0 C24 1 0.079574 0.458777 0.457233 11.00000 0.03072 0.03532 = 0.04938 -0.00494 0.01049 0.00055 AFIX 43 H24 2 0.057333 0.375518 0.472922 11.00000 -1.20000 AFIX 0 C25 1 0.190028 0.466631 0.451469 11.00000 0.02673 0.03167 = 0.03089 -0.00671 0.00347 0.00183 C26 1 0.460502 0.334342 0.694038 11.00000 0.03057 0.03020 = 0.02687 0.00503 0.00334 -0.00083 C31 1 0.508751 0.454670 0.719161 11.00000 0.03871 0.02995 = 0.03797 0.00362 -0.00286 -0.00316 C33 1 0.322099 0.588625 0.716005 11.00000 0.04723 0.02811 = 0.02728 0.00319 0.00965 0.00165 C34 1 0.247145 0.692455 0.729877 11.00000 0.06288 0.03854 = 0.03830 -0.00255 0.01182 0.01124 AFIX 43 H34 2 0.275492 0.773559 0.747727 11.00000 -1.20000 AFIX 0 C35 1 0.133295 0.682416 0.718759 11.00000 0.06333 0.05117 = 0.05654 0.00173 0.02262 0.02558 AFIX 43 H35 2 0.084032 0.753681 0.729180 11.00000 -1.20000 AFIX 0 C36 1 0.091949 0.567933 0.692394 11.00000 0.03877 0.05015 = 0.06093 0.00844 0.01333 0.01078 AFIX 43 H36 2 0.013687 0.562253 0.683966 11.00000 -1.20000 AFIX 0 C37 1 0.163243 0.461044 0.678046 11.00000 0.03629 0.03744 = 0.04413 0.00149 0.00704 0.00530 AFIX 43 H37 2 0.133994 0.382251 0.659786 11.00000 -1.20000 AFIX 0 C38 1 0.278010 0.468596 0.690312 11.00000 0.03648 0.03262 = 0.02963 0.00492 0.01045 0.00239 C39 1 0.400940 0.694376 0.466327 11.00000 0.03592 0.04218 = 0.05880 -0.00505 0.00212 -0.00709 AFIX 137 H39A 2 0.389133 0.620250 0.486490 11.00000 31.00000 H39B 2 0.365272 0.802227 0.469211 11.00000 31.00000 H39C 2 0.481374 0.710780 0.466751 11.00000 31.00000 AFIX 0 C40 1 0.373036 0.729454 0.398376 11.00000 0.05013 0.06017 = 0.06599 0.01593 0.01742 -0.00211 AFIX 137 H40A 2 0.454098 0.739351 0.399190 11.00000 41.00000 H40B 2 0.341141 0.840019 0.401321 11.00000 41.00000 H40C 2 0.339222 0.682074 0.374708 11.00000 41.00000 AFIX 0 PART 1 C27A 1 0.520362 0.195758 0.688097 21.00000 0.03545 AFIX 43 H27A 2 0.489326 0.116073 0.670291 21.00000 -1.20000 AFIX 0 C28A 1 0.625197 0.170813 0.707707 21.00000 0.04207 AFIX 43 H28A 2 0.667249 0.075623 0.702867 21.00000 -1.20000 AFIX 0 C29A 1 0.669626 0.282056 0.734187 21.00000 0.04213 0.05707 = 0.07152 0.00181 -0.01473 0.00865 AFIX 43 H29A 2 0.741839 0.262205 0.747816 21.00000 -1.20000 AFIX 0 C30A 1 0.611248 0.422200 0.741358 21.00000 0.04723 0.04447 = 0.02882 0.00253 -0.00734 -0.00416 AFIX 43 H30A 2 0.639858 0.495122 0.760907 21.00000 -1.20000 AFIX 0 C32A 1 0.447545 0.615351 0.724606 21.00000 0.03826 C41A 1 0.478704 0.737976 0.695223 21.00000 0.07107 0.02723 = 0.12397 0.01839 0.04449 0.00771 AFIX 33 H41A 2 0.441368 0.845149 0.697353 21.00000 -1.50000 H41B 2 0.559941 0.754642 0.699106 21.00000 -1.50000 H41C 2 0.454461 0.691496 0.670675 21.00000 -1.50000 AFIX 0 C42A 1 0.473950 0.687960 0.763789 21.00000 0.06162 0.14449 = 0.10012 -0.09075 -0.03095 0.02850 AFIX 33 H42D 2 0.431448 0.791182 0.765126 21.00000 -1.50000 H42E 2 0.452968 0.606970 0.781399 21.00000 -1.50000 H42F 2 0.554198 0.711824 0.769720 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C27B 1 0.525117 0.197886 0.683105 -21.00000 0.03545 AFIX 43 H27B 2 0.488953 0.116435 0.666645 -21.00000 -1.20000 AFIX 0 C28B 1 0.638403 0.182040 0.695896 -21.00000 0.04207 AFIX 43 H28B 2 0.679814 0.090400 0.688758 -21.00000 -1.20000 AFIX 0 C29B 1 0.689551 0.303292 0.719344 -21.00000 0.04213 0.05707 = 0.07152 0.00181 -0.01473 0.00865 AFIX 43 H29B 2 0.766788 0.295372 0.729216 -21.00000 -1.20000 AFIX 0 C30B 1 0.626377 0.436304 0.728183 -21.00000 0.04723 0.04447 = 0.02882 0.00253 -0.00734 -0.00416 AFIX 43 H30B 2 0.665838 0.524582 0.741705 -21.00000 -1.20000 AFIX 0 C32B 1 0.448364 0.606364 0.728682 -21.00000 0.03826 C41B 1 0.487715 0.761438 0.709446 -21.00000 0.04718 AFIX 33 H41D 2 0.447215 0.859949 0.715998 -21.00000 -1.50000 H41E 2 0.568202 0.777461 0.717356 -21.00000 -1.50000 H41F 2 0.472706 0.745330 0.682776 -21.00000 -1.50000 AFIX 0 C42B 1 0.485048 0.637155 0.769692 -21.00000 0.05455 AFIX 33 H42A 2 0.447068 0.736402 0.777142 -21.00000 -1.50000 H42B 2 0.465417 0.540362 0.783591 -21.00000 -1.50000 H42C 2 0.566199 0.654459 0.774658 -21.00000 -1.50000 AFIX 0 PART 0 C43 1 0.801293 0.754939 0.636891 11.00000 0.15988 0.13705 = 0.07998 -0.00180 -0.03723 -0.04662 PART 1 AFIX 23 D43B 4 0.730441 0.802086 0.623800 21.00000 -1.20000 D43A 4 0.833674 0.685953 0.618942 21.00000 -1.20000 AFIX 23 PART 0 PART 2 D43D 4 0.804780 0.640471 0.627088 -21.00000 -1.20000 D43C 4 0.730658 0.806421 0.624762 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 CL1A 3 0.768426 0.625942 0.669616 10.70000 0.07107 0.16898 = 0.08330 -0.00255 0.00968 -0.01060 CL2A 3 0.889641 0.915658 0.648808 10.70000 0.16844 0.07417 = 0.11767 0.00725 -0.05847 0.00168 PART 0 PART 2 CL1B 3 0.799562 0.743543 0.686408 10.30000 0.08680 0.14354 = 0.10023 0.01824 0.04401 0.02454 CL2B 3 0.902639 0.858380 0.627069 10.30000 0.09690 0.14351 = 0.07266 0.04463 0.01928 0.01525 HKLF 4 REM REM wR2 = 0.1158, GooF = S = 1.042, Restrained GooF = 1.043 for all data REM R1 = 0.0495 for 4363 Fo > 4sig(Fo) and 0.0832 for all 6222 data REM 465 parameters refined using 17 restraints END WGHT 0.0397 2.1644 REM Highest difference peak 0.248, deepest hole -0.289, 1-sigma level 0.041 Q1 1 0.7370 0.9005 0.6533 11.00000 0.05 0.25 Q2 1 0.6234 0.1610 0.7281 11.00000 0.05 0.24 Q3 1 0.7018 0.8482 0.6473 11.00000 0.05 0.24 Q4 1 0.7282 0.7632 0.6656 11.00000 0.05 0.22 Q5 1 0.1344 -0.0167 0.5203 11.00000 0.05 0.22 Q6 1 0.3946 0.6063 0.7287 11.00000 0.05 0.21 Q7 1 0.4889 0.5570 0.7288 11.00000 0.05 0.21 Q8 1 0.9194 0.9002 0.6356 11.00000 0.05 0.21 Q9 1 0.7777 0.7348 0.6237 11.00000 0.05 0.21 Q10 1 0.6650 0.2399 0.7040 11.00000 0.05 0.21 ; _shelx_res_checksum 27646 _olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems' _olex2_submission_special_instructions 'No special instructions were received' _exptl_crystal_preparation Luminescent