#------------------------------------------------------------------------------ #$Date: 2024-12-06 22:39:49 +0200 (Fri, 06 Dec 2024) $ #$Revision: 296700 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/16/01/7160171.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7160171 loop_ _publ_author_name 'Kaur, Ramandeep' 'Dilip, Haritha' 'Kirubakaran, Sivapriya' 'Babu, Srinivasarao Arulananda' _publ_section_title ; Synthesis of biaryl-based carbazoles via C-H functionalization and exploration of their anticancer activities. ; _journal_issue 45 _journal_name_full 'Organic & biomolecular chemistry' _journal_page_first 8916 _journal_page_last 8944 _journal_paper_doi 10.1039/d4ob01392a _journal_volume 22 _journal_year 2024 _chemical_formula_moiety 'C31 H25 N3 O3 S' _chemical_formula_sum 'C31 H27 N3 O3 S' _chemical_formula_weight 521.61 _chemical_name_systematic c31h27n3o3S _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-07-06 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2024-08-18 deposited with the CCDC. 2024-10-03 downloaded from the CCDC. ; _cell_angle_alpha 92.965(7) _cell_angle_beta 109.135(8) _cell_angle_gamma 96.379(8) _cell_formula_units_Z 2 _cell_length_a 8.8101(9) _cell_length_b 12.3193(11) _cell_length_c 13.1329(10) _cell_measurement_reflns_used 2255 _cell_measurement_temperature 273 _cell_measurement_theta_max 25.9230 _cell_measurement_theta_min 2.8690 _cell_volume 1332.4(2) _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 273 _diffrn_detector CCD _diffrn_detector_area_resol_mean 28.5714 _diffrn_detector_type 'Rigaku Saturn724+' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.837 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -66.00 26.00 1.00 12.03 -- 29.89 54.00 30.00 92 2 \w 94.00 119.00 1.00 12.03 -- 29.89 54.00-180.00 25 3 \w -69.00 114.00 1.00 12.03 -- 29.89 54.00 -90.00 183 ; _diffrn_measurement_device 'AFC12 (Right): Kappa 3 circle' _diffrn_measurement_device_type 'Rigaku Saturn724+ (2x2 bin mode)' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_measurement_specimen_support 'Mitegen 50um' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0374059000 _diffrn_orient_matrix_UB_12 -0.0483730000 _diffrn_orient_matrix_UB_13 0.0090188000 _diffrn_orient_matrix_UB_21 -0.0229772000 _diffrn_orient_matrix_UB_22 -0.0130878000 _diffrn_orient_matrix_UB_23 -0.0567083000 _diffrn_orient_matrix_UB_31 0.0739684000 _diffrn_orient_matrix_UB_32 0.0295820000 _diffrn_orient_matrix_UB_33 0.0002638000 _diffrn_radiation_collimation 0.3 _diffrn_radiation_monochromator Confocal _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_unetI/netI 0.0691 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.837 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 10115 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.837 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.709 _diffrn_reflns_theta_min 2.788 _diffrn_source 'Rotating Anode' _diffrn_source_current 24.0 _diffrn_source_power 1.2 _diffrn_source_target Mo _diffrn_source_type 'Rotating Anode' _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.87595 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'dull brownish brown' _exptl_crystal_colour_lustre dull _exptl_crystal_colour_modifier brownish _exptl_crystal_colour_primary brown _exptl_crystal_density_diffrn 1.300 _exptl_crystal_description block _exptl_crystal_F_000 548 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.358 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.045 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 346 _refine_ls_number_reflns 8214 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.022 _refine_ls_R_factor_all 0.1261 _refine_ls_R_factor_gt 0.0599 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0724P)^2^+0.0292P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1460 _refine_ls_wR_factor_ref 0.1980 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4088 _reflns_number_total 8214 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ob01392a2.cif _cod_data_source_block rd319 _cod_depositor_comments 'Adding full bibliography for 7160171.cif.' _cod_database_code 7160171 _shelx_shelxl_version_number 2018/3 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: N005(H005), C00A(H00A), C00I(H00I), C00J(H00J), C00L(H00L), C00M(H00M), C00N(H00N), C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y), C00Z(H00Z) 2.b Idealised Me refined as rotating group: C010(H01A,H01B,H01C), C011(H01D,H01E,H01F), C012(H01G,H01H,H01I) ; _shelx_res_file ; TITL rd319_a.res in P-1 rd319.res created by SHELXL-2018/3 at 22:13:10 on 06-Jul-2024 REM Old TITL rd 319 in P-1 REM SHELXT solution in P-1 REM R1 0.318, Rweak 0.022, Alpha 0.032, Orientation as input REM Formula found by SHELXT: C31 N4 O3 CELL 0.71073 8.8101 12.3193 13.1329 92.965 109.135 96.379 ZERR 2 0.0009 0.0011 0.001 0.007 0.008 0.008 LATT 1 SFAC C H N O S UNIT 62 54 6 6 2 L.S. 4 0 0 PLAN 1 CONF BOND $H LIST 6 MORE -1 fmap 2 53 acta REM REM REM WGHT 0.072400 0.029200 FVAR 0.64289 S001 5 -0.171276 0.770893 0.174258 11.00000 0.06595 0.07470 = 0.03805 0.01190 0.00507 0.00934 O002 4 0.253870 0.760543 0.900554 11.00000 0.05447 0.08573 = 0.03900 0.01329 0.01010 0.00049 N003 3 0.402867 0.838881 0.809155 11.00000 0.04094 0.06574 = 0.03644 0.00736 0.00825 0.00503 O004 4 0.049167 0.607270 0.203618 11.00000 0.12454 0.09057 = 0.04261 0.00861 0.03280 0.04108 N005 3 0.118713 0.607494 0.385590 11.00000 0.06343 0.05476 = 0.03746 0.00235 0.01435 0.01669 AFIX 43 H005 2 0.108334 0.641577 0.441250 11.00000 -1.20000 AFIX 0 N006 3 0.215949 0.559840 0.587512 11.00000 0.06747 0.05645 = 0.04718 0.01066 0.01769 0.00893 C007 1 0.339161 0.857839 0.627407 11.00000 0.03927 0.04069 = 0.03941 0.00509 0.01286 0.00711 O008 4 0.516003 0.824429 0.989099 11.00000 0.06202 0.17701 = 0.04465 0.02869 -0.00271 -0.01060 C009 1 0.274904 0.829305 0.709047 11.00000 0.03982 0.04659 = 0.03523 0.00267 0.00793 0.00617 C00A 1 0.239782 0.853053 0.520592 11.00000 0.04372 0.04621 = 0.03687 0.00661 0.01479 0.00690 AFIX 43 H00A 2 0.283286 0.871213 0.467068 11.00000 -1.20000 AFIX 0 C00B 1 0.074595 0.820884 0.494182 11.00000 0.04305 0.04574 = 0.03474 0.00273 0.00929 0.00652 C00C 1 0.512201 0.890783 0.680069 11.00000 0.04027 0.04534 = 0.04536 0.00665 0.01168 0.00938 C00D 1 -0.035327 0.815608 0.379904 11.00000 0.03915 0.04892 = 0.03801 0.00840 0.00784 0.00227 C00E 1 0.049201 0.647936 0.290446 11.00000 0.05709 0.05965 = 0.03836 0.00506 0.01471 0.00534 C00F 1 0.205567 0.517743 0.406761 11.00000 0.04602 0.04399 = 0.05075 0.00243 0.01346 0.00419 C00G 1 0.257744 0.495284 0.516698 11.00000 0.04735 0.04580 = 0.05571 0.00636 0.01187 0.00019 C00H 1 -0.034273 0.745252 0.295733 11.00000 0.04973 0.05768 = 0.03461 0.00762 0.00975 0.00261 C00I 1 0.012515 0.796921 0.576843 11.00000 0.03962 0.05932 = 0.04265 0.00307 0.01175 0.00121 AFIX 43 H00I 2 -0.098960 0.778657 0.559100 11.00000 -1.20000 AFIX 0 C00J 1 0.109477 0.799182 0.683714 11.00000 0.04260 0.06695 = 0.03736 0.00791 0.01343 0.00320 AFIX 43 H00J 2 0.065310 0.781101 0.736944 11.00000 -1.20000 AFIX 0 C00K 1 0.549471 0.877673 0.789951 11.00000 0.04293 0.05301 = 0.04827 0.00506 0.01033 0.00642 C00L 1 0.634581 0.929080 0.640217 11.00000 0.04628 0.05655 = 0.06364 0.01183 0.02022 0.00607 AFIX 43 H00L 2 0.610912 0.938596 0.567107 11.00000 -1.20000 AFIX 0 C00M 1 -0.150681 0.888960 0.344061 11.00000 0.05176 0.06280 = 0.05266 0.00612 0.01023 0.01511 AFIX 43 H00M 2 -0.169179 0.942099 0.389908 11.00000 -1.20000 AFIX 0 C00N 1 0.242018 0.453781 0.331396 11.00000 0.05367 0.05214 = 0.06658 -0.01059 0.01929 0.00184 AFIX 43 H00N 2 0.205314 0.467024 0.258842 11.00000 -1.20000 AFIX 0 C00O 1 0.399587 0.808061 0.909308 11.00000 0.05587 0.07818 = 0.04161 0.01141 0.00986 0.00682 C00P 1 0.352679 0.409201 0.549019 11.00000 0.04785 0.04448 = 0.07226 0.01083 0.01127 -0.00067 C00Q 1 0.218445 0.714141 0.995059 11.00000 0.06787 0.07584 = 0.03641 0.01027 0.01614 0.00095 C00R 1 0.791301 0.952586 0.711141 11.00000 0.04252 0.06549 = 0.08268 0.01302 0.01952 0.00378 AFIX 43 H00R 2 0.874191 0.979307 0.686109 11.00000 -1.20000 AFIX 0 C00S 1 0.335142 0.368125 0.364444 11.00000 0.05860 0.05394 = 0.08801 -0.00969 0.03140 0.00342 AFIX 43 H00S 2 0.359133 0.325140 0.312900 11.00000 -1.20000 AFIX 0 C00T 1 0.267167 0.540001 0.690525 11.00000 0.07751 0.06969 = 0.05066 0.01662 0.01688 0.00939 AFIX 43 H00T 2 0.238543 0.583434 0.739533 11.00000 -1.20000 AFIX 0 C00U 1 0.825795 0.936596 0.819394 11.00000 0.04049 0.07539 = 0.07769 0.00990 0.00532 0.00100 AFIX 43 H00U 2 0.932693 0.951661 0.865656 11.00000 -1.20000 AFIX 0 C00V 1 -0.231250 0.873646 0.236045 11.00000 0.05520 0.06863 = 0.05578 0.01756 0.00264 0.01526 AFIX 43 H00V 2 -0.310852 0.915081 0.199785 11.00000 -1.20000 AFIX 0 C00W 1 0.706999 0.899035 0.861163 11.00000 0.04528 0.07793 = 0.05683 0.00827 0.00432 0.00464 AFIX 43 H00W 2 0.731861 0.888534 0.934147 11.00000 -1.20000 AFIX 0 C00X 1 0.390708 0.346746 0.469522 11.00000 0.05636 0.04934 = 0.09695 0.00800 0.02479 0.00819 AFIX 43 H00X 2 0.454125 0.290747 0.489404 11.00000 -1.20000 AFIX 0 C00Y 1 0.361307 0.457971 0.729717 11.00000 0.08255 0.07677 = 0.06224 0.02836 0.01491 0.00770 AFIX 43 H00Y 2 0.394976 0.447526 0.802998 11.00000 -1.20000 AFIX 0 C00Z 1 0.402937 0.393750 0.659385 11.00000 0.06611 0.05910 = 0.08545 0.02837 0.01143 0.00906 AFIX 43 H00Z 2 0.465777 0.338575 0.684600 11.00000 -1.20000 AFIX 0 C010 1 0.042045 0.671325 0.948071 11.00000 0.07126 0.12595 = 0.06291 0.02628 0.02075 -0.01103 AFIX 137 H01A 2 -0.018302 0.730676 0.923117 11.00000 -1.50000 H01B 2 0.006596 0.638297 1.002470 11.00000 -1.50000 H01C 2 0.024432 0.617476 0.888416 11.00000 -1.50000 AFIX 0 C011 1 0.251377 0.803483 1.083485 11.00000 0.17051 0.14454 = 0.08439 -0.04601 0.07892 -0.06397 AFIX 137 H01D 2 0.365878 0.827693 1.112967 11.00000 -1.50000 H01E 2 0.213646 0.776485 1.139423 11.00000 -1.50000 H01F 2 0.195825 0.863835 1.055039 11.00000 -1.50000 AFIX 0 C012 1 0.315928 0.622536 1.027939 11.00000 0.11932 0.15264 = 0.12817 0.09251 0.05636 0.05509 AFIX 137 H01G 2 0.299889 0.572596 0.965593 11.00000 -1.50000 H01H 2 0.282002 0.584439 1.080402 11.00000 -1.50000 H01I 2 0.428700 0.651556 1.059006 11.00000 -1.50000 AFIX 0 HKLF 4 REM rd319_a.res in P-1 REM wR2 = 0.1980, GooF = S = 1.022, Restrained GooF = 1.022 for all data REM R1 = 0.0599 for 4088 Fo > 4sig(Fo) and 0.1261 for all 8214 data REM 346 parameters refined using 0 restraints END WGHT 0.0713 0.0342 REM Highest difference peak 0.358, deepest hole -0.265, 1-sigma level 0.045 Q1 1 0.2777 0.8732 0.5836 11.00000 0.05 0.20 ; _shelx_res_checksum 53674 _olex2_submission_original_sample_id 'rd 319' _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.212 _oxdiff_exptl_absorpt_empirical_full_min 0.862 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 S001 S -0.17128(8) 0.77089(6) 0.17426(5) 0.0624(2) Uani 1 1 d . . . . . O002 O 0.25387(19) 0.76054(15) 0.90055(12) 0.0616(4) Uani 1 1 d . . . . . N003 N 0.4029(2) 0.83888(16) 0.80915(14) 0.0490(4) Uani 1 1 d . . . . . O004 O 0.0492(3) 0.60727(17) 0.20362(14) 0.0825(6) Uani 1 1 d . . . . . N005 N 0.1187(2) 0.60749(15) 0.38559(14) 0.0519(5) Uani 1 1 d . . . . . H005 H 0.108334 0.641577 0.441250 0.062 Uiso 1 1 calc R U . . . N006 N 0.2159(2) 0.55984(16) 0.58751(16) 0.0572(5) Uani 1 1 d . . . . . C007 C 0.3392(2) 0.85784(16) 0.62741(16) 0.0397(4) Uani 1 1 d . . . . . O008 O 0.5160(2) 0.8244(2) 0.98910(15) 0.1012(8) Uani 1 1 d . . . . . C009 C 0.2749(2) 0.82931(17) 0.70905(15) 0.0417(4) Uani 1 1 d . . . . . C00A C 0.2398(2) 0.85305(16) 0.52059(16) 0.0418(5) Uani 1 1 d . . . . . H00A H 0.283286 0.871213 0.467068 0.050 Uiso 1 1 calc R U . . . C00B C 0.0746(2) 0.82088(17) 0.49418(16) 0.0421(5) Uani 1 1 d . . . . . C00C C 0.5122(2) 0.89078(17) 0.68007(17) 0.0440(5) Uani 1 1 d . . . . . C00D C -0.0353(2) 0.81561(17) 0.37990(16) 0.0434(5) Uani 1 1 d . . . . . C00E C 0.0492(3) 0.6479(2) 0.29045(18) 0.0522(5) Uani 1 1 d . . . . . C00F C 0.2056(2) 0.51774(18) 0.40676(18) 0.0478(5) Uani 1 1 d . . . . . C00G C 0.2577(3) 0.49528(18) 0.51670(19) 0.0514(5) Uani 1 1 d . . . . . C00H C -0.0343(3) 0.74525(19) 0.29573(16) 0.0487(5) Uani 1 1 d . . . . . C00I C 0.0125(2) 0.79692(19) 0.57684(17) 0.0482(5) Uani 1 1 d . . . . . H00I H -0.098960 0.778657 0.559100 0.058 Uiso 1 1 calc R U . . . C00J C 0.1095(2) 0.79918(19) 0.68371(17) 0.0492(5) Uani 1 1 d . . . . . H00J H 0.065310 0.781101 0.736944 0.059 Uiso 1 1 calc R U . . . C00K C 0.5495(2) 0.87767(18) 0.78995(18) 0.0493(5) Uani 1 1 d . . . . . C00L C 0.6346(3) 0.92908(19) 0.6402(2) 0.0549(6) Uani 1 1 d . . . . . H00L H 0.610912 0.938596 0.567107 0.066 Uiso 1 1 calc R U . . . C00M C -0.1507(3) 0.8890(2) 0.34406(19) 0.0569(6) Uani 1 1 d . . . . . H00M H -0.169179 0.942099 0.389908 0.068 Uiso 1 1 calc R U . . . C00N C 0.2420(3) 0.4538(2) 0.3314(2) 0.0587(6) Uani 1 1 d . . . . . H00N H 0.205314 0.467024 0.258842 0.070 Uiso 1 1 calc R U . . . C00O C 0.3996(3) 0.8081(2) 0.90931(19) 0.0601(6) Uani 1 1 d . . . . . C00P C 0.3527(3) 0.40920(19) 0.5490(2) 0.0574(6) Uani 1 1 d . . . . . C00Q C 0.2184(3) 0.7141(2) 0.99506(18) 0.0609(6) Uani 1 1 d . . . . . C00R C 0.7913(3) 0.9526(2) 0.7111(2) 0.0640(7) Uani 1 1 d . . . . . H00R H 0.874191 0.979307 0.686109 0.077 Uiso 1 1 calc R U . . . C00S C 0.3351(3) 0.3681(2) 0.3644(2) 0.0661(7) Uani 1 1 d . . . . . H00S H 0.359133 0.325140 0.312900 0.079 Uiso 1 1 calc R U . . . C00T C 0.2672(3) 0.5400(2) 0.6905(2) 0.0668(7) Uani 1 1 d . . . . . H00T H 0.238543 0.583434 0.739533 0.080 Uiso 1 1 calc R U . . . C00U C 0.8258(3) 0.9366(2) 0.8194(2) 0.0686(7) Uani 1 1 d . . . . . H00U H 0.932693 0.951661 0.865656 0.082 Uiso 1 1 calc R U . . . C00V C -0.2313(3) 0.8736(2) 0.2360(2) 0.0629(6) Uani 1 1 d . . . . . H00V H -0.310852 0.915081 0.199785 0.075 Uiso 1 1 calc R U . . . C00W C 0.7070(3) 0.8990(2) 0.8612(2) 0.0634(7) Uani 1 1 d . . . . . H00W H 0.731861 0.888534 0.934147 0.076 Uiso 1 1 calc R U . . . C00X C 0.3907(3) 0.3467(2) 0.4695(3) 0.0677(7) Uani 1 1 d . . . . . H00X H 0.454125 0.290747 0.489404 0.081 Uiso 1 1 calc R U . . . C00Y C 0.3613(3) 0.4580(3) 0.7297(2) 0.0756(8) Uani 1 1 d . . . . . H00Y H 0.394976 0.447526 0.802998 0.091 Uiso 1 1 calc R U . . . C00Z C 0.4029(3) 0.3937(2) 0.6594(2) 0.0729(8) Uani 1 1 d . . . . . H00Z H 0.465777 0.338575 0.684600 0.087 Uiso 1 1 calc R U . . . C010 C 0.0420(3) 0.6713(3) 0.9481(2) 0.0885(10) Uani 1 1 d . . . . . H01A H -0.018302 0.730676 0.923117 0.133 Uiso 1 1 calc R U . . . H01B H 0.006596 0.638297 1.002470 0.133 Uiso 1 1 calc R U . . . H01C H 0.024432 0.617476 0.888416 0.133 Uiso 1 1 calc R U . . . C011 C 0.2514(5) 0.8035(4) 1.0835(3) 0.1331(17) Uani 1 1 d . . . . . H01D H 0.365878 0.827693 1.112967 0.200 Uiso 1 1 calc R U . . . H01E H 0.213646 0.776485 1.139423 0.200 Uiso 1 1 calc R U . . . H01F H 0.195825 0.863835 1.055039 0.200 Uiso 1 1 calc R U . . . C012 C 0.3159(5) 0.6225(4) 1.0279(3) 0.1238(16) Uani 1 1 d . . . . . H01G H 0.299889 0.572596 0.965593 0.186 Uiso 1 1 calc R U . . . H01H H 0.282002 0.584439 1.080402 0.186 Uiso 1 1 calc R U . . . H01I H 0.428700 0.651556 1.059006 0.186 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S001 0.0659(4) 0.0747(5) 0.0381(3) 0.0119(3) 0.0051(3) 0.0093(3) O002 0.0545(9) 0.0857(13) 0.0390(9) 0.0133(8) 0.0101(7) 0.0005(9) N003 0.0409(9) 0.0657(12) 0.0364(9) 0.0074(8) 0.0083(7) 0.0050(8) O004 0.1245(17) 0.0906(15) 0.0426(10) 0.0086(9) 0.0328(10) 0.0411(13) N005 0.0634(12) 0.0548(11) 0.0375(9) 0.0024(8) 0.0144(8) 0.0167(9) N006 0.0675(12) 0.0564(12) 0.0472(11) 0.0107(9) 0.0177(9) 0.0089(10) C007 0.0393(10) 0.0407(11) 0.0394(10) 0.0051(8) 0.0129(8) 0.0071(8) O008 0.0620(11) 0.177(2) 0.0446(10) 0.0287(13) -0.0027(9) -0.0106(13) C009 0.0398(10) 0.0466(12) 0.0352(10) 0.0027(9) 0.0079(8) 0.0062(9) C00A 0.0437(11) 0.0462(12) 0.0369(10) 0.0066(9) 0.0148(9) 0.0069(9) C00B 0.0430(10) 0.0457(12) 0.0347(10) 0.0027(8) 0.0093(8) 0.0065(9) C00C 0.0403(10) 0.0453(12) 0.0454(12) 0.0066(9) 0.0117(9) 0.0094(9) C00D 0.0392(10) 0.0489(12) 0.0380(11) 0.0084(9) 0.0078(8) 0.0023(9) C00E 0.0571(13) 0.0597(14) 0.0384(11) 0.0051(10) 0.0147(10) 0.0053(11) C00F 0.0460(12) 0.0440(12) 0.0508(13) 0.0024(10) 0.0135(10) 0.0042(9) C00G 0.0473(12) 0.0458(12) 0.0557(14) 0.0064(10) 0.0119(10) 0.0002(10) C00H 0.0497(12) 0.0577(14) 0.0346(10) 0.0076(9) 0.0098(9) 0.0026(10) C00I 0.0396(11) 0.0593(14) 0.0427(12) 0.0031(10) 0.0118(9) 0.0012(9) C00J 0.0426(11) 0.0669(15) 0.0374(11) 0.0079(10) 0.0134(9) 0.0032(10) C00K 0.0429(11) 0.0530(13) 0.0483(13) 0.0051(10) 0.0103(9) 0.0064(10) C00L 0.0463(12) 0.0565(14) 0.0636(15) 0.0118(12) 0.0202(11) 0.0061(10) C00M 0.0518(13) 0.0628(15) 0.0527(14) 0.0061(11) 0.0102(11) 0.0151(11) C00N 0.0537(13) 0.0521(14) 0.0666(16) -0.0106(12) 0.0193(12) 0.0018(11) C00O 0.0559(14) 0.0782(18) 0.0416(12) 0.0114(12) 0.0099(11) 0.0068(12) C00P 0.0479(12) 0.0445(13) 0.0723(17) 0.0108(12) 0.0113(11) -0.0007(10) C00Q 0.0679(15) 0.0758(17) 0.0364(12) 0.0103(11) 0.0161(11) 0.0009(13) C00R 0.0425(12) 0.0655(16) 0.0827(19) 0.0130(14) 0.0195(12) 0.0038(11) C00S 0.0586(15) 0.0539(15) 0.088(2) -0.0097(14) 0.0314(14) 0.0034(12) C00T 0.0775(18) 0.0697(17) 0.0507(15) 0.0166(13) 0.0169(13) 0.0094(14) C00U 0.0405(12) 0.0754(18) 0.0777(19) 0.0099(15) 0.0053(12) 0.0010(12) C00V 0.0552(14) 0.0686(17) 0.0558(15) 0.0176(12) 0.0026(11) 0.0153(12) C00W 0.0453(12) 0.0779(18) 0.0568(15) 0.0083(13) 0.0043(11) 0.0046(12) C00X 0.0564(15) 0.0493(15) 0.097(2) 0.0080(14) 0.0248(15) 0.0082(11) C00Y 0.083(2) 0.077(2) 0.0622(18) 0.0284(15) 0.0149(15) 0.0077(15) C00Z 0.0661(17) 0.0591(16) 0.085(2) 0.0284(15) 0.0114(15) 0.0091(13) C010 0.0713(18) 0.126(3) 0.0629(18) 0.0263(18) 0.0207(15) -0.0110(18) C011 0.171(4) 0.145(4) 0.084(3) -0.046(2) 0.079(3) -0.064(3) C012 0.119(3) 0.153(4) 0.128(3) 0.093(3) 0.056(3) 0.055(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C00V S001 C00H 91.32(11) . . ? C00O O002 C00Q 121.61(18) . . ? C009 N003 C00K 107.55(16) . . ? C00O N003 C009 129.10(18) . . ? C00O N003 C00K 123.09(18) . . ? C00E N005 H005 115.4 . . ? C00E N005 C00F 129.20(19) . . ? C00F N005 H005 115.4 . . ? C00T N006 C00G 117.5(2) . . ? C009 C007 C00C 106.94(17) . . ? C00A C007 C009 120.88(18) . . ? C00A C007 C00C 132.17(18) . . ? C007 C009 N003 108.95(17) . . ? C00J C009 N003 130.82(18) . . ? C00J C009 C007 120.23(18) . . ? C007 C00A H00A 120.4 . . ? C007 C00A C00B 119.27(18) . . ? C00B C00A H00A 120.4 . . ? C00A C00B C00D 120.39(18) . . ? C00A C00B C00I 118.95(18) . . ? C00I C00B C00D 120.63(18) . . ? C00K C00C C007 108.00(17) . . ? C00L C00C C007 132.1(2) . . ? C00L C00C C00K 119.9(2) . . ? C00H C00D C00B 125.82(19) . . ? C00H C00D C00M 111.35(19) . . ? C00M C00D C00B 122.76(19) . . ? O004 C00E N005 123.5(2) . . ? O004 C00E C00H 120.6(2) . . ? N005 C00E C00H 115.84(19) . . ? N005 C00F C00G 114.44(18) . . ? C00N C00F N005 125.6(2) . . ? C00N C00F C00G 119.9(2) . . ? N006 C00G C00F 117.5(2) . . ? N006 C00G C00P 122.8(2) . . ? C00F C00G C00P 119.7(2) . . ? C00D C00H S001 111.72(17) . . ? C00D C00H C00E 133.02(19) . . ? C00E C00H S001 115.01(16) . . ? C00B C00I H00I 118.6 . . ? C00J C00I C00B 122.84(19) . . ? C00J C00I H00I 118.6 . . ? C009 C00J H00J 121.1 . . ? C00I C00J C009 117.77(19) . . ? C00I C00J H00J 121.1 . . ? C00C C00K N003 108.50(18) . . ? C00W C00K N003 129.9(2) . . ? C00W C00K C00C 121.6(2) . . ? C00C C00L H00L 120.6 . . ? C00R C00L C00C 118.8(2) . . ? C00R C00L H00L 120.6 . . ? C00D C00M H00M 123.5 . . ? C00V C00M C00D 113.0(2) . . ? C00V C00M H00M 123.5 . . ? C00F C00N H00N 120.1 . . ? C00F C00N C00S 119.7(2) . . ? C00S C00N H00N 120.1 . . ? O002 C00O N003 110.45(19) . . ? O008 C00O O002 127.2(2) . . ? O008 C00O N003 122.4(2) . . ? C00X C00P C00G 118.7(2) . . ? C00Z C00P C00G 116.3(2) . . ? C00Z C00P C00X 125.0(2) . . ? C010 C00Q O002 102.59(18) . . ? C011 C00Q O002 109.4(2) . . ? C011 C00Q C010 111.7(3) . . ? C012 C00Q O002 108.5(2) . . ? C012 C00Q C010 110.5(3) . . ? C012 C00Q C011 113.5(3) . . ? C00L C00R H00R 119.9 . . ? C00L C00R C00U 120.2(2) . . ? C00U C00R H00R 119.9 . . ? C00N C00S H00S 119.2 . . ? C00X C00S C00N 121.6(2) . . ? C00X C00S H00S 119.2 . . ? N006 C00T H00T 118.1 . . ? N006 C00T C00Y 123.8(3) . . ? C00Y C00T H00T 118.1 . . ? C00R C00U H00U 118.9 . . ? C00W C00U C00R 122.3(2) . . ? C00W C00U H00U 118.9 . . ? S001 C00V H00V 123.7 . . ? C00M C00V S001 112.64(18) . . ? C00M C00V H00V 123.7 . . ? C00K C00W H00W 121.4 . . ? C00U C00W C00K 117.2(2) . . ? C00U C00W H00W 121.4 . . ? C00P C00X H00X 119.9 . . ? C00S C00X C00P 120.3(2) . . ? C00S C00X H00X 119.9 . . ? C00T C00Y H00Y 120.6 . . ? C00Z C00Y C00T 118.8(3) . . ? C00Z C00Y H00Y 120.6 . . ? C00P C00Z H00Z 119.6 . . ? C00Y C00Z C00P 120.8(2) . . ? C00Y C00Z H00Z 119.6 . . ? C00Q C010 H01A 109.5 . . ? C00Q C010 H01B 109.5 . . ? C00Q C010 H01C 109.5 . . ? H01A C010 H01B 109.5 . . ? H01A C010 H01C 109.5 . . ? H01B C010 H01C 109.5 . . ? C00Q C011 H01D 109.5 . . ? C00Q C011 H01E 109.5 . . ? C00Q C011 H01F 109.5 . . ? H01D C011 H01E 109.5 . . ? H01D C011 H01F 109.5 . . ? H01E C011 H01F 109.5 . . ? C00Q C012 H01G 109.5 . . ? C00Q C012 H01H 109.5 . . ? C00Q C012 H01I 109.5 . . ? H01G C012 H01H 109.5 . . ? H01G C012 H01I 109.5 . . ? H01H C012 H01I 109.5 . . ? 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 S001 C00H 1.725(2) . ? S001 C00V 1.692(3) . ? O002 C00O 1.317(3) . ? O002 C00Q 1.501(3) . ? N003 C009 1.413(2) . ? N003 C00K 1.431(3) . ? N003 C00O 1.396(3) . ? O004 C00E 1.221(3) . ? N005 H005 0.8600 . ? N005 C00E 1.347(3) . ? N005 C00F 1.402(3) . ? N006 C00G 1.359(3) . ? N006 C00T 1.324(3) . ? C007 C009 1.409(3) . ? C007 C00A 1.383(3) . ? C007 C00C 1.452(3) . ? O008 C00O 1.191(3) . ? C009 C00J 1.386(3) . ? C00A H00A 0.9300 . ? C00A C00B 1.386(3) . ? C00B C00D 1.489(3) . ? C00B C00I 1.397(3) . ? C00C C00K 1.393(3) . ? C00C C00L 1.393(3) . ? C00D C00H 1.372(3) . ? C00D C00M 1.416(3) . ? C00E C00H 1.484(3) . ? C00F C00G 1.417(3) . ? C00F C00N 1.374(3) . ? C00G C00P 1.420(3) . ? C00I H00I 0.9300 . ? C00I C00J 1.380(3) . ? C00J H00J 0.9300 . ? C00K C00W 1.383(3) . ? C00L H00L 0.9300 . ? C00L C00R 1.378(3) . ? C00M H00M 0.9300 . ? C00M C00V 1.354(3) . ? C00N H00N 0.9300 . ? C00N C00S 1.408(3) . ? C00P C00X 1.413(4) . ? C00P C00Z 1.400(4) . ? C00Q C010 1.493(4) . ? C00Q C011 1.490(4) . ? C00Q C012 1.490(4) . ? C00R H00R 0.9300 . ? C00R C00U 1.383(3) . ? C00S H00S 0.9300 . ? C00S C00X 1.355(4) . ? C00T H00T 0.9300 . ? C00T C00Y 1.391(4) . ? C00U H00U 0.9300 . ? C00U C00W 1.380(3) . ? C00V H00V 0.9300 . ? C00W H00W 0.9300 . ? C00X H00X 0.9300 . ? C00Y H00Y 0.9300 . ? C00Y C00Z 1.351(4) . ? C00Z H00Z 0.9300 . ? C010 H01A 0.9600 . ? C010 H01B 0.9600 . ? C010 H01C 0.9600 . ? C011 H01D 0.9600 . ? C011 H01E 0.9600 . ? C011 H01F 0.9600 . ? C012 H01G 0.9600 . ? C012 H01H 0.9600 . ? C012 H01I 0.9600 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N003 C009 C00J C00I -179.8(2) . . . . ? N003 C00K C00W C00U -179.8(2) . . . . ? O004 C00E C00H S001 16.8(3) . . . . ? O004 C00E C00H C00D -169.4(2) . . . . ? N005 C00E C00H S001 -161.42(17) . . . . ? N005 C00E C00H C00D 12.3(4) . . . . ? N005 C00F C00G N006 1.4(3) . . . . ? N005 C00F C00G C00P -177.38(19) . . . . ? N005 C00F C00N C00S 177.9(2) . . . . ? N006 C00G C00P C00X -179.7(2) . . . . ? N006 C00G C00P C00Z -0.3(3) . . . . ? N006 C00T C00Y C00Z -0.4(4) . . . . ? C007 C009 C00J C00I 0.9(3) . . . . ? C007 C00A C00B C00D 179.66(18) . . . . ? C007 C00A C00B C00I 1.7(3) . . . . ? C007 C00C C00K N003 -1.1(2) . . . . ? C007 C00C C00K C00W 177.8(2) . . . . ? C007 C00C C00L C00R -179.0(2) . . . . ? C009 N003 C00K C00C -0.4(2) . . . . ? C009 N003 C00K C00W -179.2(2) . . . . ? C009 N003 C00O O002 2.8(3) . . . . ? C009 N003 C00O O008 -177.2(3) . . . . ? C009 C007 C00A C00B 0.7(3) . . . . ? C009 C007 C00C C00K 2.2(2) . . . . ? C009 C007 C00C C00L -178.3(2) . . . . ? C00A C007 C009 N003 178.51(18) . . . . ? C00A C007 C009 C00J -2.0(3) . . . . ? C00A C007 C00C C00K -179.0(2) . . . . ? C00A C007 C00C C00L 0.5(4) . . . . ? C00A C00B C00D C00H 65.4(3) . . . . ? C00A C00B C00D C00M -111.2(2) . . . . ? C00A C00B C00I C00J -2.9(3) . . . . ? C00B C00D C00H S001 -175.98(16) . . . . ? C00B C00D C00H C00E 10.1(4) . . . . ? C00B C00D C00M C00V 176.4(2) . . . . ? C00B C00I C00J C009 1.6(3) . . . . ? C00C C007 C009 N003 -2.5(2) . . . . ? C00C C007 C009 C00J 176.92(19) . . . . ? C00C C007 C00A C00B -177.9(2) . . . . ? C00C C00K C00W C00U 1.6(4) . . . . ? C00C C00L C00R C00U 1.0(4) . . . . ? C00D C00B C00I C00J 179.1(2) . . . . ? C00D C00M C00V S001 0.0(3) . . . . ? C00E N005 C00F C00G -177.9(2) . . . . ? C00E N005 C00F C00N 2.4(4) . . . . ? C00F N005 C00E O004 2.0(4) . . . . ? C00F N005 C00E C00H -179.8(2) . . . . ? C00F C00G C00P C00X -0.9(3) . . . . ? C00F C00G C00P C00Z 178.5(2) . . . . ? C00F C00N C00S C00X -0.1(4) . . . . ? C00G N006 C00T C00Y 0.4(4) . . . . ? C00G C00F C00N C00S -1.8(3) . . . . ? C00G C00P C00X C00S -1.0(4) . . . . ? C00G C00P C00Z C00Y 0.3(4) . . . . ? C00H S001 C00V C00M 0.4(2) . . . . ? C00H C00D C00M C00V -0.6(3) . . . . ? C00I C00B C00D C00H -116.6(2) . . . . ? C00I C00B C00D C00M 66.8(3) . . . . ? C00K N003 C009 C007 1.9(2) . . . . ? C00K N003 C009 C00J -177.5(2) . . . . ? C00K N003 C00O O002 -170.6(2) . . . . ? C00K N003 C00O O008 9.4(4) . . . . ? C00K C00C C00L C00R 0.4(3) . . . . ? C00L C00C C00K N003 179.4(2) . . . . ? C00L C00C C00K C00W -1.8(3) . . . . ? C00L C00R C00U C00W -1.2(4) . . . . ? C00M C00D C00H S001 0.9(2) . . . . ? C00M C00D C00H C00E -173.0(2) . . . . ? C00N C00F C00G N006 -178.9(2) . . . . ? C00N C00F C00G C00P 2.3(3) . . . . ? C00N C00S C00X C00P 1.5(4) . . . . ? C00O O002 C00Q C010 179.3(2) . . . . ? C00O O002 C00Q C011 60.6(3) . . . . ? C00O O002 C00Q C012 -63.7(3) . . . . ? C00O N003 C009 C007 -172.3(2) . . . . ? C00O N003 C009 C00J 8.3(4) . . . . ? C00O N003 C00K C00C 174.2(2) . . . . ? C00O N003 C00K C00W -4.6(4) . . . . ? C00Q O002 C00O N003 176.85(19) . . . . ? C00Q O002 C00O O008 -3.1(4) . . . . ? C00R C00U C00W C00K -0.1(4) . . . . ? C00T N006 C00G C00F -178.8(2) . . . . ? C00T N006 C00G C00P -0.1(3) . . . . ? C00T C00Y C00Z C00P 0.1(4) . . . . ? C00V S001 C00H C00D -0.78(18) . . . . ? C00V S001 C00H C00E 174.31(18) . . . . ? C00X C00P C00Z C00Y 179.7(3) . . . . ? C00Z C00P C00X C00S 179.7(2) . . . . ?