#------------------------------------------------------------------------------ #$Date: 2020-02-04 22:02:08 +0200 (Tue, 04 Feb 2020) $ #$Revision: 247579 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125665.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_7125665 loop_ _publ_author_name 'Kahar, Nilesh' 'Jadhav, Pankaj' 'Reddy, R. V. Ramana' 'Dawande, Sudam' _publ_section_title ; A rhodium(ii) catalysed domino synthesis of azepino fused diindoles from isatin tethered N-sulfonyl-1,2,3-triazoles and indoles. ; _journal_issue 8 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 1207 _journal_page_last 1210 _journal_paper_doi 10.1039/c9cc08377d _journal_volume 56 _journal_year 2020 _chemical_formula_moiety 'C33 H25 N3 O4 S1' _chemical_formula_sum 'C33 H25 N3 O4 S' _chemical_formula_weight 559.62 _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4.3 _audit_creation_date 2019-04-20T10:36:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_update_record ; 2019-04-21 deposited with the CCDC. 2019-12-17 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 96.380(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.2400(18) _cell_length_b 12.733(3) _cell_length_c 22.312(5) _cell_measurement_reflns_used 24 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 25.956 _cell_measurement_theta_min 2.304 _cell_measurement_wavelength 0.71073 _cell_volume 2608.8(10) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX3' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Ortep for Windows (Farrugia, 2012)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 120(2) _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1771 _diffrn_reflns_av_unetI/netI 0.0936 _diffrn_reflns_Laue_measured_fraction_full 1 _diffrn_reflns_Laue_measured_fraction_max 0.978 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 51039 _diffrn_reflns_point_group_measured_fraction_full 1 _diffrn_reflns_point_group_measured_fraction_max 0.978 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.956 _diffrn_reflns_theta_min 2.304 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.171 _exptl_absorpt_correction_type none _exptl_crystal_colour Brown _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Needle _exptl_crystal_F_000 1168 _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _refine_diff_density_max 0.264 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.069 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 375 _refine_ls_number_reflns 5003 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.075 _refine_ls_R_factor_all 0.1226 _refine_ls_R_factor_gt 0.0605 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+1.7763P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0933 _refine_ls_wR_factor_ref 0.1091 _reflns_Friedel_coverage 0 _reflns_number_gt 3188 _reflns_number_total 5003 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc08377d2.cif _cod_data_source_block AV-NMK-330 _cod_depositor_comments 'Adding full bibliography for 7125665--7125666.cif.' _cod_original_cell_volume 2608.9(9) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7125665 _shelx_res_file ; TITL TRYf2_a.res in P2(1)/n shelx.res created by SHELXL-2018/1 at 10:35:42 on 20-Apr-2019 CELL 0.71073 9.24 12.7335 22.3117 90 96.38 90 ZERR 4 0.0018 0.0027 0.0049 0 0.007 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O S UNIT 132 100 12 16 4 L.S. 20 PLAN 5 TEMP -153.15 BOND $H fmap 2 acta MERG 2 REM REM REM WGHT 0.031100 1.776300 FVAR 0.32104 S001 5 0.519074 0.825147 0.618874 11.00000 0.01548 0.00960 = 0.02298 -0.00149 0.00144 -0.00128 O002 4 0.528659 0.539778 0.578199 11.00000 0.01529 0.01358 = 0.02365 0.00300 0.00317 0.00345 O003 4 0.414485 0.905442 0.600415 11.00000 0.02324 0.00956 = 0.03201 0.00015 0.00110 0.00512 O004 4 0.664243 0.853523 0.642522 11.00000 0.01859 0.01582 = 0.03164 -0.00256 -0.00207 -0.00584 O005 4 -0.157243 0.680991 0.566680 11.00000 0.01539 0.02049 = 0.03985 -0.00031 0.00663 0.00179 N006 3 0.294012 0.831776 0.474195 11.00000 0.01824 0.01019 = 0.01738 0.00281 0.00052 0.00037 N007 3 0.165437 0.543865 0.555525 11.00000 0.01070 0.01109 = 0.02441 0.00052 0.00696 -0.00066 N008 3 0.535882 0.751173 0.558777 11.00000 0.01097 0.01295 = 0.01991 -0.00130 0.00308 0.00096 C009 1 0.419300 0.580661 0.550451 11.00000 0.01350 0.01392 = 0.01349 -0.00154 0.00789 0.00244 C00A 1 0.408360 0.690911 0.538220 11.00000 0.00984 0.01182 = 0.01565 -0.00103 0.00362 -0.00112 C00B 1 0.287884 0.738941 0.505598 11.00000 0.01958 0.00736 = 0.01483 -0.00196 0.00443 -0.00027 C00C 1 0.097604 0.478063 0.594682 11.00000 0.01153 0.01576 = 0.01593 -0.00319 0.00232 -0.00358 C00D 1 -0.037720 0.521496 0.603856 11.00000 0.01409 0.01297 = 0.01899 -0.00298 0.00044 -0.00150 C00E 1 0.051270 0.801825 0.479036 11.00000 0.01679 0.01186 = 0.01656 -0.00222 0.00026 0.00300 C00F 1 0.291346 0.514312 0.525110 11.00000 0.01359 0.00930 = 0.02069 -0.00034 0.00513 -0.00071 AFIX 23 H00A 2 0.270445 0.526295 0.481159 11.00000 -1.20000 H00B 2 0.313789 0.438941 0.531907 11.00000 -1.20000 AFIX 0 C00G 1 -0.054419 0.619540 0.569609 11.00000 0.01015 0.01477 = 0.02506 -0.00602 0.00169 -0.00155 C00H 1 0.082467 0.631078 0.539956 11.00000 0.00960 0.01312 = 0.01766 -0.00468 -0.00191 0.00073 C00I 1 0.441855 0.742150 0.669852 11.00000 0.01602 0.01245 = 0.01602 -0.00493 0.00271 0.00001 C00J 1 0.531142 0.675960 0.707139 11.00000 0.01950 0.01823 = 0.02248 -0.00542 -0.00054 0.00048 AFIX 43 H00J 2 0.634076 0.681428 0.708968 11.00000 -1.20000 AFIX 0 C00K 1 0.153471 0.869781 0.457516 11.00000 0.02007 0.01348 = 0.01487 -0.00297 -0.00177 0.00421 C00L 1 0.426690 0.819745 0.384846 11.00000 0.01340 0.01669 = 0.02049 0.00178 0.00156 -0.00406 C00M 1 0.397936 0.877654 0.331847 11.00000 0.02017 0.01302 = 0.02529 0.00428 0.00362 -0.00060 AFIX 43 H00M 2 0.375674 0.950315 0.333883 11.00000 -1.20000 AFIX 0 C00N 1 0.132545 0.715015 0.508634 11.00000 0.01143 0.01081 = 0.01544 -0.00355 -0.00082 0.00031 C00O 1 -0.129979 0.468889 0.638773 11.00000 0.01394 0.02401 = 0.02101 -0.00095 0.00163 -0.00224 AFIX 43 H00O 2 -0.222785 0.496919 0.644406 11.00000 -1.20000 AFIX 0 C00P 1 0.145133 0.384541 0.620988 11.00000 0.01514 0.01658 = 0.02432 -0.00247 0.00070 0.00049 AFIX 43 H00P 2 0.237484 0.355990 0.615099 11.00000 -1.20000 AFIX 0 C00Q 1 0.420589 0.869849 0.446147 11.00000 0.02044 0.01341 = 0.02167 0.00437 0.00292 -0.00469 AFIX 23 H00C 2 0.510877 0.853058 0.472576 11.00000 -1.20000 H00D 2 0.414547 0.947113 0.441602 11.00000 -1.20000 AFIX 0 C00R 1 0.458967 0.713544 0.380197 11.00000 0.01662 0.01925 = 0.02581 0.00681 0.00491 0.00270 AFIX 43 H00R 2 0.479400 0.672973 0.415866 11.00000 -1.20000 AFIX 0 C00S 1 -0.032821 0.983609 0.415720 11.00000 0.03562 0.01852 = 0.02500 0.00331 -0.00150 0.00976 AFIX 43 H00S 2 -0.063400 1.045968 0.394617 11.00000 -1.20000 AFIX 0 C00T 1 -0.096562 0.826816 0.467549 11.00000 0.01815 0.02118 = 0.02415 -0.00295 0.00074 0.00339 AFIX 43 H00T 2 -0.168191 0.781888 0.481176 11.00000 -1.20000 AFIX 0 C00U 1 0.052622 0.333798 0.656417 11.00000 0.02166 0.02079 = 0.02493 0.00715 0.00234 -0.00356 AFIX 43 H00U 2 0.082779 0.269337 0.675282 11.00000 -1.20000 AFIX 0 C00V 1 0.291695 0.735078 0.667469 11.00000 0.01766 0.02103 = 0.01894 -0.00296 0.00241 0.00430 AFIX 43 H00V 2 0.230942 0.781585 0.642690 11.00000 -1.20000 AFIX 0 C00W 1 0.113943 0.960650 0.425378 11.00000 0.02461 0.01810 = 0.02313 0.00008 0.00178 0.00118 AFIX 43 H00W 2 0.184740 1.005043 0.410691 11.00000 -1.20000 AFIX 0 C00X 1 0.468106 0.601812 0.741650 11.00000 0.03987 0.01690 = 0.01583 0.00074 -0.00059 0.00431 AFIX 43 H00X 2 0.528709 0.557818 0.768112 11.00000 -1.20000 AFIX 0 C00Y 1 -0.083444 0.374764 0.665120 11.00000 0.01862 0.03008 = 0.02344 0.00424 0.00471 -0.00837 AFIX 43 H00Y 2 -0.144632 0.337694 0.689344 11.00000 -1.20000 AFIX 0 C00Z 1 0.231652 0.659829 0.701452 11.00000 0.02048 0.03430 = 0.02054 -0.00661 0.00639 -0.00831 AFIX 43 H00Z 2 0.128676 0.655009 0.699743 11.00000 -1.20000 AFIX 0 C010 1 0.401590 0.830055 0.276307 11.00000 0.02073 0.02751 = 0.02138 0.00546 0.00390 -0.00227 AFIX 43 H010 2 0.382496 0.870494 0.240521 11.00000 -1.20000 AFIX 0 C011 1 0.317411 0.590760 0.738165 11.00000 0.03524 0.02412 = 0.01701 -0.00891 0.00849 -0.00620 C012 1 0.432709 0.724348 0.272327 11.00000 0.02058 0.03293 = 0.02516 -0.00579 0.00928 -0.00236 AFIX 43 H012 2 0.434114 0.691956 0.234040 11.00000 -1.20000 AFIX 0 C013 1 -0.137341 0.917584 0.436156 11.00000 0.02477 0.02800 = 0.02425 -0.00131 -0.00513 0.01464 AFIX 43 H013 2 -0.237587 0.935190 0.428417 11.00000 -1.20000 AFIX 0 C014 1 0.461872 0.665965 0.324719 11.00000 0.02053 0.01739 = 0.03769 -0.00095 0.01231 -0.00114 AFIX 43 H014 2 0.483837 0.593285 0.322463 11.00000 -1.20000 AFIX 0 C015 1 0.248919 0.506710 0.773472 11.00000 0.05194 0.03530 = 0.02586 0.00340 0.00922 -0.01632 AFIX 137 H01A 2 0.316789 0.447792 0.780880 11.00000 -1.50000 H01B 2 0.158906 0.482066 0.750383 11.00000 -1.50000 H01C 2 0.226584 0.535689 0.812083 11.00000 -1.50000 AFIX 0 H008 2 0.613177 0.711988 0.565305 11.00000 0.02563 HKLF 4 REM TRYf2_a.res in P2(1)/n REM R1 = 0.0605 for 3188 Fo > 4sig(Fo) and 0.1226 for all 5003 data REM 375 parameters refined using 0 restraints END WGHT 0.0305 1.8058 REM Highest difference peak 0.264, deepest hole -0.427, 1-sigma level 0.069 Q1 1 0.3581 0.4610 0.7926 11.00000 0.05 0.26 Q2 1 0.4582 0.6256 0.4989 11.00000 0.05 0.25 Q3 1 0.4135 0.6800 0.4726 11.00000 0.05 0.25 Q4 1 0.1610 0.5626 0.6565 11.00000 0.05 0.24 Q5 1 0.5752 0.5562 0.6609 11.00000 0.05 0.24 ; _shelx_res_checksum 55753 loop_ _symmetry_equiv_pos_as_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' 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 S001 S 0.51907(8) 0.82515(6) 0.61887(3) 0.01607(18) Uani 1 1 d . . O002 O 0.5287(2) 0.53978(14) 0.57820(8) 0.0174(5) Uani 1 1 d . . O003 O 0.4145(2) 0.90544(14) 0.60041(9) 0.0218(5) Uani 1 1 d . . O004 O 0.6642(2) 0.85352(15) 0.64252(9) 0.0224(5) Uani 1 1 d . . O005 O -0.1572(2) 0.68099(16) 0.56668(9) 0.0250(5) Uani 1 1 d . . N006 N 0.2940(2) 0.83178(17) 0.47419(10) 0.0154(5) Uani 1 1 d . . N007 N 0.1654(2) 0.54387(17) 0.55552(10) 0.0150(5) Uani 1 1 d . . N008 N 0.5359(3) 0.75117(19) 0.55878(10) 0.0145(5) Uani 1 1 d . . C009 C 0.4193(3) 0.5807(2) 0.55045(12) 0.0132(6) Uani 1 1 d . . C00A C 0.4084(3) 0.6909(2) 0.53822(12) 0.0123(6) Uani 1 1 d . . C00B C 0.2879(3) 0.7389(2) 0.50560(12) 0.0137(6) Uani 1 1 d . . C00C C 0.0976(3) 0.4781(2) 0.59468(12) 0.0143(6) Uani 1 1 d . . C00D C -0.0377(3) 0.5215(2) 0.60386(12) 0.0155(7) Uani 1 1 d . . C00E C 0.0513(3) 0.8018(2) 0.47904(12) 0.0152(7) Uani 1 1 d . . C00F C 0.2913(3) 0.5143(2) 0.52511(12) 0.0143(6) Uani 1 1 d . . H00A H 0.270445 0.526295 0.481159 0.017 Uiso 1 1 calc R U H00B H 0.313789 0.438941 0.531907 0.017 Uiso 1 1 calc R U C00G C -0.0544(3) 0.6195(2) 0.56961(13) 0.0167(7) Uani 1 1 d . . C00H C 0.0825(3) 0.6311(2) 0.53996(12) 0.0137(6) Uani 1 1 d . . C00I C 0.4419(3) 0.7421(2) 0.66985(12) 0.0148(7) Uani 1 1 d . . C00J C 0.5311(3) 0.6760(2) 0.70714(12) 0.0203(7) Uani 1 1 d . . H00J H 0.634076 0.681428 0.708968 0.024 Uiso 1 1 calc R U C00K C 0.1535(3) 0.8698(2) 0.45752(12) 0.0164(7) Uani 1 1 d . . C00L C 0.4267(3) 0.8197(2) 0.38485(12) 0.0169(7) Uani 1 1 d . . C00M C 0.3979(3) 0.8777(2) 0.33185(13) 0.0194(7) Uani 1 1 d . . H00M H 0.375674 0.950315 0.333883 0.023 Uiso 1 1 calc R U C00N C 0.1325(3) 0.7150(2) 0.50863(12) 0.0127(6) Uani 1 1 d . . C00O C -0.1300(3) 0.4689(2) 0.63877(12) 0.0197(7) Uani 1 1 d . . H00O H -0.222785 0.496919 0.644406 0.024 Uiso 1 1 calc R U C00P C 0.1451(3) 0.3845(2) 0.62099(13) 0.0188(7) Uani 1 1 d . . H00P H 0.237484 0.35599 0.615099 0.023 Uiso 1 1 calc R U C00Q C 0.4206(3) 0.8698(2) 0.44615(12) 0.0185(7) Uani 1 1 d . . H00C H 0.510877 0.853058 0.472576 0.022 Uiso 1 1 calc R U H00D H 0.414547 0.947113 0.441602 0.022 Uiso 1 1 calc R U C00R C 0.4590(3) 0.7135(2) 0.38020(14) 0.0204(7) Uani 1 1 d . . H00R H 0.4794 0.672973 0.415866 0.024 Uiso 1 1 calc R U C00S C -0.0328(3) 0.9836(2) 0.41572(13) 0.0267(8) Uani 1 1 d . . H00S H -0.0634 1.045968 0.394617 0.032 Uiso 1 1 calc R U C00T C -0.0966(3) 0.8268(2) 0.46755(13) 0.0213(7) Uani 1 1 d . . H00T H -0.168191 0.781888 0.481176 0.026 Uiso 1 1 calc R U C00U C 0.0526(3) 0.3338(2) 0.65642(13) 0.0225(7) Uani 1 1 d . . H00U H 0.082779 0.269337 0.675282 0.027 Uiso 1 1 calc R U C00V C 0.2917(3) 0.7351(2) 0.66747(13) 0.0192(7) Uani 1 1 d . . H00V H 0.230942 0.781585 0.64269 0.023 Uiso 1 1 calc R U C00W C 0.1139(3) 0.9606(2) 0.42538(13) 0.0220(7) Uani 1 1 d . . H00W H 0.18474 1.005043 0.410691 0.026 Uiso 1 1 calc R U C00X C 0.4681(3) 0.6018(2) 0.74165(13) 0.0245(8) Uani 1 1 d . . H00X H 0.528709 0.557818 0.768112 0.029 Uiso 1 1 calc R U C00Y C -0.0834(3) 0.3748(2) 0.66512(13) 0.0239(8) Uani 1 1 d . . H00Y H -0.144632 0.337694 0.689344 0.029 Uiso 1 1 calc R U C00Z C 0.2317(3) 0.6598(2) 0.70145(13) 0.0248(8) Uani 1 1 d . . H00Z H 0.128676 0.655009 0.699743 0.03 Uiso 1 1 calc R U C010 C 0.4016(3) 0.8301(2) 0.27631(13) 0.0231(7) Uani 1 1 d . . H010 H 0.382496 0.870494 0.240521 0.028 Uiso 1 1 calc R U C011 C 0.3174(3) 0.5908(2) 0.73817(13) 0.0250(8) Uani 1 1 d . . C012 C 0.4327(3) 0.7243(3) 0.27233(14) 0.0257(8) Uani 1 1 d . . H012 H 0.434114 0.691956 0.23404 0.031 Uiso 1 1 calc R U C013 C -0.1373(3) 0.9176(2) 0.43616(13) 0.0263(8) Uani 1 1 d . . H013 H -0.237587 0.93519 0.428417 0.032 Uiso 1 1 calc R U C014 C 0.4619(3) 0.6660(2) 0.32472(14) 0.0245(7) Uani 1 1 d . . H014 H 0.483837 0.593285 0.322463 0.029 Uiso 1 1 calc R U C015 C 0.2489(4) 0.5067(3) 0.77347(14) 0.0373(9) Uani 1 1 d . . H01A H 0.316789 0.447792 0.78088 0.056 Uiso 1 1 calc R U H01B H 0.158906 0.482066 0.750383 0.056 Uiso 1 1 calc R U H01C H 0.226584 0.535689 0.812083 0.056 Uiso 1 1 calc R U H008 H 0.613(3) 0.712(2) 0.5653(13) 0.026(9) Uiso 1 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S001 0.0155(4) 0.0096(4) 0.0230(4) -0.0015(3) 0.0014(3) -0.0013(3) O002 0.0153(11) 0.0136(11) 0.0236(11) 0.0030(9) 0.0032(9) 0.0034(9) O003 0.0232(12) 0.0096(11) 0.0320(13) 0.0002(9) 0.0011(9) 0.0051(9) O004 0.0186(11) 0.0158(12) 0.0316(12) -0.0026(9) -0.0021(9) -0.0058(9) O005 0.0154(11) 0.0205(12) 0.0398(13) -0.0003(10) 0.0066(10) 0.0018(10) N006 0.0182(13) 0.0102(13) 0.0174(13) 0.0028(11) 0.0005(10) 0.0004(11) N007 0.0107(13) 0.0111(13) 0.0244(14) 0.0005(11) 0.0070(10) -0.0007(10) N008 0.0110(13) 0.0130(14) 0.0199(14) -0.0013(11) 0.0031(11) 0.0010(11) C009 0.0135(16) 0.0139(16) 0.0135(15) -0.0015(12) 0.0079(13) 0.0024(13) C00A 0.0098(14) 0.0118(16) 0.0156(15) -0.0010(12) 0.0036(12) -0.0011(12) C00B 0.0196(17) 0.0074(15) 0.0148(15) -0.0020(12) 0.0044(13) -0.0003(12) C00C 0.0115(15) 0.0158(16) 0.0159(15) -0.0032(13) 0.0023(12) -0.0036(13) C00D 0.0141(15) 0.0130(16) 0.0190(16) -0.0030(13) 0.0004(12) -0.0015(13) C00E 0.0168(16) 0.0119(17) 0.0166(15) -0.0022(12) 0.0003(12) 0.0030(13) C00F 0.0136(15) 0.0093(15) 0.0207(16) -0.0003(13) 0.0051(12) -0.0007(12) C00G 0.0101(15) 0.0148(17) 0.0251(17) -0.0060(14) 0.0017(13) -0.0015(13) C00H 0.0096(15) 0.0131(16) 0.0177(16) -0.0047(12) -0.0019(12) 0.0007(13) C00I 0.0160(16) 0.0125(16) 0.0160(15) -0.0049(13) 0.0027(13) 0.0000(13) C00J 0.0195(16) 0.0182(17) 0.0225(17) -0.0054(14) -0.0005(13) 0.0005(14) C00K 0.0201(16) 0.0135(16) 0.0149(15) -0.0030(12) -0.0018(13) 0.0042(13) C00L 0.0134(15) 0.0167(17) 0.0205(16) 0.0018(14) 0.0016(12) -0.0041(13) C00M 0.0202(17) 0.0130(17) 0.0253(18) 0.0043(14) 0.0036(13) -0.0006(13) C00N 0.0114(15) 0.0108(15) 0.0154(15) -0.0035(12) -0.0008(12) 0.0003(12) C00O 0.0139(16) 0.0240(19) 0.0210(17) -0.0010(14) 0.0016(13) -0.0022(14) C00P 0.0151(16) 0.0166(18) 0.0243(17) -0.0025(14) 0.0007(13) 0.0005(13) C00Q 0.0204(16) 0.0134(16) 0.0217(17) 0.0044(13) 0.0029(13) -0.0047(13) C00R 0.0166(17) 0.0192(17) 0.0258(18) 0.0068(14) 0.0049(14) 0.0027(13) C00S 0.036(2) 0.0185(18) 0.0250(18) 0.0033(15) -0.0015(15) 0.0098(15) C00T 0.0181(16) 0.0212(18) 0.0241(17) -0.0029(14) 0.0007(13) 0.0034(14) C00U 0.0217(17) 0.0208(18) 0.0249(17) 0.0071(15) 0.0023(14) -0.0036(15) C00V 0.0177(17) 0.0210(18) 0.0189(16) -0.0030(14) 0.0024(13) 0.0043(14) C00W 0.0246(18) 0.0181(18) 0.0231(17) 0.0001(14) 0.0018(14) 0.0012(14) C00X 0.040(2) 0.0169(18) 0.0158(17) 0.0007(14) -0.0006(15) 0.0043(15) C00Y 0.0186(17) 0.030(2) 0.0234(18) 0.0042(15) 0.0047(14) -0.0084(15) C00Z 0.0205(17) 0.034(2) 0.0205(17) -0.0066(16) 0.0064(14) -0.0083(16) C010 0.0207(17) 0.0275(19) 0.0214(17) 0.0055(15) 0.0039(13) -0.0023(15) C011 0.035(2) 0.0241(19) 0.0170(17) -0.0089(14) 0.0085(15) -0.0062(16) C012 0.0206(18) 0.033(2) 0.0252(19) -0.0058(16) 0.0093(14) -0.0024(15) C013 0.0248(18) 0.028(2) 0.0242(18) -0.0013(15) -0.0051(15) 0.0146(16) C014 0.0205(17) 0.0174(18) 0.038(2) -0.0010(16) 0.0123(15) -0.0011(14) C015 0.052(2) 0.035(2) 0.0259(19) 0.0034(16) 0.0092(17) -0.0163(18) 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 0 '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 0.006 '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 O004 S001 O003 119.94(12) O004 S001 N008 105.84(12) O003 S001 N008 107.03(12) O004 S001 C00I 110.10(13) O003 S001 C00I 107.74(13) N008 S001 C00I 105.20(12) C00B N006 C00K 110.1(2) C00B N006 C00Q 125.4(2) C00K N006 C00Q 122.2(2) C00H N007 C00C 111.4(2) C00H N007 C00F 122.9(2) C00C N007 C00F 124.6(2) C00A N008 S001 114.43(18) C00A N008 H008 112(2) S001 N008 H008 109.8(19) O002 C009 C00A 122.9(3) O002 C009 C00F 120.8(2) C00A C009 C00F 116.2(2) C00B C00A C009 124.2(2) C00B C00A N008 120.6(2) C009 C00A N008 115.1(2) N006 C00B C00A 124.3(2) N006 C00B C00N 107.2(2) C00A C00B C00N 127.3(2) C00P C00C C00D 121.7(3) C00P C00C N007 129.5(2) C00D C00C N007 108.8(2) C00O C00D C00C 120.3(3) C00O C00D C00G 132.0(3) C00C C00D C00G 107.7(2) C00T C00E C00K 118.5(3) C00T C00E C00N 134.5(3) C00K C00E C00N 106.9(2) N007 C00F C009 108.2(2) N007 C00F H00A 110.1 C009 C00F H00A 110.1 N007 C00F H00B 110.1 C009 C00F H00B 110.1 H00A C00F H00B 108.4 O005 C00G C00D 127.5(3) O005 C00G C00H 126.9(3) C00D C00G C00H 105.6(2) N007 C00H C00N 123.0(2) N007 C00H C00G 106.5(2) C00N C00H C00G 130.1(3) C00V C00I C00J 120.6(3) C00V C00I S001 119.4(2) C00J C00I S001 119.6(2) C00X C00J C00I 119.2(3) C00X C00J H00J 120.4 C00I C00J H00J 120.4 C00W C00K N006 127.6(3) C00W C00K C00E 122.8(3) N006 C00K C00E 109.6(2) C00R C00L C00M 118.2(3) C00R C00L C00Q 120.4(3) C00M C00L C00Q 121.3(3) C010 C00M C00L 120.5(3) C010 C00M H00M 119.8 C00L C00M H00M 119.8 C00H C00N C00E 129.2(2) C00H C00N C00B 124.3(2) C00E C00N C00B 106.2(2) C00Y C00O C00D 118.4(3) C00Y C00O H00O 120.8 C00D C00O H00O 120.8 C00C C00P C00U 117.3(3) C00C C00P H00P 121.4 C00U C00P H00P 121.4 N006 C00Q C00L 110.9(2) N006 C00Q H00C 109.5 C00L C00Q H00C 109.5 N006 C00Q H00D 109.5 C00L C00Q H00D 109.5 H00C C00Q H00D 108 C014 C00R C00L 121.3(3) C014 C00R H00R 119.4 C00L C00R H00R 119.4 C00W C00S C013 121.7(3) C00W C00S H00S 119.2 C013 C00S H00S 119.2 C013 C00T C00E 119.3(3) C013 C00T H00T 120.4 C00E C00T H00T 120.4 C00P C00U C00Y 121.8(3) C00P C00U H00U 119.1 C00Y C00U H00U 119.1 C00Z C00V C00I 119.2(3) C00Z C00V H00V 120.4 C00I C00V H00V 120.4 C00S C00W C00K 117.0(3) C00S C00W H00W 121.5 C00K C00W H00W 121.5 C00J C00X C011 121.1(3) C00J C00X H00X 119.4 C011 C00X H00X 119.4 C00O C00Y C00U 120.5(3) C00O C00Y H00Y 119.7 C00U C00Y H00Y 119.7 C00V C00Z C011 121.8(3) C00V C00Z H00Z 119.1 C011 C00Z H00Z 119.1 C012 C010 C00M 120.7(3) C012 C010 H010 119.6 C00M C010 H010 119.6 C00Z C011 C00X 118.1(3) C00Z C011 C015 120.8(3) C00X C011 C015 121.1(3) C010 C012 C014 119.4(3) C010 C012 H012 120.3 C014 C012 H012 120.3 C00T C013 C00S 120.7(3) C00T C013 H013 119.7 C00S C013 H013 119.7 C00R C014 C012 119.9(3) C00R C014 H014 120 C012 C014 H014 120 C011 C015 H01A 109.5 C011 C015 H01B 109.5 H01A C015 H01B 109.5 C011 C015 H01C 109.5 H01A C015 H01C 109.5 H01B C015 H01C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S001 O004 1.432(2) S001 O003 1.4354(19) S001 N008 1.660(2) S001 C00I 1.761(3) O002 C009 1.239(3) O005 C00G 1.227(3) N006 C00B 1.379(3) N006 C00K 1.397(3) N006 C00Q 1.469(3) N007 C00H 1.372(3) N007 C00C 1.407(3) N007 C00F 1.460(3) N008 C00A 1.438(3) N008 H008 0.87(3) C009 C00A 1.432(4) C009 C00F 1.511(4) C00A C00B 1.401(4) C00B C00N 1.476(4) C00C C00P 1.378(4) C00C C00D 1.403(4) C00D C00O 1.389(4) C00D C00G 1.463(4) C00E C00T 1.398(4) C00E C00K 1.404(4) C00E C00N 1.453(4) C00F H00A 0.99 C00F H00B 0.99 C00G C00H 1.498(4) C00H C00N 1.384(4) C00I C00V 1.386(4) C00I C00J 1.389(4) C00J C00X 1.387(4) C00J H00J 0.95 C00K C00W 1.389(4) C00L C00R 1.391(4) C00L C00M 1.394(4) C00L C00Q 1.516(4) C00M C010 1.383(4) C00M H00M 0.95 C00O C00Y 1.382(4) C00O H00O 0.95 C00P C00U 1.387(4) C00P H00P 0.95 C00Q H00C 0.99 C00Q H00D 0.99 C00R C014 1.381(4) C00R H00R 0.95 C00S C00W 1.381(4) C00S C013 1.395(4) C00S H00S 0.95 C00T C013 1.382(4) C00T H00T 0.95 C00U C00Y 1.395(4) C00U H00U 0.95 C00V C00Z 1.376(4) C00V H00V 0.95 C00W H00W 0.95 C00X C011 1.393(4) C00X H00X 0.95 C00Y H00Y 0.95 C00Z C011 1.389(4) C00Z H00Z 0.95 C010 C012 1.381(4) C010 H010 0.95 C011 C015 1.509(4) C012 C014 1.386(4) C012 H012 0.95 C013 H013 0.95 C014 H014 0.95 C015 H01A 0.98 C015 H01B 0.98 C015 H01C 0.98