#------------------------------------------------------------------------------ #$Date: 2021-09-27 12:01:51 +0300 (Mon, 27 Sep 2021) $ #$Revision: 269321 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/47/1564728.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_1564728 loop_ _publ_author_name 'Kubasov, A.S.' 'Turishev, E.S.' 'Golubev, A.V.' 'Bykov, A.Yu.' 'Zhizhin, K.Yu.' 'Kuznetsov, N.T.' _publ_section_title ; The method for synthesis of 2-sulfonium closo-decaborate anions derivatives with exo-polyhedral aminogroups ; _journal_name_full 'Inorganica Chimica Acta' _journal_page_first 119589 _journal_paper_doi 10.1016/j.ica.2020.119589 _journal_volume 507 _journal_year 2020 _chemical_formula_moiety '2(C24 H20 P), C9 H15 B10 N O2 S' _chemical_formula_sum 'C57 H55 B10 N O2 P2 S' _chemical_formula_weight 988.12 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _cell_angle_alpha 90 _cell_angle_beta 95.879(13) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 20.087(6) _cell_length_b 14.334(4) _cell_length_c 18.695(5) _cell_measurement_reflns_used 2679 _cell_measurement_temperature 296 _cell_measurement_theta_max 25.546 _cell_measurement_theta_min 2.485 _cell_volume 5354(3) _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve (Bourhis et al., 2015)' _diffrn_ambient_temperature 296.15 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0906 _diffrn_reflns_av_unetI/netI 0.0409 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 93770 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.221 _diffrn_reflns_theta_min 2.007 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 0.164 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.6774 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0402 before and 0.0332 after correction. The Ratio of minimum to maximum transmission is 0.9087. The \l/2 correction factor is Not present.' _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.226 _exptl_crystal_description plate _exptl_crystal_F_000 2064 _exptl_crystal_size_max 0.9 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.318 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.043 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 718 _refine_ls_number_reflns 11891 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0525 _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^)+(0.0887P)^2^+0.9967P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1423 _refine_ls_wR_factor_ref 0.1579 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 8601 _reflns_number_total 11891 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file 19kub12_0m_a.cif _cod_data_source_block 19kub12_0m_a _cod_original_cell_volume 5355(3) _cod_database_code 1564728 _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. ; _shelx_estimated_absorpt_t_max 0.984 _shelx_estimated_absorpt_t_min 0.867 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C57(H57), C39(H39), C55(H55), C56(H56), C53(H53), C38(H38), C51(H51), C42(H42), C54(H54), C47(H47), C41(H41), C48(H48), C35(H35), C45(H45), C49(H49), C29(H29), C44(H44), C43(H43), C11(H11), C36(H36), C50(H50), C37(H37), C33(H33), C23(H23), C27(H27), C15(H15), C26(H26), C17(H17), C30(H30), C25(H25), C12(H12), C21(H21), C14(H14), C24(H24), C32(H32), C20(H20), C31(H31), C13(H13), C19(H19), C18(H18) ; _shelx_res_file ; TITL 19kub12_0m_a.res in P2(1)/c 19kub12_0m_a.res created by SHELXL-2017/1 at 15:24:09 on 19-Dec-2019 REM Old TITL Integration of 19kub12 REM SHELXT solution in P2(1)/c REM R1 0.219, Rweak 0.010, Alpha 0.067, Orientation a'=c, b'=-b, c'=a REM Formula found by SHELXT: C70 Cl3 CELL 0.71073 20.0873 14.3337 18.6954 90 95.879 90 ZERR 4 0.0059 0.0041 0.005 0 0.013 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H B N O P S UNIT 228 220 40 4 8 8 4 L.S. 4 PLAN 20 SIZE 0.1 0.4 0.9 TEMP 23 LIST 6 fmap 2 acta OMIT -2 55 OMIT 0 3 1 OMIT 0 1 1 REM REM REM WGHT 0.088700 0.996700 FVAR 0.72375 P2 6 0.019535 0.481660 0.329159 11.00000 0.04016 0.04153 = 0.03768 -0.00587 0.00454 0.00288 S1 7 0.211076 0.919982 0.486409 11.00000 0.06631 0.03803 = 0.05775 0.00160 -0.01013 0.00120 P1 6 0.496330 0.651791 0.702759 11.00000 0.04982 0.08086 = 0.05194 -0.00438 0.00478 0.01122 O2 5 0.312514 0.714696 0.529254 11.00000 0.07798 0.05576 = 0.07276 0.00394 0.02706 0.00746 C52 1 -0.036282 0.576806 0.338977 11.00000 0.04412 0.04235 = 0.03861 -0.00674 0.00431 0.00491 N1 4 0.259600 0.813743 0.601123 11.00000 0.05362 0.04427 = 0.05391 0.00813 0.00501 0.00849 O1 5 0.208012 0.874647 0.695673 11.00000 0.09994 0.09028 = 0.08021 -0.01755 0.01929 0.02578 C57 1 -0.076863 0.612037 0.281313 11.00000 0.04971 0.05601 = 0.03711 -0.00362 0.00395 0.00624 AFIX 43 H57 2 -0.074909 0.587180 0.235626 11.00000 -1.20000 AFIX 0 C34 1 0.024349 0.457474 0.235822 11.00000 0.04306 0.04643 = 0.04000 -0.00773 0.00775 0.00489 C39 1 0.078964 0.485969 0.201385 11.00000 0.04858 0.04816 = 0.04952 -0.00171 0.01185 0.00288 AFIX 43 H39 2 0.115180 0.515213 0.227130 11.00000 -1.20000 AFIX 0 C55 1 -0.123388 0.721357 0.358929 11.00000 0.06085 0.04866 = 0.06579 -0.00508 0.01286 0.01567 AFIX 43 H55 2 -0.152734 0.770030 0.365611 11.00000 -1.20000 AFIX 0 C46 1 0.099930 0.515715 0.371617 11.00000 0.04400 0.04326 = 0.04121 -0.00353 0.00204 0.00137 C56 1 -0.120530 0.684470 0.291504 11.00000 0.05291 0.05971 = 0.05458 0.00695 0.00258 0.01279 AFIX 43 H56 2 -0.147959 0.708171 0.252639 11.00000 -1.20000 AFIX 0 C53 1 -0.038956 0.615007 0.407063 11.00000 0.06675 0.06267 = 0.04110 -0.01281 -0.00517 0.01757 AFIX 43 H53 2 -0.011132 0.592360 0.446023 11.00000 -1.20000 AFIX 0 C9 1 0.280975 0.727338 0.580000 11.00000 0.04712 0.04158 = 0.05742 0.00753 0.00413 0.00624 C38 1 0.078863 0.470325 0.128256 11.00000 0.06900 0.05950 = 0.05346 0.00208 0.02574 0.01133 AFIX 43 H38 2 0.115451 0.488218 0.104767 11.00000 -1.20000 AFIX 0 C51 1 0.142873 0.452571 0.408092 11.00000 0.05568 0.04664 = 0.07792 0.00508 -0.00464 0.00118 AFIX 43 H51 2 0.129439 0.391147 0.413725 11.00000 -1.20000 AFIX 0 C42 1 -0.087891 0.300698 0.439398 11.00000 0.05171 0.08419 = 0.04439 0.00560 0.00617 -0.01217 AFIX 43 H42 2 -0.123977 0.302940 0.466796 11.00000 -1.20000 AFIX 0 C54 1 -0.083061 0.686585 0.416452 11.00000 0.07559 0.06296 = 0.05229 -0.02063 0.00759 0.01655 AFIX 43 H54 2 -0.085498 0.711459 0.462054 11.00000 -1.20000 AFIX 0 C40 1 -0.011052 0.378639 0.369616 11.00000 0.04373 0.04727 = 0.04065 -0.00418 0.00454 -0.00200 C2 1 0.258780 0.659569 0.632587 11.00000 0.04473 0.05118 = 0.06609 0.01703 0.00096 0.00348 C47 1 0.120559 0.607702 0.365695 11.00000 0.06196 0.04848 = 0.06884 0.00844 -0.00879 -0.00288 AFIX 43 H47 2 0.092085 0.651018 0.341455 11.00000 -1.20000 AFIX 0 C41 1 -0.065401 0.382234 0.410232 11.00000 0.04392 0.06240 = 0.04380 -0.00173 0.00403 0.00199 AFIX 43 H41 2 -0.086346 0.438763 0.417675 11.00000 -1.20000 AFIX 0 C22 1 0.464049 0.651323 0.788388 11.00000 0.06396 0.06601 = 0.06452 -0.00593 0.02007 -0.00441 C4 1 0.205965 0.664461 0.742290 11.00000 0.06411 0.11944 = 0.06977 0.03378 0.01096 -0.00300 C48 1 0.182820 0.634775 0.395514 11.00000 0.06805 0.05462 = 0.07291 0.00038 -0.00039 -0.01628 AFIX 43 H48 2 0.196114 0.696643 0.392210 11.00000 -1.20000 AFIX 0 C10 1 0.485631 0.766640 0.666134 11.00000 0.04357 0.08374 = 0.05814 0.00051 0.00162 -0.00213 C3 1 0.229568 0.708867 0.683981 11.00000 0.04500 0.07827 = 0.05704 0.01803 0.00169 0.00126 C35 1 -0.029176 0.413906 0.197184 11.00000 0.04928 0.08860 = 0.05470 -0.02608 0.01166 -0.00788 AFIX 43 H35 2 -0.065308 0.393452 0.220361 11.00000 -1.20000 AFIX 0 C45 1 0.019305 0.292813 0.359293 11.00000 0.05814 0.04961 = 0.07199 -0.00650 0.01916 -0.00103 AFIX 43 H45 2 0.055601 0.289676 0.332242 11.00000 -1.20000 AFIX 0 C28 1 0.453663 0.567390 0.643810 11.00000 0.06831 0.07744 = 0.06989 -0.01266 -0.00357 0.02503 B5 3 0.174891 1.147533 0.478268 11.00000 0.04372 0.03878 = 0.04711 0.00138 0.00921 0.00669 C1 1 0.272074 0.899438 0.563326 11.00000 0.06317 0.04129 = 0.06518 0.01056 -0.00888 0.00267 C49 1 0.225304 0.571133 0.430019 11.00000 0.05230 0.07386 = 0.07464 -0.00300 -0.00844 -0.00850 AFIX 43 H49 2 0.267750 0.589590 0.449395 11.00000 -1.20000 AFIX 0 B9 3 0.243513 1.123713 0.545285 11.00000 0.05840 0.04398 = 0.03552 -0.00119 0.00224 -0.00235 C8 1 0.228943 0.809051 0.664636 11.00000 0.05319 0.06587 = 0.05572 0.00119 0.00096 0.01091 C29 1 0.441242 0.586582 0.571337 11.00000 0.06518 0.10815 = 0.06708 -0.02037 -0.00023 0.01818 AFIX 43 H29 2 0.451703 0.644730 0.553461 11.00000 -1.20000 AFIX 0 B2 3 0.228136 1.046083 0.469510 11.00000 0.04531 0.03722 = 0.04033 -0.00152 0.00203 0.00691 C44 1 -0.004031 0.212743 0.388824 11.00000 0.07419 0.04992 = 0.07700 0.00094 0.00612 -0.00414 AFIX 43 H44 2 0.016617 0.155844 0.381906 11.00000 -1.20000 AFIX 0 C5 1 0.212643 0.569613 0.746265 11.00000 0.06986 0.13319 = 0.11219 0.07061 0.00895 -0.01188 C43 1 -0.057910 0.216945 0.428574 11.00000 0.06859 0.06336 = 0.05925 0.00994 -0.00260 -0.01416 AFIX 43 H43 2 -0.073968 0.162756 0.448111 11.00000 -1.20000 AFIX 0 B7 3 0.301954 1.209988 0.447706 11.00000 0.05055 0.05677 = 0.06204 0.00940 0.01440 -0.00074 B8 3 0.235299 1.237776 0.502967 11.00000 0.06790 0.03923 = 0.04568 -0.00275 0.01302 -0.00302 B4 3 0.215422 1.207818 0.409049 11.00000 0.05678 0.04492 = 0.04126 0.00492 0.00759 0.01159 C11 1 0.433138 0.821669 0.682656 11.00000 0.05528 0.07049 = 0.08501 -0.01053 -0.00075 -0.00259 AFIX 43 H11 2 0.403311 0.799420 0.713539 11.00000 -1.20000 AFIX 0 B1 3 0.185718 1.097584 0.398358 11.00000 0.05951 0.04574 = 0.03915 -0.00082 -0.00419 0.00730 C36 1 -0.028855 0.400823 0.124021 11.00000 0.06392 0.10969 = 0.05618 -0.03596 0.00033 0.00099 AFIX 43 H36 2 -0.065309 0.373106 0.097536 11.00000 -1.20000 AFIX 0 C16 1 0.584208 0.624893 0.712282 11.00000 0.05995 0.14449 = 0.04446 0.00951 0.00610 0.03616 C50 1 0.205891 0.481118 0.436170 11.00000 0.05746 0.06543 = 0.11079 0.01439 -0.02496 0.00290 AFIX 43 H50 2 0.235279 0.438184 0.459513 11.00000 -1.20000 AFIX 0 C37 1 0.025160 0.428726 0.090748 11.00000 0.08068 0.08432 = 0.04428 -0.01360 0.01204 0.01921 AFIX 43 H37 2 0.025313 0.419166 0.041563 11.00000 -1.20000 AFIX 0 C33 1 0.437430 0.479856 0.669403 11.00000 0.14006 0.06369 = 0.10688 -0.00755 -0.02373 0.02541 AFIX 43 H33 2 0.445527 0.466175 0.718144 11.00000 -1.20000 AFIX 0 C23 1 0.506559 0.680002 0.848349 11.00000 0.08987 0.09844 = 0.07263 -0.02452 0.02743 -0.03245 AFIX 43 H23 2 0.551418 0.692341 0.843994 11.00000 -1.20000 AFIX 0 C27 1 0.398387 0.627310 0.796425 11.00000 0.05853 0.11356 = 0.08058 0.00607 0.01327 -0.00311 AFIX 43 H27 2 0.370699 0.604838 0.757295 11.00000 -1.20000 AFIX 0 B3 3 0.269955 1.107476 0.399604 11.00000 0.06399 0.05320 = 0.04518 0.00235 0.01799 0.01522 C7 1 0.264924 0.564315 0.635625 11.00000 0.06662 0.05067 = 0.10824 0.02644 0.00319 0.00158 B6 3 0.311447 1.095091 0.489689 11.00000 0.04218 0.05759 = 0.06219 0.01395 0.00445 0.00709 C15 1 0.529826 0.802540 0.621840 11.00000 0.06957 0.14624 = 0.08751 0.03703 0.02128 0.00967 AFIX 43 H15 2 0.566112 0.766795 0.611021 11.00000 -1.20000 AFIX 0 C26 1 0.374084 0.636732 0.862456 11.00000 0.07582 0.13654 = 0.10739 0.02280 0.04132 -0.00241 AFIX 43 H26 2 0.330071 0.620504 0.867954 11.00000 -1.20000 AFIX 0 C17 1 0.630529 0.692196 0.739051 11.00000 0.05412 0.20284 = 0.07434 0.00064 0.00088 0.01182 AFIX 43 H17 2 0.616386 0.751772 0.750132 11.00000 -1.20000 AFIX 0 C6 1 0.240226 0.520003 0.694556 11.00000 0.07219 0.07423 = 0.15566 0.06221 -0.00531 -0.00862 B10 3 0.309944 1.194067 0.537882 11.00000 0.06322 0.06117 = 0.06408 0.00642 -0.01028 -0.01808 C30 1 0.412662 0.517295 0.525049 11.00000 0.08206 0.14064 = 0.07934 -0.03762 -0.00816 0.03529 AFIX 43 H30 2 0.403754 0.529691 0.476178 11.00000 -1.20000 AFIX 0 C25 1 0.415104 0.670143 0.919995 11.00000 0.14184 0.12648 = 0.09713 -0.02157 0.07011 -0.02229 AFIX 43 H25 2 0.397921 0.679656 0.963756 11.00000 -1.20000 AFIX 0 C12 1 0.424741 0.910033 0.653345 11.00000 0.08675 0.07789 = 0.10285 -0.01936 -0.02995 0.00385 AFIX 43 H12 2 0.389086 0.947016 0.664196 11.00000 -1.20000 AFIX 0 C21 1 0.605221 0.536240 0.694334 11.00000 0.10244 0.18484 = 0.07967 0.01219 0.02243 0.08092 AFIX 43 H21 2 0.574707 0.491624 0.675459 11.00000 -1.20000 AFIX 0 C14 1 0.521037 0.890898 0.593240 11.00000 0.10183 0.16364 = 0.11917 0.06194 0.01195 -0.02078 AFIX 43 H14 2 0.551241 0.914585 0.563359 11.00000 -1.20000 AFIX 0 C24 1 0.481612 0.689832 0.913747 11.00000 0.13618 0.12921 = 0.07837 -0.03891 0.04643 -0.05362 AFIX 43 H24 2 0.509430 0.709682 0.953673 11.00000 -1.20000 AFIX 0 C32 1 0.409494 0.414097 0.622403 11.00000 0.17272 0.06649 = 0.14179 -0.02407 -0.03608 0.03270 AFIX 43 H32 2 0.398289 0.355982 0.639766 11.00000 -1.20000 AFIX 0 C20 1 0.673341 0.516331 0.705490 11.00000 0.11212 0.27123 = 0.11748 0.03827 0.04074 0.11415 AFIX 43 H20 2 0.688575 0.457497 0.693949 11.00000 -1.20000 AFIX 0 C31 1 0.397872 0.432081 0.551113 11.00000 0.11945 0.09622 = 0.13538 -0.05573 -0.02639 0.03991 AFIX 43 H31 2 0.379734 0.386033 0.519923 11.00000 -1.20000 AFIX 0 C13 1 0.468564 0.942616 0.608787 11.00000 0.12807 0.10314 = 0.09882 0.02226 -0.03510 -0.03121 AFIX 43 H13 2 0.462238 1.001683 0.588649 11.00000 -1.20000 AFIX 0 C19 1 0.717691 0.581345 0.732879 11.00000 0.07993 0.38079 = 0.09426 0.08812 0.02907 0.10279 AFIX 43 H19 2 0.762757 0.565639 0.740929 11.00000 -1.20000 AFIX 0 C18 1 0.698135 0.668937 0.748926 11.00000 0.05494 0.31660 = 0.08944 0.02554 0.00384 0.02459 AFIX 43 H18 2 0.729667 0.713038 0.766378 11.00000 -1.20000 AFIX 0 H5 2 0.121985 1.152413 0.491262 11.00000 0.06172 H7 2 0.339325 1.257032 0.422699 11.00000 0.06376 H8 2 0.220328 1.306177 0.524624 11.00000 0.05622 H1A 2 0.317355 0.896808 0.548372 11.00000 0.07811 H1 2 0.148730 1.068001 0.360206 11.00000 0.06142 H4A 2 0.195231 1.262887 0.370645 11.00000 0.05147 H6 2 0.354732 1.046285 0.495871 11.00000 0.08011 H1B 2 0.273285 0.946713 0.598809 11.00000 0.06495 H9 2 0.231196 1.096583 0.597540 11.00000 0.05055 H10 2 0.347263 1.223217 0.585031 11.00000 0.08802 H5A 2 0.199797 0.530046 0.782197 11.00000 0.13674 H6A 2 0.246763 0.452514 0.692670 11.00000 0.12993 H3 2 0.297831 1.082300 0.351387 11.00000 0.08205 H7A 2 0.283238 0.531393 0.600954 11.00000 0.07528 H4 2 0.187931 0.693683 0.777341 11.00000 0.10632 HKLF 4 REM 19kub12_0m_a.res in P2(1)/c REM R1 = 0.0525 for 8601 Fo > 4sig(Fo) and 0.0762 for all 11891 data REM 718 parameters refined using 0 restraints END WGHT 0.0888 0.9968 REM Highest difference peak 0.318, deepest hole -0.261, 1-sigma level 0.043 Q1 1 0.0199 0.4710 0.2782 11.00000 0.05 0.32 Q2 1 0.4703 0.7361 0.8272 11.00000 0.05 0.31 Q3 1 0.0605 0.5052 0.3576 11.00000 0.05 0.26 Q4 1 0.5301 0.7602 0.5855 11.00000 0.05 0.25 Q5 1 -0.0030 0.4264 0.3485 11.00000 0.05 0.25 Q6 1 -0.0115 0.5406 0.3290 11.00000 0.05 0.24 Q7 1 -0.0294 0.3788 0.3975 11.00000 0.05 0.24 Q8 1 0.6091 0.6538 0.7821 11.00000 0.05 0.24 Q9 1 0.4760 0.6115 0.6652 11.00000 0.05 0.22 Q10 1 0.4844 0.6422 0.7535 11.00000 0.05 0.21 Q11 1 0.2091 0.8690 0.4500 11.00000 0.05 0.21 Q12 1 0.4317 0.7504 0.8844 11.00000 0.05 0.21 Q13 1 0.5420 0.6324 0.6910 11.00000 0.05 0.21 Q14 1 0.1874 1.0886 0.4453 11.00000 0.05 0.21 Q15 1 -0.0458 0.6036 0.3110 11.00000 0.05 0.20 Q16 1 -0.0354 0.5980 0.3647 11.00000 0.05 0.20 Q17 1 0.2110 1.1077 0.5050 11.00000 0.05 0.20 Q18 1 0.0374 0.4824 0.2215 11.00000 0.05 0.19 Q19 1 -0.0383 0.4247 0.1558 11.00000 0.05 0.19 Q20 1 0.0071 0.4313 0.2276 11.00000 0.05 0.19 ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P2 P 0.01954(2) 0.48166(3) 0.32916(2) 0.03975(12) Uani 1 1 d . . . . . S1 S 0.21108(3) 0.91998(3) 0.48641(3) 0.05517(15) Uani 1 1 d . . . . . P1 P 0.49633(3) 0.65179(5) 0.70276(3) 0.06090(17) Uani 1 1 d . . . . . O2 O 0.31251(9) 0.71470(11) 0.52925(9) 0.0675(4) Uani 1 1 d . . . . . C52 C -0.03628(9) 0.57681(12) 0.33898(9) 0.0417(4) Uani 1 1 d . . . . . N1 N 0.25960(8) 0.81374(11) 0.60112(9) 0.0506(4) Uani 1 1 d . . . . . O1 O 0.20801(10) 0.87465(15) 0.69567(10) 0.0894(6) Uani 1 1 d . . . . . C57 C -0.07686(9) 0.61204(14) 0.28131(10) 0.0476(4) Uani 1 1 d . . . . . H57 H -0.074909 0.587180 0.235626 0.057 Uiso 1 1 calc R . . . . C34 C 0.02435(9) 0.45747(13) 0.23582(10) 0.0429(4) Uani 1 1 d . . . . . C39 C 0.07896(10) 0.48597(14) 0.20139(11) 0.0483(4) Uani 1 1 d . . . . . H39 H 0.115180 0.515213 0.227130 0.058 Uiso 1 1 calc R . . . . C55 C -0.12339(11) 0.72136(15) 0.35893(12) 0.0580(5) Uani 1 1 d . . . . . H55 H -0.152734 0.770030 0.365611 0.070 Uiso 1 1 calc R . . . . C46 C 0.09993(9) 0.51572(13) 0.37162(9) 0.0430(4) Uani 1 1 d . . . . . C56 C -0.12053(10) 0.68447(15) 0.29150(12) 0.0559(5) Uani 1 1 d . . . . . H56 H -0.147959 0.708171 0.252639 0.067 Uiso 1 1 calc R . . . . C53 C -0.03896(11) 0.61501(16) 0.40706(11) 0.0576(5) Uani 1 1 d . . . . . H53 H -0.011132 0.592360 0.446023 0.069 Uiso 1 1 calc R . . . . C9 C 0.28098(10) 0.72734(13) 0.58000(11) 0.0488(4) Uani 1 1 d . . . . . C38 C 0.07886(12) 0.47032(15) 0.12826(12) 0.0593(5) Uani 1 1 d . . . . . H38 H 0.115451 0.488218 0.104767 0.071 Uiso 1 1 calc R . . . . C51 C 0.14287(11) 0.45257(15) 0.40809(13) 0.0609(5) Uani 1 1 d . . . . . H51 H 0.129439 0.391147 0.413725 0.073 Uiso 1 1 calc R . . . . C42 C -0.08789(11) 0.30070(18) 0.43940(11) 0.0600(6) Uani 1 1 d . . . . . H42 H -0.123977 0.302940 0.466796 0.072 Uiso 1 1 calc R . . . . C54 C -0.08306(12) 0.68658(16) 0.41645(12) 0.0635(6) Uani 1 1 d . . . . . H54 H -0.085498 0.711459 0.462054 0.076 Uiso 1 1 calc R . . . . C40 C -0.01105(9) 0.37864(13) 0.36962(10) 0.0439(4) Uani 1 1 d . . . . . C2 C 0.25878(10) 0.65957(15) 0.63259(12) 0.0543(5) Uani 1 1 d . . . . . C47 C 0.12056(11) 0.60770(15) 0.36569(13) 0.0608(5) Uani 1 1 d . . . . . H47 H 0.092085 0.651018 0.341455 0.073 Uiso 1 1 calc R . . . . C41 C -0.06540(9) 0.38223(15) 0.41023(10) 0.0501(4) Uani 1 1 d . . . . . H41 H -0.086346 0.438763 0.417675 0.060 Uiso 1 1 calc R . . . . C22 C 0.46405(12) 0.65132(17) 0.78839(13) 0.0639(6) Uani 1 1 d . . . . . C4 C 0.20596(14) 0.6645(3) 0.74229(17) 0.0842(9) Uani 1 1 d . . . . . C48 C 0.18282(12) 0.63478(17) 0.39551(13) 0.0657(6) Uani 1 1 d . . . . . H48 H 0.196114 0.696643 0.392210 0.079 Uiso 1 1 calc R . . . . C10 C 0.48563(10) 0.76664(18) 0.66613(12) 0.0621(6) Uani 1 1 d . . . . . C3 C 0.22957(10) 0.70887(17) 0.68398(12) 0.0603(5) Uani 1 1 d . . . . . C35 C -0.02918(11) 0.41391(18) 0.19718(12) 0.0638(6) Uani 1 1 d . . . . . H35 H -0.065308 0.393452 0.220361 0.077 Uiso 1 1 calc R . . . . C45 C 0.01931(11) 0.29281(15) 0.35929(13) 0.0591(5) Uani 1 1 d . . . . . H45 H 0.055601 0.289676 0.332242 0.071 Uiso 1 1 calc R . . . . C28 C 0.45366(13) 0.56739(19) 0.64381(14) 0.0726(7) Uani 1 1 d . . . . . B5 B 0.17489(11) 1.14753(14) 0.47827(12) 0.0429(4) Uani 1 1 d . . . . . C1 C 0.27207(12) 0.89944(15) 0.56333(14) 0.0576(5) Uani 1 1 d . . . . . C49 C 0.22530(12) 0.57113(18) 0.43002(13) 0.0680(6) Uani 1 1 d . . . . . H49 H 0.267750 0.589590 0.449395 0.082 Uiso 1 1 calc R . . . . B9 B 0.24351(12) 1.12371(15) 0.54528(11) 0.0461(5) Uani 1 1 d . . . . . C8 C 0.22894(11) 0.80905(16) 0.66464(12) 0.0586(5) Uani 1 1 d . . . . . C29 C 0.44124(13) 0.5866(2) 0.57134(14) 0.0806(8) Uani 1 1 d . . . . . H29 H 0.451703 0.644730 0.553461 0.097 Uiso 1 1 calc R . . . . B2 B 0.22814(10) 1.04608(14) 0.46951(11) 0.0411(4) Uani 1 1 d . . . . . C44 C -0.00403(13) 0.21274(16) 0.38882(14) 0.0671(6) Uani 1 1 d . . . . . H44 H 0.016617 0.155844 0.381906 0.081 Uiso 1 1 calc R . . . . C5 C 0.21264(17) 0.5696(3) 0.7463(2) 0.1051(13) Uani 1 1 d . . . . . C43 C -0.05791(12) 0.21694(17) 0.42857(12) 0.0644(6) Uani 1 1 d . . . . . H43 H -0.073968 0.162756 0.448111 0.077 Uiso 1 1 calc R . . . . B7 B 0.30195(12) 1.20999(18) 0.44771(14) 0.0559(6) Uani 1 1 d . . . . . B8 B 0.23530(13) 1.23778(16) 0.50297(12) 0.0504(5) Uani 1 1 d . . . . . B4 B 0.21542(12) 1.20782(16) 0.40905(12) 0.0475(5) Uani 1 1 d . . . . . C11 C 0.43314(12) 0.82167(18) 0.68266(15) 0.0708(6) Uani 1 1 d . . . . . H11 H 0.403311 0.799420 0.713539 0.085 Uiso 1 1 calc R . . . . B1 B 0.18572(12) 1.09758(16) 0.39836(12) 0.0488(5) Uani 1 1 d . . . . . C36 C -0.02886(13) 0.4008(2) 0.12402(13) 0.0770(8) Uani 1 1 d . . . . . H36 H -0.065309 0.373106 0.097536 0.092 Uiso 1 1 calc R . . . . C16 C 0.58421(13) 0.6249(2) 0.71228(12) 0.0829(9) Uani 1 1 d . . . . . C50 C 0.20589(12) 0.48112(19) 0.43617(17) 0.0802(8) Uani 1 1 d . . . . . H50 H 0.235279 0.438184 0.459513 0.096 Uiso 1 1 calc R . . . . C37 C 0.02516(13) 0.42873(19) 0.09075(12) 0.0694(7) Uani 1 1 d . . . . . H37 H 0.025313 0.419166 0.041563 0.083 Uiso 1 1 calc R . . . . C33 C 0.43743(19) 0.4799(2) 0.6694(2) 0.1061(11) Uani 1 1 d . . . . . H33 H 0.445527 0.466175 0.718144 0.127 Uiso 1 1 calc R . . . . C23 C 0.50656(16) 0.6800(2) 0.84835(15) 0.0857(8) Uani 1 1 d . . . . . H23 H 0.551418 0.692341 0.843994 0.103 Uiso 1 1 calc R . . . . C27 C 0.39839(13) 0.6273(2) 0.79643(16) 0.0838(8) Uani 1 1 d . . . . . H27 H 0.370699 0.604838 0.757295 0.101 Uiso 1 1 calc R . . . . B3 B 0.26995(13) 1.10748(17) 0.39960(12) 0.0533(5) Uani 1 1 d . . . . . C7 C 0.26492(13) 0.56431(18) 0.63563(19) 0.0756(8) Uani 1 1 d . . . . . B6 B 0.31145(11) 1.09509(18) 0.48969(14) 0.0540(6) Uani 1 1 d . . . . . C15 C 0.52983(15) 0.8025(3) 0.62184(17) 0.1002(11) Uani 1 1 d . . . . . H15 H 0.566112 0.766795 0.611021 0.120 Uiso 1 1 calc R . . . . C26 C 0.37408(16) 0.6367(3) 0.8625(2) 0.1044(11) Uani 1 1 d . . . . . H26 H 0.330071 0.620504 0.867954 0.125 Uiso 1 1 calc R . . . . C17 C 0.63053(14) 0.6922(3) 0.73905(16) 0.1108(13) Uani 1 1 d . . . . . H17 H 0.616386 0.751772 0.750132 0.133 Uiso 1 1 calc R . . . . C6 C 0.24023(16) 0.5200(3) 0.6946(3) 0.1019(12) Uani 1 1 d . . . . . B10 B 0.30994(14) 1.19407(19) 0.53788(15) 0.0640(7) Uani 1 1 d . . . . . C30 C 0.41266(16) 0.5173(3) 0.52505(18) 0.1018(11) Uani 1 1 d . . . . . H30 H 0.403754 0.529691 0.476178 0.122 Uiso 1 1 calc R . . . . C25 C 0.4151(2) 0.6701(3) 0.9200(2) 0.1178(13) Uani 1 1 d . . . . . H25 H 0.397921 0.679656 0.963756 0.141 Uiso 1 1 calc R . . . . C12 C 0.42474(17) 0.9100(2) 0.65335(19) 0.0919(9) Uani 1 1 d . . . . . H12 H 0.389086 0.947016 0.664196 0.110 Uiso 1 1 calc R . . . . C21 C 0.60522(19) 0.5362(3) 0.69433(18) 0.1214(15) Uani 1 1 d . . . . . H21 H 0.574707 0.491624 0.675459 0.146 Uiso 1 1 calc R . . . . C14 C 0.5210(2) 0.8909(4) 0.5932(2) 0.1282(15) Uani 1 1 d . . . . . H14 H 0.551241 0.914585 0.563359 0.154 Uiso 1 1 calc R . . . . C24 C 0.4816(2) 0.6898(3) 0.91375(18) 0.1121(13) Uani 1 1 d . . . . . H24 H 0.509430 0.709682 0.953673 0.135 Uiso 1 1 calc R . . . . C32 C 0.4095(2) 0.4141(2) 0.6224(3) 0.1306(16) Uani 1 1 d . . . . . H32 H 0.398289 0.355982 0.639766 0.157 Uiso 1 1 calc R . . . . C20 C 0.6733(3) 0.5163(5) 0.7055(3) 0.165(3) Uani 1 1 d . . . . . H20 H 0.688575 0.457497 0.693949 0.198 Uiso 1 1 calc R . . . . C31 C 0.3979(2) 0.4321(3) 0.5511(3) 0.1197(15) Uani 1 1 d . . . . . H31 H 0.379734 0.386033 0.519923 0.144 Uiso 1 1 calc R . . . . C13 C 0.4686(2) 0.9426(3) 0.6088(2) 0.1132(13) Uani 1 1 d . . . . . H13 H 0.462238 1.001683 0.588649 0.136 Uiso 1 1 calc R . . . . C19 C 0.7177(2) 0.5813(7) 0.7329(3) 0.184(4) Uani 1 1 d . . . . . H19 H 0.762757 0.565639 0.740929 0.220 Uiso 1 1 calc R . . . . C18 C 0.69814(18) 0.6689(5) 0.7489(2) 0.154(2) Uani 1 1 d . . . . . H18 H 0.729667 0.713038 0.766378 0.185 Uiso 1 1 calc R . . . . H5 H 0.1220(11) 1.1524(15) 0.4913(12) 0.062(6) Uiso 1 1 d . . . . . H7 H 0.3393(11) 1.2570(16) 0.4227(12) 0.064(6) Uiso 1 1 d . . . . . H8 H 0.2203(10) 1.3062(15) 0.5246(11) 0.056(6) Uiso 1 1 d . . . . . H1A H 0.3174(14) 0.8968(18) 0.5484(14) 0.078(8) Uiso 1 1 d . . . . . H1 H 0.1487(11) 1.0680(15) 0.3602(12) 0.061(6) Uiso 1 1 d . . . . . H4A H 0.1952(10) 1.2629(14) 0.3706(11) 0.051(5) Uiso 1 1 d . . . . . H6 H 0.3547(13) 1.0463(18) 0.4959(14) 0.080(7) Uiso 1 1 d . . . . . H1B H 0.2733(11) 0.9467(18) 0.5988(13) 0.065(7) Uiso 1 1 d . . . . . H9 H 0.2312(10) 1.0966(14) 0.5975(11) 0.051(5) Uiso 1 1 d . . . . . H10 H 0.3473(13) 1.2232(19) 0.5850(14) 0.088(8) Uiso 1 1 d . . . . . H5A H 0.1998(19) 0.530(3) 0.782(2) 0.137(13) Uiso 1 1 d . . . . . H6A H 0.2468(18) 0.453(3) 0.693(2) 0.130(12) Uiso 1 1 d . . . . . H3 H 0.2978(13) 1.0823(18) 0.3514(14) 0.082(8) Uiso 1 1 d . . . . . H7A H 0.2832(13) 0.5314(19) 0.6010(15) 0.075(9) Uiso 1 1 d . . . . . H4 H 0.1879(17) 0.694(2) 0.7773(18) 0.106(12) 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 P2 0.0402(2) 0.0415(2) 0.0377(2) -0.00587(18) 0.00454(17) 0.00288(18) S1 0.0663(3) 0.0380(2) 0.0578(3) 0.0016(2) -0.0101(2) 0.0012(2) P1 0.0498(3) 0.0809(4) 0.0519(3) -0.0044(3) 0.0048(2) 0.0112(3) O2 0.0780(10) 0.0558(9) 0.0728(10) 0.0039(8) 0.0271(8) 0.0075(8) C52 0.0441(9) 0.0423(9) 0.0386(9) -0.0067(7) 0.0043(7) 0.0049(7) N1 0.0536(9) 0.0443(9) 0.0539(9) 0.0081(7) 0.0050(7) 0.0085(7) O1 0.0999(14) 0.0903(14) 0.0802(12) -0.0176(10) 0.0193(10) 0.0258(11) C57 0.0497(10) 0.0560(11) 0.0371(9) -0.0036(8) 0.0039(8) 0.0062(9) C34 0.0431(9) 0.0464(10) 0.0400(9) -0.0077(8) 0.0077(7) 0.0049(8) C39 0.0486(10) 0.0482(10) 0.0495(10) -0.0017(8) 0.0119(8) 0.0029(8) C55 0.0608(12) 0.0487(11) 0.0658(13) -0.0051(10) 0.0129(10) 0.0157(9) C46 0.0440(9) 0.0433(9) 0.0412(9) -0.0035(8) 0.0020(7) 0.0014(8) C56 0.0529(11) 0.0597(12) 0.0546(11) 0.0069(10) 0.0026(9) 0.0128(9) C53 0.0667(13) 0.0627(13) 0.0411(10) -0.0128(9) -0.0052(9) 0.0176(10) C9 0.0471(10) 0.0416(10) 0.0574(11) 0.0075(8) 0.0041(9) 0.0062(8) C38 0.0690(14) 0.0595(13) 0.0535(12) 0.0021(10) 0.0257(10) 0.0113(11) C51 0.0557(12) 0.0466(11) 0.0779(15) 0.0051(10) -0.0046(11) 0.0012(9) C42 0.0517(11) 0.0842(16) 0.0444(10) 0.0056(10) 0.0062(9) -0.0122(11) C54 0.0756(14) 0.0630(13) 0.0523(12) -0.0206(10) 0.0076(10) 0.0166(11) C40 0.0437(9) 0.0473(10) 0.0406(9) -0.0042(8) 0.0045(7) -0.0020(8) C2 0.0447(10) 0.0512(11) 0.0661(13) 0.0170(10) 0.0010(9) 0.0035(9) C47 0.0620(13) 0.0485(11) 0.0688(14) 0.0084(10) -0.0088(10) -0.0029(10) C41 0.0439(10) 0.0624(12) 0.0438(10) -0.0017(9) 0.0040(8) 0.0020(9) C22 0.0640(13) 0.0660(14) 0.0645(13) -0.0059(11) 0.0201(11) -0.0044(11) C4 0.0641(15) 0.119(3) 0.0698(17) 0.0338(18) 0.0110(13) -0.0030(16) C48 0.0680(14) 0.0546(13) 0.0729(15) 0.0004(11) -0.0004(11) -0.0163(11) C10 0.0436(11) 0.0837(16) 0.0581(12) 0.0005(11) 0.0016(9) -0.0021(10) C3 0.0450(10) 0.0783(15) 0.0570(12) 0.0180(11) 0.0017(9) 0.0013(10) C35 0.0493(11) 0.0886(17) 0.0547(12) -0.0261(12) 0.0117(9) -0.0079(11) C45 0.0581(12) 0.0496(11) 0.0720(14) -0.0065(10) 0.0192(10) -0.0010(9) C28 0.0683(14) 0.0774(17) 0.0699(15) -0.0127(13) -0.0036(12) 0.0250(13) B5 0.0437(11) 0.0388(10) 0.0471(11) 0.0014(8) 0.0092(9) 0.0067(8) C1 0.0632(14) 0.0413(11) 0.0652(13) 0.0106(10) -0.0089(11) 0.0027(9) C49 0.0523(12) 0.0739(16) 0.0746(15) -0.0030(12) -0.0084(11) -0.0085(11) B9 0.0584(13) 0.0440(11) 0.0355(10) -0.0012(9) 0.0022(9) -0.0023(9) C8 0.0532(11) 0.0659(14) 0.0557(12) 0.0012(10) 0.0010(9) 0.0109(10) C29 0.0652(14) 0.108(2) 0.0671(15) -0.0204(15) -0.0002(12) 0.0182(14) B2 0.0453(10) 0.0372(10) 0.0403(10) -0.0015(8) 0.0020(8) 0.0069(8) C44 0.0742(15) 0.0499(12) 0.0770(15) 0.0009(11) 0.0061(12) -0.0041(11) C5 0.0699(18) 0.133(3) 0.112(3) 0.071(3) 0.0090(18) -0.0119(19) C43 0.0686(14) 0.0634(14) 0.0593(13) 0.0099(11) -0.0026(11) -0.0142(11) B7 0.0505(12) 0.0568(14) 0.0620(14) 0.0094(11) 0.0144(11) -0.0007(11) B8 0.0679(14) 0.0392(11) 0.0457(11) -0.0028(9) 0.0130(10) -0.0030(10) B4 0.0568(12) 0.0449(11) 0.0413(11) 0.0049(9) 0.0076(9) 0.0116(10) C11 0.0553(13) 0.0705(16) 0.0850(17) -0.0105(13) -0.0008(12) -0.0026(11) B1 0.0595(13) 0.0457(12) 0.0391(10) -0.0008(9) -0.0042(9) 0.0073(10) C36 0.0639(14) 0.110(2) 0.0562(13) -0.0360(14) 0.0003(11) 0.0010(14) C16 0.0599(14) 0.144(3) 0.0445(12) 0.0095(14) 0.0061(10) 0.0362(17) C50 0.0575(13) 0.0654(15) 0.111(2) 0.0144(14) -0.0250(13) 0.0029(11) C37 0.0807(16) 0.0843(17) 0.0443(11) -0.0136(11) 0.0120(11) 0.0192(13) C33 0.140(3) 0.0637(18) 0.107(2) -0.0076(16) -0.024(2) 0.0254(18) C23 0.0899(19) 0.098(2) 0.0726(16) -0.0245(15) 0.0274(14) -0.0325(16) C27 0.0585(14) 0.114(2) 0.0806(18) 0.0061(16) 0.0133(13) -0.0031(14) B3 0.0640(14) 0.0532(13) 0.0452(12) 0.0023(10) 0.0180(10) 0.0152(11) C7 0.0666(15) 0.0507(13) 0.108(2) 0.0264(14) 0.0032(15) 0.0016(11) B6 0.0422(11) 0.0576(14) 0.0622(14) 0.0139(11) 0.0045(10) 0.0071(10) C15 0.0696(17) 0.146(3) 0.088(2) 0.037(2) 0.0213(15) 0.0097(18) C26 0.0758(18) 0.137(3) 0.107(3) 0.023(2) 0.0413(18) -0.0024(19) C17 0.0541(15) 0.203(4) 0.0743(18) 0.001(2) 0.0009(13) 0.012(2) C6 0.0722(18) 0.074(2) 0.156(3) 0.062(2) -0.005(2) -0.0086(15) B10 0.0632(15) 0.0612(15) 0.0641(15) 0.0064(12) -0.0103(12) -0.0181(12) C30 0.0821(19) 0.141(3) 0.0793(19) -0.038(2) -0.0082(15) 0.035(2) C25 0.142(3) 0.126(3) 0.097(3) -0.022(2) 0.070(3) -0.022(3) C12 0.0868(19) 0.0779(19) 0.103(2) -0.0194(17) -0.0300(18) 0.0038(15) C21 0.102(2) 0.185(4) 0.080(2) 0.012(2) 0.0224(17) 0.081(3) C14 0.102(3) 0.164(4) 0.119(3) 0.062(3) 0.012(2) -0.021(3) C24 0.136(3) 0.129(3) 0.0784(19) -0.0389(19) 0.046(2) -0.054(2) C32 0.173(4) 0.066(2) 0.142(4) -0.024(2) -0.036(3) 0.033(2) C20 0.112(3) 0.271(7) 0.117(4) 0.038(4) 0.041(3) 0.114(4) C31 0.119(3) 0.096(3) 0.135(3) -0.056(2) -0.026(2) 0.040(2) C13 0.128(3) 0.103(3) 0.099(2) 0.022(2) -0.035(2) -0.031(2) C19 0.080(3) 0.381(11) 0.094(3) 0.088(5) 0.029(2) 0.103(5) C18 0.0549(18) 0.317(8) 0.089(2) 0.026(3) 0.0038(17) 0.025(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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C52 P2 C34 110.17(8) . . C52 P2 C46 107.04(9) . . C52 P2 C40 109.81(9) . . C34 P2 C46 110.36(9) . . C34 P2 C40 107.82(9) . . C46 P2 C40 111.65(9) . . C1 S1 B2 99.78(10) . . C22 P1 C28 110.69(13) . . C22 P1 C16 110.67(11) . . C10 P1 C22 107.82(11) . . C10 P1 C28 110.77(12) . . C10 P1 C16 108.29(13) . . C28 P1 C16 108.58(14) . . C57 C52 P2 121.74(14) . . C57 C52 C53 119.72(17) . . C53 C52 P2 118.53(14) . . C9 N1 C1 123.04(18) . . C9 N1 C8 112.18(17) . . C8 N1 C1 124.66(19) . . C52 C57 C56 119.93(18) . . C39 C34 P2 121.24(15) . . C35 C34 P2 118.69(14) . . C35 C34 C39 119.99(18) . . C38 C39 C34 119.2(2) . . C54 C55 C56 120.18(19) . . C51 C46 P2 121.93(15) . . C51 C46 C47 118.99(18) . . C47 C46 P2 119.04(15) . . C55 C56 C57 120.10(19) . . C54 C53 C52 119.66(19) . . O2 C9 N1 124.24(18) . . O2 C9 C2 129.82(19) . . N1 C9 C2 105.92(17) . . C37 C38 C39 120.0(2) . . C46 C51 C50 119.7(2) . . C43 C42 C41 121.1(2) . . C55 C54 C53 120.40(19) . . C41 C40 P2 121.34(15) . . C41 C40 C45 119.08(18) . . C45 C40 P2 119.57(15) . . C3 C2 C9 107.83(19) . . C7 C2 C9 130.4(2) . . C7 C2 C3 121.8(2) . . C48 C47 C46 120.2(2) . . C42 C41 C40 119.3(2) . . C23 C22 P1 117.95(18) . . C27 C22 P1 122.3(2) . . C27 C22 C23 119.7(2) . . C5 C4 C3 117.3(3) . . C49 C48 C47 120.2(2) . . C11 C10 P1 120.42(19) . . C15 C10 P1 121.1(2) . . C15 C10 C11 118.5(3) . . C2 C3 C4 121.3(3) . . C2 C3 C8 108.78(19) . . C4 C3 C8 129.9(3) . . C36 C35 C34 119.8(2) . . C44 C45 C40 120.5(2) . . C29 C28 P1 119.7(2) . . C29 C28 C33 119.4(3) . . C33 C28 P1 120.7(2) . . B9 B5 B2 59.73(12) . . B9 B5 B8 60.62(13) . . B9 B5 B4 102.66(15) . . B8 B5 B2 102.12(15) . . B8 B5 B4 60.11(12) . . B4 B5 B2 90.32(13) . . B1 B5 B9 112.12(15) . . B1 B5 B2 56.83(12) . . B1 B5 B8 112.73(16) . . B1 B5 B4 57.61(13) . . N1 C1 S1 112.75(15) . . C50 C49 C48 120.3(2) . . B5 B9 B2 60.81(11) . . B5 B9 B8 59.78(13) . . B5 B9 B6 102.02(14) . . B2 B9 B8 102.28(14) . . B2 B9 B6 59.80(12) . . B8 B9 B6 89.67(14) . . B10 B9 B5 112.65(16) . . B10 B9 B2 112.16(17) . . B10 B9 B8 57.61(14) . . B10 B9 B6 56.66(15) . . N1 C8 C3 105.15(18) . . O1 C8 N1 125.4(2) . . O1 C8 C3 129.4(2) . . C28 C29 C30 119.1(3) . . B5 B2 S1 129.48(14) . . B5 B2 B3 89.83(13) . . B9 B2 S1 118.86(13) . . B9 B2 B5 59.46(12) . . B9 B2 B3 102.01(15) . . B9 B2 B6 61.23(13) . . B1 B2 S1 118.18(14) . . B1 B2 B5 57.62(12) . . B1 B2 B9 112.59(15) . . B1 B2 B3 57.30(13) . . B1 B2 B6 112.13(17) . . B3 B2 S1 133.12(14) . . B6 B2 S1 121.22(13) . . B6 B2 B5 102.08(15) . . B6 B2 B3 59.16(13) . . C43 C44 C45 120.0(2) . . C6 C5 C4 121.7(3) . . C42 C43 C44 120.1(2) . . B8 B7 B6 90.22(15) . . B4 B7 B8 59.88(13) . . B4 B7 B6 102.09(16) . . B3 B7 B8 102.47(16) . . B3 B7 B4 60.65(13) . . B3 B7 B6 59.76(14) . . B10 B7 B8 57.55(15) . . B10 B7 B4 112.58(17) . . B10 B7 B3 112.26(18) . . B10 B7 B6 56.98(15) . . B5 B8 B9 59.60(12) . . B5 B8 B7 102.30(15) . . B5 B8 B4 60.37(13) . . B9 B8 B7 90.63(15) . . B4 B8 B9 102.12(15) . . B4 B8 B7 59.95(13) . . B10 B8 B5 112.33(17) . . B10 B8 B9 57.43(14) . . B10 B8 B7 57.52(15) . . B10 B8 B4 112.61(17) . . B5 B4 B3 90.65(14) . . B7 B4 B5 101.86(15) . . B7 B4 B3 59.49(14) . . B8 B4 B5 59.52(12) . . B8 B4 B7 60.17(14) . . B8 B4 B3 101.85(15) . . B1 B4 B5 57.46(12) . . B1 B4 B7 112.02(16) . . B1 B4 B8 112.05(16) . . B1 B4 B3 57.43(14) . . C10 C11 C12 120.0(3) . . B5 B1 B4 64.93(13) . . B5 B1 B3 99.84(16) . . B2 B1 B5 65.55(13) . . B2 B1 B4 99.96(16) . . B2 B1 B3 66.45(14) . . B4 B1 B3 65.25(14) . . C37 C36 C35 119.7(2) . . C17 C16 P1 119.9(3) . . C21 C16 P1 119.4(3) . . C21 C16 C17 120.7(3) . . C49 C50 C51 120.6(2) . . C38 C37 C36 121.2(2) . . C32 C33 C28 119.6(4) . . C24 C23 C22 119.6(3) . . C26 C27 C22 120.0(3) . . B7 B3 B2 101.52(15) . . B7 B3 B4 59.86(13) . . B7 B3 B6 60.66(14) . . B4 B3 B2 89.20(14) . . B1 B3 B2 56.26(12) . . B1 B3 B7 112.24(16) . . B1 B3 B4 57.31(13) . . B1 B3 B6 111.62(16) . . B6 B3 B2 59.63(12) . . B6 B3 B4 102.17(15) . . C2 C7 C6 116.4(3) . . B2 B6 B9 58.97(12) . . B2 B6 B7 101.88(15) . . B7 B6 B9 89.48(15) . . B3 B6 B9 101.88(15) . . B3 B6 B2 61.22(13) . . B3 B6 B7 59.58(14) . . B10 B6 B9 57.03(14) . . B10 B6 B2 111.73(17) . . B10 B6 B7 57.51(15) . . B10 B6 B3 112.57(18) . . C10 C15 C14 120.8(3) . . C25 C26 C27 119.8(3) . . C18 C17 C16 119.1(4) . . C5 C6 C7 121.5(3) . . B9 B10 B7 99.61(17) . . B9 B10 B8 64.96(15) . . B7 B10 B8 64.92(15) . . B6 B10 B9 66.31(15) . . B6 B10 B7 65.50(16) . . B6 B10 B8 99.75(17) . . C31 C30 C29 120.4(3) . . C26 C25 C24 120.9(3) . . C13 C12 C11 119.9(3) . . C16 C21 C20 118.0(5) . . C13 C14 C15 119.6(4) . . C23 C24 C25 119.8(3) . . C31 C32 C33 121.2(4) . . C19 C20 C21 121.0(6) . . C32 C31 C30 120.1(3) . . C14 C13 C12 121.0(4) . . C20 C19 C18 121.7(4) . . C19 C18 C17 119.5(5) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 P2 C52 1.7869(18) . P2 C34 1.7914(18) . P2 C46 1.7927(19) . P2 C40 1.796(2) . S1 C1 1.815(2) . S1 B2 1.873(2) . P1 C22 1.788(2) . P1 C10 1.787(3) . P1 C28 1.794(3) . P1 C16 1.798(3) . O2 C9 1.207(2) . C52 C57 1.379(3) . C52 C53 1.392(3) . N1 C9 1.382(2) . N1 C1 1.452(3) . N1 C8 1.394(3) . O1 C8 1.203(3) . C57 C56 1.385(3) . C34 C39 1.389(3) . C34 C35 1.382(3) . C39 C38 1.385(3) . C55 C56 1.374(3) . C55 C54 1.372(3) . C46 C51 1.381(3) . C46 C47 1.390(3) . C53 C54 1.378(3) . C9 C2 1.483(3) . C38 C37 1.362(3) . C51 C50 1.382(3) . C42 C41 1.385(3) . C42 C43 1.367(3) . C40 C41 1.393(3) . C40 C45 1.395(3) . C2 C3 1.372(3) . C2 C7 1.372(3) . C47 C48 1.372(3) . C22 C23 1.400(4) . C22 C27 1.386(3) . C4 C3 1.387(3) . C4 C5 1.367(5) . C48 C49 1.365(3) . C10 C11 1.377(3) . C10 C15 1.374(4) . C3 C8 1.481(3) . C35 C36 1.381(3) . C45 C44 1.377(3) . C28 C29 1.380(4) . C28 C33 1.393(4) . B5 B9 1.798(3) . B5 B2 1.822(3) . B5 B8 1.801(3) . B5 B4 1.817(3) . B5 B1 1.691(3) . C49 C50 1.356(4) . B9 B2 1.803(3) . B9 B8 1.816(3) . B9 B6 1.844(3) . B9 B10 1.690(3) . C29 C30 1.401(4) . B2 B1 1.676(3) . B2 B3 1.847(3) . B2 B6 1.819(3) . C44 C43 1.375(3) . C5 C6 1.363(6) . B7 B8 1.817(3) . B7 B4 1.813(3) . B7 B3 1.806(4) . B7 B6 1.826(3) . B7 B10 1.693(4) . B8 B4 1.812(3) . B8 B10 1.693(4) . B4 B1 1.694(3) . B4 B3 1.827(3) . C11 C12 1.383(4) . B1 B3 1.696(4) . C36 C37 1.365(4) . C16 C17 1.397(5) . C16 C21 1.391(5) . C33 C32 1.369(5) . C23 C24 1.375(4) . C27 C26 1.380(4) . B3 B6 1.810(4) . C7 C6 1.405(5) . B6 B10 1.683(4) . C15 C14 1.379(5) . C26 C25 1.373(5) . C17 C18 1.392(5) . C30 C31 1.359(6) . C25 C24 1.382(5) . C12 C13 1.355(5) . C21 C20 1.392(6) . C14 C13 1.345(6) . C32 C31 1.354(6) . C20 C19 1.353(10) . C19 C18 1.358(9) .