#------------------------------------------------------------------------------ #$Date: 2020-03-05 01:31:14 +0200 (Thu, 05 Mar 2020) $ #$Revision: 248800 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125695.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_7125695 loop_ _publ_author_name 'G\'omez-Torres, Alejandra' 'Aguilar-Calder\'on, J Rolando' 'Saucedo, Carlos' 'Jordan, Aldo' 'Metta-Maga\~na, Alejandro' 'Pinter, Balazs' 'Fortier, Skye' _publ_section_title ; Reversible oxidative-addition and reductive-elimination of thiophene from a titanium complex and its thermally-induced hydrodesulphurization chemistry. ; _journal_issue 10 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 1545 _journal_page_last 1548 _journal_paper_doi 10.1039/c9cc09267f _journal_volume 56 _journal_year 2020 _chemical_formula_moiety 'C65 H92 N6 S Ti, 3(C3)' _chemical_formula_sum 'C74 H92 N6 S Ti' _chemical_formula_weight 1145.49 _chemical_name_systematic DippL2Ti_k2-S(CH)3CH _chemical_properties_physical Air-sensitive,Moisture-sensitive,Light-sensitive,Photo-sensitive _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_block_doi 10.5517/ccdc.csd.cc23wzmm _audit_creation_date 2019-11-02 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-11-03 deposited with the CCDC. 2019-12-26 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 110.80(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.184(4) _cell_length_b 16.616(3) _cell_length_c 23.789(5) _cell_measurement_reflns_used 9842 _cell_measurement_temperature 100 _cell_measurement_theta_max 25.926 _cell_measurement_theta_min 2.361 _cell_volume 7089(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 'XL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_av_unetI/netI 0.0359 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 135214 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.366 _diffrn_reflns_theta_min 2.090 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.193 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6836 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1194 before and 0.0627 after correction. The Ratio of minimum to maximum transmission is 0.9171. The \l/2 correction factor is Not present.' _exptl_crystal_colour 'clear dark red' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.073 _exptl_crystal_description needle _exptl_crystal_F_000 2464 _exptl_crystal_recrystallization_method 'Toluene/hexanes at -32 celsius' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.313 _refine_diff_density_min -0.642 _refine_diff_density_rms 0.067 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 765 _refine_ls_number_reflns 14454 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.032 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0673 _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^)+(0.1038P)^2^+8.6153P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1837 _refine_ls_wR_factor_ref 0.2059 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10775 _reflns_number_total 14454 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc09267f2.cif _cod_data_source_block at_bthio_2_0m _cod_depositor_comments 'Adding full bibliography for 7125695.cif.' _cod_database_code 7125695 _shelx_shelxl_version_number 2017/1 _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 0.981 _shelx_estimated_absorpt_t_min 0.972 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C20(H20), C11(H11), C8(H8), C23(H23), C59(H59), C56(H56), C44(H44), C47(H47) 2.b Aromatic/amide H refined with riding coordinates: C37(H37), C64(H64), C36(H36), C40(H40), C6(H6), C4(H4), C54(H54), C5(H5), C18(H18), C62(H62), C52(H52), C41(H41), C53(H53), C16(H16), C63(H63), C42(H42), C17(H17) 2.c Idealised Me refined as rotating group: C13(H13A,H13B,H13C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C32(H32A,H32B, H32C), C9(H9A,H9B,H9C), C21(H21A,H21B,H21C), C10(H10A,H10B,H10C), C12(H12A, H12B,H12C), C30(H30A,H30B,H30C), C22(H22A,H22B,H22C), C61(H61A,H61B,H61C), C34(H34A,H34B,H34C), C33(H33A,H33B,H33C), C24(H24A,H24B,H24C), C58(H58A,H58B, H58C), C25(H25A,H25B,H25C), C57(H57A,H57B,H57C), C60(H60A,H60B,H60C), C45(H45A, H45B,H45C), C46(H46A,H46B,H46C), C49(H49A,H49B,H49C), C48(H48A,H48B,H48C) ; _shelx_res_file ; TITL at_bthio_2_0m_a.res in P2(1)/n at_bthio_2_0m.res created by SHELXL-2017/1 at 15:18:37 on 02-Nov-2019 REM Old TITL AT_BThio_2_0m in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.205, Rweak 0.012, Alpha 0.056 REM 0.459 for 524 systematic absences, Orientation as input REM Formula found by SHELXT: C74 N6 S Ti1 H92 CELL 0.71073 19.1842 16.6158 23.7894 90 110.801 90 ZERR 4 0.0038 0.0033 0.0048 0 0.03 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N S Ti UNIT 296 368 24 4 4 L.S. 16 PLAN 20 SIZE 0.15 0.1 0.1 TEMP 100 list 4 fmap 2 53 acta REM REM REM WGHT 0.103800 8.615301 FVAR 0.29329 TI1 5 0.570597 0.660561 0.284612 11.00000 0.01970 0.02302 = 0.02358 0.00297 0.00657 0.00111 S1 4 0.658012 0.762514 0.281203 11.00000 0.03688 0.03773 = 0.03543 -0.00210 0.01055 -0.01223 N2 3 0.458657 0.628656 0.271869 11.00000 0.02226 0.02580 = 0.03007 0.00462 0.00993 -0.00080 N1 3 0.482695 0.721480 0.214319 11.00000 0.01980 0.02430 = 0.02589 0.00409 0.00526 -0.00050 N4 3 0.616856 0.569440 0.275057 11.00000 0.02353 0.02738 = 0.02506 -0.00076 0.00676 -0.00038 N6 3 0.685458 0.466510 0.246169 11.00000 0.03365 0.02631 = 0.02804 -0.00325 0.01004 0.00508 N5 3 0.692579 0.467031 0.340374 11.00000 0.03288 0.02741 = 0.02607 0.00096 0.00551 0.00845 N3 3 0.353335 0.694768 0.205513 11.00000 0.02092 0.02593 = 0.04066 0.00591 0.00687 -0.00147 C1 1 0.429135 0.681416 0.226693 11.00000 0.02234 0.02355 = 0.02947 -0.00007 0.00816 -0.00043 C35 1 0.661158 0.507879 0.286205 11.00000 0.02467 0.02349 = 0.02647 -0.00237 0.00658 0.00028 C14 1 0.471081 0.790564 0.176788 11.00000 0.01913 0.02653 = 0.02877 0.00583 0.00051 -0.00203 C2 1 0.412532 0.589648 0.300135 11.00000 0.02226 0.03091 = 0.03599 0.00764 0.01129 0.00005 C38 1 0.702368 0.498508 0.399548 11.00000 0.03877 0.03053 = 0.02492 0.00243 0.00787 0.01040 C7 1 0.381707 0.513359 0.279806 11.00000 0.02817 0.03036 = 0.03957 0.00681 0.01215 -0.00219 C50 1 0.678137 0.491871 0.185950 11.00000 0.03655 0.02814 = 0.02641 -0.00366 0.01160 0.00717 C15 1 0.496671 0.789734 0.128024 11.00000 0.03075 0.03404 = 0.03007 0.00616 0.00658 -0.00244 C19 1 0.439802 0.861477 0.191038 11.00000 0.02071 0.02741 = 0.04209 0.00536 0.00472 0.00091 C20 1 0.537132 0.718995 0.113011 11.00000 0.03892 0.04095 = 0.02823 0.00074 0.01206 -0.00319 AFIX 13 H20 2 0.536659 0.674163 0.139641 11.00000 -1.20000 AFIX 0 C51 1 0.735712 0.537214 0.178757 11.00000 0.04193 0.03264 = 0.03799 -0.00662 0.01735 0.00047 C3 1 0.399248 0.627450 0.348661 11.00000 0.03143 0.03591 = 0.03891 0.00560 0.01519 0.00020 C37 1 0.729813 0.401801 0.275354 11.00000 0.04606 0.02972 = 0.03680 -0.00178 0.01172 0.01473 AFIX 43 H37 2 0.752408 0.364805 0.257941 11.00000 -1.20000 AFIX 0 C11 1 0.395145 0.467969 0.228862 11.00000 0.03344 0.03007 = 0.04190 0.00179 0.01346 -0.00765 AFIX 13 H11 2 0.420338 0.504477 0.209882 11.00000 -1.20000 AFIX 0 C39 1 0.653478 0.477187 0.427977 11.00000 0.04062 0.05090 = 0.03132 0.01162 0.01062 0.00944 C55 1 0.617160 0.464356 0.137498 11.00000 0.03867 0.03434 = 0.03188 -0.00812 0.01204 0.00285 C8 1 0.434534 0.706761 0.376830 11.00000 0.04118 0.03877 = 0.04000 -0.00210 0.02366 -0.00538 AFIX 13 H8 2 0.467661 0.724881 0.356097 11.00000 -1.20000 AFIX 0 C65 1 0.606882 0.679761 0.375165 11.00000 0.03483 0.03939 = 0.03337 0.00669 0.01508 0.00739 PART 1 C64 1 0.640713 0.737397 0.411334 11.00000 0.04389 0.05432 = 0.02488 0.00589 0.00950 0.01071 AFIX 43 H64 2 0.642658 0.733046 0.450838 11.00000 -1.20000 AFIX 0 PART 0 C36 1 0.734214 0.402133 0.332326 11.00000 0.04393 0.03042 = 0.03744 0.00256 0.00965 0.01669 AFIX 43 H36 2 0.760493 0.365465 0.361758 11.00000 -1.20000 AFIX 0 C26 1 0.295877 0.683840 0.158244 11.00000 0.02341 0.02509 = 0.04777 0.00695 0.00344 -0.00270 C40 1 0.668194 0.506929 0.486273 11.00000 0.05855 0.06608 = 0.03175 0.01279 0.02095 0.01709 AFIX 43 H40 2 0.636199 0.493768 0.506470 11.00000 -1.20000 AFIX 0 C13 1 0.321130 0.441897 0.180947 11.00000 0.03821 0.04087 = 0.04774 -0.00036 0.01199 -0.00723 AFIX 137 H13A 2 0.298805 0.400369 0.197001 11.00000 -1.50000 H13B 2 0.330223 0.421775 0.146349 11.00000 -1.50000 H13C 2 0.288047 0.487231 0.169507 11.00000 -1.50000 AFIX 0 C23 1 0.422634 0.869175 0.248254 11.00000 0.02814 0.02952 = 0.05626 -0.00212 0.01838 -0.00219 AFIX 13 H23 2 0.405146 0.816374 0.256020 11.00000 -1.20000 AFIX 0 C27 1 0.298518 0.656666 0.096706 11.00000 0.02846 0.03626 = 0.03943 0.00514 -0.00357 -0.00551 C6 1 0.336196 0.477674 0.307569 11.00000 0.03879 0.03712 = 0.05178 0.00577 0.01888 -0.01191 AFIX 43 H6 2 0.315641 0.427289 0.294634 11.00000 -1.20000 AFIX 0 C59 1 0.555571 0.415685 0.146942 11.00000 0.04300 0.05262 = 0.03162 -0.00650 0.01025 -0.00726 AFIX 13 H59 2 0.553688 0.430109 0.186321 11.00000 -1.20000 AFIX 0 C43 1 0.764536 0.547501 0.426839 11.00000 0.05241 0.04487 = 0.02920 -0.00402 0.01050 -0.00571 C4 1 0.352625 0.588840 0.374078 11.00000 0.04566 0.04843 = 0.04813 0.00204 0.02667 -0.00505 AFIX 43 H4 2 0.342831 0.613591 0.405550 11.00000 -1.20000 AFIX 0 C54 1 0.616234 0.480849 0.079618 11.00000 0.04874 0.05260 = 0.02829 -0.00769 0.01286 0.00117 AFIX 43 H54 2 0.576538 0.462998 0.046403 11.00000 -1.20000 AFIX 0 C5 1 0.321046 0.515422 0.353704 11.00000 0.04654 0.05017 = 0.05630 0.00618 0.03136 -0.01193 AFIX 43 H5 2 0.289647 0.491215 0.370830 11.00000 -1.20000 AFIX 0 C28 1 0.368201 0.607536 0.103324 11.00000 0.03656 0.03788 = 0.03305 0.00172 0.00414 -0.00376 AFIX 137 H28A 2 0.411779 0.638773 0.124363 11.00000 -1.50000 H28B 2 0.368379 0.593624 0.064209 11.00000 -1.50000 H28C 2 0.368282 0.559304 0.125565 11.00000 -1.50000 AFIX 0 C29 1 0.300424 0.734775 0.061288 11.00000 0.03909 0.04271 = 0.03835 0.01045 -0.00580 -0.00441 AFIX 137 H29A 2 0.253664 0.762455 0.051370 11.00000 -1.50000 H29B 2 0.308841 0.721092 0.025009 11.00000 -1.50000 H29C 2 0.339945 0.769004 0.085616 11.00000 -1.50000 AFIX 0 C18 1 0.429733 0.927872 0.152918 11.00000 0.04606 0.03169 = 0.05538 0.01319 0.00991 0.00979 AFIX 43 H18 2 0.407676 0.974219 0.160880 11.00000 -1.20000 AFIX 0 C32 1 0.235287 0.744350 0.227342 11.00000 0.02815 0.04297 = 0.07928 -0.00036 0.02187 0.00471 AFIX 137 H32A 2 0.263305 0.708660 0.259050 11.00000 -1.50000 H32B 2 0.188729 0.757153 0.231803 11.00000 -1.50000 H32C 2 0.263213 0.792883 0.229323 11.00000 -1.50000 AFIX 0 C31 1 0.220435 0.703774 0.166984 11.00000 0.02134 0.03825 = 0.06750 0.00450 0.00839 0.00097 C56 1 0.800464 0.569511 0.231921 11.00000 0.04819 0.05346 = 0.04282 -0.01384 0.01747 -0.01522 AFIX 13 H56 2 0.787489 0.563882 0.268029 11.00000 -1.20000 AFIX 0 PART 1 C62 1 0.686329 0.821953 0.344605 11.00000 0.04063 0.03308 = 0.04208 -0.00115 0.00140 -0.00774 AFIX 43 H62 2 0.711639 0.868921 0.342470 11.00000 -1.20000 AFIX 0 PART 0 C52 1 0.731992 0.551443 0.119828 11.00000 0.05694 0.04369 = 0.04365 -0.00640 0.02667 -0.00645 AFIX 43 H52 2 0.769850 0.580559 0.113343 11.00000 -1.20000 AFIX 0 C41 1 0.728386 0.554685 0.513888 11.00000 0.08470 0.04568 = 0.02690 -0.00064 0.01898 0.00541 AFIX 43 H41 2 0.737259 0.573444 0.552648 11.00000 -1.20000 AFIX 0 C9 1 0.376986 0.772946 0.371083 11.00000 0.05153 0.04268 = 0.06319 -0.00654 0.03520 -0.00008 AFIX 137 H9A 2 0.350378 0.784128 0.329329 11.00000 -1.50000 H9B 2 0.401922 0.820832 0.390733 11.00000 -1.50000 H9C 2 0.342542 0.755417 0.389579 11.00000 -1.50000 AFIX 0 C53 1 0.673508 0.523279 0.071236 11.00000 0.06460 0.04920 = 0.03209 -0.00550 0.02321 0.00146 AFIX 43 H53 2 0.672616 0.532934 0.032479 11.00000 -1.20000 AFIX 0 C21 1 0.500806 0.690173 0.047448 11.00000 0.05692 0.05633 = 0.03125 -0.00254 0.01500 -0.01004 AFIX 137 H21A 2 0.448275 0.682725 0.038163 11.00000 -1.50000 H21B 2 0.522903 0.640100 0.042471 11.00000 -1.50000 H21C 2 0.508616 0.729742 0.020876 11.00000 -1.50000 AFIX 0 C10 1 0.481735 0.695283 0.443789 11.00000 0.05909 0.05762 = 0.03959 -0.00403 0.02591 -0.00756 AFIX 137 H10A 2 0.449514 0.684443 0.465885 11.00000 -1.50000 H10B 2 0.509840 0.743358 0.459054 11.00000 -1.50000 H10C 2 0.515290 0.650888 0.448190 11.00000 -1.50000 AFIX 0 C12 1 0.444572 0.393896 0.251017 11.00000 0.04791 0.04234 = 0.04702 0.00116 0.01463 0.00779 AFIX 137 H12A 2 0.494301 0.410680 0.274513 11.00000 -1.50000 H12B 2 0.445465 0.363112 0.217130 11.00000 -1.50000 H12C 2 0.424990 0.361377 0.275320 11.00000 -1.50000 AFIX 0 C16 1 0.485775 0.858961 0.092441 11.00000 0.06159 0.04864 = 0.03664 0.01646 0.01693 0.00156 AFIX 43 H16 2 0.502146 0.859350 0.060036 11.00000 -1.20000 AFIX 0 PART 1 C63 1 0.676074 0.808319 0.396977 11.00000 0.05882 0.04029 = 0.03423 -0.01019 -0.00009 -0.00811 AFIX 43 H63 2 0.693032 0.847579 0.426590 11.00000 -1.20000 AFIX 0 PART 0 C30 1 0.231929 0.604438 0.057881 11.00000 0.03853 0.04800 = 0.04894 0.00160 -0.00586 -0.01192 AFIX 137 H30A 2 0.231850 0.554468 0.078115 11.00000 -1.50000 H30B 2 0.236534 0.593859 0.019680 11.00000 -1.50000 H30C 2 0.186138 0.632624 0.051790 11.00000 -1.50000 AFIX 0 C22 1 0.618180 0.740679 0.123815 11.00000 0.04404 0.06196 = 0.04267 -0.00836 0.01895 -0.00727 AFIX 137 H22A 2 0.619774 0.784868 0.098302 11.00000 -1.50000 H22B 2 0.643059 0.695027 0.114814 11.00000 -1.50000 H22C 2 0.642686 0.755781 0.165125 11.00000 -1.50000 AFIX 0 C61 1 0.478994 0.432431 0.099691 11.00000 0.03669 0.06966 = 0.04667 -0.01388 0.01139 -0.00559 AFIX 137 H61A 2 0.470272 0.489427 0.096512 11.00000 -1.50000 H61B 2 0.441336 0.406744 0.111281 11.00000 -1.50000 H61C 2 0.477174 0.411662 0.061538 11.00000 -1.50000 AFIX 0 C34 1 0.168882 0.759654 0.118080 11.00000 0.02942 0.05056 = 0.08646 0.00977 0.00302 0.00886 AFIX 137 H34A 2 0.194018 0.809607 0.118063 11.00000 -1.50000 H34B 2 0.124138 0.769820 0.126250 11.00000 -1.50000 H34C 2 0.156385 0.734332 0.079474 11.00000 -1.50000 AFIX 0 C42 1 0.775636 0.575042 0.484860 11.00000 0.07674 0.04951 = 0.03252 -0.00747 0.01412 -0.01147 AFIX 43 H42 2 0.816251 0.608071 0.504149 11.00000 -1.20000 AFIX 0 C44 1 0.587932 0.422525 0.398027 11.00000 0.05491 0.12794 = 0.03392 -0.00075 0.01240 -0.03149 AFIX 13 H44 2 0.572127 0.432264 0.354658 11.00000 -1.20000 AFIX 0 C33 1 0.179782 0.623652 0.169076 11.00000 0.02993 0.05002 = 0.08424 0.00169 0.01919 -0.00850 AFIX 137 H33A 2 0.165810 0.597376 0.130713 11.00000 -1.50000 H33B 2 0.135915 0.634775 0.178298 11.00000 -1.50000 H33C 2 0.212483 0.589266 0.199510 11.00000 -1.50000 AFIX 0 C17 1 0.451742 0.926104 0.103921 11.00000 0.07431 0.04153 = 0.05343 0.02617 0.01722 0.00653 AFIX 43 H17 2 0.443518 0.970500 0.078580 11.00000 -1.20000 AFIX 0 C24 1 0.360829 0.929502 0.243696 11.00000 0.07265 0.04208 = 0.12863 0.02476 0.06805 0.02463 AFIX 137 H24A 2 0.377481 0.982813 0.239275 11.00000 -1.50000 H24B 2 0.348762 0.926898 0.279513 11.00000 -1.50000 H24C 2 0.317383 0.916729 0.209432 11.00000 -1.50000 AFIX 0 C58 1 0.815357 0.658399 0.224608 11.00000 0.04123 0.04755 = 0.09013 -0.02601 0.01912 -0.00638 AFIX 137 H58A 2 0.832723 0.664786 0.191671 11.00000 -1.50000 H58B 2 0.852586 0.677869 0.260880 11.00000 -1.50000 H58C 2 0.770132 0.688464 0.216673 11.00000 -1.50000 AFIX 0 C47 1 0.819749 0.569803 0.396864 11.00000 0.07230 0.10819 = 0.03472 -0.02072 0.01806 -0.04934 AFIX 13 H47 2 0.797221 0.555752 0.354187 11.00000 -1.20000 AFIX 0 C25 1 0.494199 0.887766 0.301331 11.00000 0.05162 0.06342 = 0.05689 -0.01869 0.02547 -0.01299 AFIX 137 H25A 2 0.531638 0.848669 0.302769 11.00000 -1.50000 H25B 2 0.484188 0.885774 0.338082 11.00000 -1.50000 H25C 2 0.511651 0.940514 0.296428 11.00000 -1.50000 AFIX 0 C57 1 0.871435 0.521030 0.241557 11.00000 0.05905 0.04973 = 0.10066 -0.01158 -0.01963 0.00479 AFIX 137 H57A 2 0.862340 0.465307 0.247119 11.00000 -1.50000 H57B 2 0.910673 0.540680 0.276566 11.00000 -1.50000 H57C 2 0.885893 0.526636 0.207041 11.00000 -1.50000 AFIX 0 C60 1 0.572918 0.326097 0.147868 11.00000 0.05950 0.04757 = 0.09093 0.01344 0.00739 -0.00919 AFIX 137 H60A 2 0.573920 0.310195 0.109367 11.00000 -1.50000 H60B 2 0.535155 0.296066 0.156500 11.00000 -1.50000 H60C 2 0.620607 0.315586 0.178322 11.00000 -1.50000 AFIX 0 C45 1 0.520815 0.438274 0.416003 11.00000 0.04849 0.13573 = 0.06889 0.05237 0.01541 -0.00042 AFIX 137 H45A 2 0.532703 0.424337 0.457531 11.00000 -1.50000 H45B 2 0.479550 0.406230 0.391545 11.00000 -1.50000 H45C 2 0.507711 0.494224 0.410312 11.00000 -1.50000 AFIX 0 C46 1 0.608551 0.335279 0.408016 11.00000 0.10796 0.09785 = 0.15962 -0.05853 0.08689 -0.05777 AFIX 137 H46A 2 0.645055 0.322708 0.390290 11.00000 -1.50000 H46B 2 0.564945 0.302803 0.389757 11.00000 -1.50000 H46C 2 0.628856 0.324461 0.450396 11.00000 -1.50000 AFIX 0 C49 1 0.835403 0.661308 0.400963 11.00000 0.04992 0.10038 = 0.09405 0.03926 0.00949 -0.01616 AFIX 137 H49A 2 0.789137 0.690089 0.384908 11.00000 -1.50000 H49B 2 0.866428 0.674438 0.378268 11.00000 -1.50000 H49C 2 0.860364 0.676212 0.442258 11.00000 -1.50000 AFIX 0 C48 1 0.891538 0.521795 0.423231 11.00000 0.07899 0.10588 = 0.14221 -0.04474 0.07280 -0.01545 AFIX 137 H48A 2 0.915315 0.535158 0.464970 11.00000 -1.50000 H48B 2 0.924329 0.534604 0.402005 11.00000 -1.50000 H48C 2 0.880286 0.465317 0.419362 11.00000 -1.50000 AFIX 0 C74 1 0.478217 -0.000936 0.516954 11.00000 0.16170 0.44519 = 0.14731 0.04292 0.07638 -0.07743 C71 1 0.927678 0.336896 0.706475 11.00000 0.37651 0.05405 = 0.37423 -0.02210 0.26610 -0.00911 C72 1 0.580659 0.075127 0.418713 11.00000 0.35819 0.33450 = 0.24153 -0.12185 0.22603 -0.14262 PART 2 C73 1 0.542833 0.065807 0.456761 11.00000 0.17198 0.27761 = 0.17920 0.02059 0.10017 -0.02467 PART 0 C70 1 0.893908 0.339805 0.637971 11.00000 0.44380 0.07822 = 0.22874 -0.05308 -0.08412 0.00186 C68 1 0.881349 0.347455 0.544651 11.00000 0.50353 0.13238 = 0.41928 -0.00271 0.37162 -0.03028 C69 1 0.842178 0.314439 0.601562 11.00000 0.17375 0.56377 = 0.23775 -0.14218 0.00942 -0.03921 C66 1 0.773605 0.202585 0.513519 11.00000 0.44772 0.39508 = 0.17499 -0.10095 -0.02526 0.30838 C67 1 0.800873 0.290843 0.542534 11.00000 0.23063 0.31932 = 0.33326 -0.19837 -0.07189 0.12843 H65 2 0.589143 0.631868 0.392498 11.00000 0.05443 HKLF 4 REM at_bthio_2_0m_a.res in P2(1)/n REM R1 = 0.0673 for 10775 Fo > 4sig(Fo) and 0.0921 for all 14454 data REM 765 parameters refined using 0 restraints END WGHT 0.1038 8.6209 REM Highest difference peak 1.313, deepest hole -0.642, 1-sigma level 0.067 Q1 1 0.5770 0.8135 0.3477 11.00000 0.05 1.31 Q2 1 0.9498 0.3428 0.6774 11.00000 0.05 0.58 Q3 1 0.8363 0.2743 0.6182 11.00000 0.05 0.58 Q4 1 0.7741 0.2618 0.5481 11.00000 0.05 0.57 Q5 1 0.9626 0.3300 0.7420 11.00000 0.05 0.54 Q6 1 0.6198 0.8011 0.3049 11.00000 0.05 0.54 Q7 1 0.6829 0.7015 0.3682 11.00000 0.05 0.54 Q8 1 0.8202 0.3546 0.5852 11.00000 0.05 0.52 Q9 1 0.9453 0.3597 0.6190 11.00000 0.05 0.50 Q10 1 0.4632 0.9586 0.2818 11.00000 0.05 0.48 Q11 1 0.8943 0.3251 0.6971 11.00000 0.05 0.48 Q12 1 0.8280 0.3213 0.5140 11.00000 0.05 0.48 Q13 1 0.9162 0.3353 0.5585 11.00000 0.05 0.47 Q14 1 0.6866 0.7549 0.3268 11.00000 0.05 0.47 Q15 1 0.8709 0.3650 0.5856 11.00000 0.05 0.46 Q16 1 0.5039 -0.0164 0.5407 11.00000 0.05 0.45 Q17 1 0.5844 0.6844 0.3219 11.00000 0.05 0.44 Q18 1 0.6258 0.0956 0.4646 11.00000 0.05 0.43 Q19 1 0.8605 0.3753 0.5178 11.00000 0.05 0.42 Q20 1 0.8373 0.3618 0.6510 11.00000 0.05 0.41 ; _shelx_res_checksum 85854 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.57060(2) 0.66056(3) 0.28461(2) 0.02240(13) Uani 1 1 d . . . S1 S 0.65801(4) 0.76251(5) 0.28120(3) 0.03730(19) Uani 1 1 d . . . N2 N 0.45866(12) 0.62866(13) 0.27187(10) 0.0259(5) Uani 1 1 d . . . N1 N 0.48269(12) 0.72148(13) 0.21432(9) 0.0241(4) Uani 1 1 d . . . N4 N 0.61686(12) 0.56944(13) 0.27506(9) 0.0258(5) Uani 1 1 d . . . N6 N 0.68546(13) 0.46651(13) 0.24617(10) 0.0296(5) Uani 1 1 d . . . N5 N 0.69258(13) 0.46703(14) 0.34037(10) 0.0301(5) Uani 1 1 d . . . N3 N 0.35334(12) 0.69477(13) 0.20551(11) 0.0303(5) Uani 1 1 d . . . C1 C 0.42913(14) 0.68142(15) 0.22669(12) 0.0254(5) Uani 1 1 d . . . C35 C 0.66116(14) 0.50788(15) 0.28620(11) 0.0256(5) Uani 1 1 d . . . C14 C 0.47108(14) 0.79056(16) 0.17679(12) 0.0270(6) Uani 1 1 d . . . C2 C 0.41253(15) 0.58965(16) 0.30013(13) 0.0295(6) Uani 1 1 d . . . C38 C 0.70237(17) 0.49851(17) 0.39955(12) 0.0323(6) Uani 1 1 d . . . C7 C 0.38171(16) 0.51336(17) 0.27981(13) 0.0327(6) Uani 1 1 d . . . C50 C 0.67814(16) 0.49187(16) 0.18595(12) 0.0303(6) Uani 1 1 d . . . C15 C 0.49667(16) 0.78973(17) 0.12802(12) 0.0328(6) Uani 1 1 d . . . C19 C 0.43980(15) 0.86148(17) 0.19104(13) 0.0318(6) Uani 1 1 d . . . C20 C 0.53713(17) 0.71900(19) 0.11301(13) 0.0360(7) Uani 1 1 d . . . H20 H 0.536659 0.674163 0.139641 0.043 Uiso 1 1 calc R . . C51 C 0.73571(18) 0.53721(18) 0.17876(14) 0.0367(7) Uani 1 1 d . . . C3 C 0.39925(17) 0.62745(18) 0.34866(13) 0.0347(6) Uani 1 1 d . . . C37 C 0.72981(18) 0.40180(18) 0.27535(13) 0.0383(7) Uani 1 1 d . . . H37 H 0.752408 0.364805 0.257941 0.046 Uiso 1 1 calc R . . C11 C 0.39515(17) 0.46797(17) 0.22886(13) 0.0351(6) Uani 1 1 d . . . H11 H 0.420338 0.504477 0.209882 0.042 Uiso 1 1 calc R . . C39 C 0.65348(18) 0.4772(2) 0.42798(14) 0.0415(7) Uani 1 1 d . . . C55 C 0.61716(17) 0.46436(18) 0.13750(13) 0.0351(6) Uani 1 1 d . . . C8 C 0.43453(18) 0.70676(18) 0.37683(14) 0.0375(7) Uani 1 1 d . . . H8 H 0.467661 0.724881 0.356097 0.045 Uiso 1 1 calc R . . C65 C 0.60688(17) 0.67976(19) 0.37516(13) 0.0351(6) Uani 1 1 d . . . C64 C 0.64071(18) 0.7374(2) 0.41133(13) 0.0418(7) Uani 1 1 d . A 1 H64 H 0.642658 0.733046 0.450838 0.050 Uiso 1 1 calc R A 1 C36 C 0.73421(18) 0.40213(18) 0.33233(14) 0.0386(7) Uani 1 1 d . . . H36 H 0.760493 0.365465 0.361758 0.046 Uiso 1 1 calc R . . C26 C 0.29588(15) 0.68384(17) 0.15824(14) 0.0346(7) Uani 1 1 d . . . C40 C 0.6682(2) 0.5069(2) 0.48627(14) 0.0508(9) Uani 1 1 d . . . H40 H 0.636199 0.493768 0.506470 0.061 Uiso 1 1 calc R . . C13 C 0.32113(18) 0.4419(2) 0.18095(15) 0.0432(7) Uani 1 1 d . . . H13A H 0.298805 0.400369 0.197001 0.065 Uiso 1 1 calc GR . . H13B H 0.330223 0.421775 0.146349 0.065 Uiso 1 1 calc GR . . H13C H 0.288047 0.487231 0.169507 0.065 Uiso 1 1 calc GR . . C23 C 0.42263(16) 0.86917(18) 0.24825(15) 0.0371(7) Uani 1 1 d . . . H23 H 0.405146 0.816374 0.256020 0.044 Uiso 1 1 calc R . . C27 C 0.29852(17) 0.65667(18) 0.09671(14) 0.0389(7) Uani 1 1 d . . . C6 C 0.33620(18) 0.47767(19) 0.30757(15) 0.0418(7) Uani 1 1 d . . . H6 H 0.315641 0.427289 0.294634 0.050 Uiso 1 1 calc R . . C59 C 0.55557(19) 0.4157(2) 0.14694(14) 0.0432(7) Uani 1 1 d . . . H59 H 0.553688 0.430109 0.186321 0.052 Uiso 1 1 calc R . . C43 C 0.7645(2) 0.5475(2) 0.42684(13) 0.0432(8) Uani 1 1 d . . . C4 C 0.35262(19) 0.5888(2) 0.37408(15) 0.0447(8) Uani 1 1 d . . . H4 H 0.342831 0.613591 0.405550 0.054 Uiso 1 1 calc R . . C54 C 0.6162(2) 0.4808(2) 0.07962(14) 0.0434(8) Uani 1 1 d . . . H54 H 0.576538 0.462998 0.046403 0.052 Uiso 1 1 calc R . . C5 C 0.3210(2) 0.5154(2) 0.35370(16) 0.0475(8) Uani 1 1 d . . . H5 H 0.289647 0.491215 0.370830 0.057 Uiso 1 1 calc R . . C28 C 0.36820(17) 0.60754(19) 0.10332(13) 0.0381(7) Uani 1 1 d . . . H28A H 0.411779 0.638773 0.124363 0.057 Uiso 1 1 calc GR . . H28B H 0.368379 0.593624 0.064209 0.057 Uiso 1 1 calc GR . . H28C H 0.368282 0.559304 0.125565 0.057 Uiso 1 1 calc GR . . C29 C 0.30042(19) 0.7348(2) 0.06129(14) 0.0453(8) Uani 1 1 d . . . H29A H 0.253664 0.762455 0.051370 0.068 Uiso 1 1 calc GR . . H29B H 0.308841 0.721092 0.025009 0.068 Uiso 1 1 calc GR . . H29C H 0.339945 0.769004 0.085616 0.068 Uiso 1 1 calc GR . . C18 C 0.42973(19) 0.92787(19) 0.15292(16) 0.0466(8) Uani 1 1 d . . . H18 H 0.407676 0.974219 0.160880 0.056 Uiso 1 1 calc R . . C32 C 0.23529(18) 0.7443(2) 0.22734(18) 0.0494(9) Uani 1 1 d . . . H32A H 0.263305 0.708660 0.259050 0.074 Uiso 1 1 calc GR . . H32B H 0.188729 0.757153 0.231803 0.074 Uiso 1 1 calc GR . . H32C H 0.263213 0.792883 0.229323 0.074 Uiso 1 1 calc GR . . C31 C 0.22044(16) 0.70377(19) 0.16698(17) 0.0444(8) Uani 1 1 d . . . C56 C 0.8005(2) 0.5695(2) 0.23192(15) 0.0478(8) Uani 1 1 d . . . H56 H 0.787489 0.563882 0.268029 0.057 Uiso 1 1 calc R . . C62 C 0.68633(18) 0.82195(19) 0.34461(14) 0.0422(7) Uani 1 1 d . A 1 H62 H 0.711639 0.868921 0.342470 0.051 Uiso 1 1 calc R A 1 C52 C 0.7320(2) 0.5514(2) 0.11983(15) 0.0457(8) Uani 1 1 d . . . H52 H 0.769850 0.580559 0.113343 0.055 Uiso 1 1 calc R . . C41 C 0.7284(2) 0.5547(2) 0.51389(14) 0.0527(9) Uani 1 1 d . . . H41 H 0.737259 0.573444 0.552648 0.063 Uiso 1 1 calc R . . C9 C 0.3770(2) 0.7729(2) 0.37108(17) 0.0484(8) Uani 1 1 d . . . H9A H 0.350378 0.784128 0.329329 0.073 Uiso 1 1 calc GR . . H9B H 0.401922 0.820832 0.390733 0.073 Uiso 1 1 calc GR . . H9C H 0.342542 0.755417 0.389579 0.073 Uiso 1 1 calc GR . . C53 C 0.6735(2) 0.5233(2) 0.07124(14) 0.0470(8) Uani 1 1 d . . . H53 H 0.672616 0.532934 0.032479 0.056 Uiso 1 1 calc R . . C21 C 0.5008(2) 0.6902(2) 0.04745(14) 0.0483(8) Uani 1 1 d . . . H21A H 0.448275 0.682725 0.038163 0.073 Uiso 1 1 calc GR . . H21B H 0.522903 0.640100 0.042471 0.073 Uiso 1 1 calc GR . . H21C H 0.508616 0.729742 0.020876 0.073 Uiso 1 1 calc GR . . C10 C 0.4817(2) 0.6953(2) 0.44379(15) 0.0498(8) Uani 1 1 d . . . H10A H 0.449514 0.684443 0.465885 0.075 Uiso 1 1 calc GR . . H10B H 0.509840 0.743358 0.459054 0.075 Uiso 1 1 calc GR . . H10C H 0.515290 0.650888 0.448190 0.075 Uiso 1 1 calc GR . . C12 C 0.4446(2) 0.3939(2) 0.25102(16) 0.0464(8) Uani 1 1 d . . . H12A H 0.494301 0.410680 0.274513 0.070 Uiso 1 1 calc GR . . H12B H 0.445465 0.363112 0.217130 0.070 Uiso 1 1 calc GR . . H12C H 0.424990 0.361377 0.275320 0.070 Uiso 1 1 calc GR . . C16 C 0.4858(2) 0.8590(2) 0.09244(15) 0.0491(8) Uani 1 1 d . . . H16 H 0.502146 0.859350 0.060036 0.059 Uiso 1 1 calc R . . C63 C 0.6761(2) 0.8083(2) 0.39698(15) 0.0489(9) Uani 1 1 d . A 1 H63 H 0.693032 0.847579 0.426590 0.059 Uiso 1 1 calc R A 1 C30 C 0.23193(19) 0.6044(2) 0.05788(16) 0.0510(9) Uani 1 1 d . . . H30A H 0.231850 0.554468 0.078115 0.076 Uiso 1 1 calc GR . . H30B H 0.236534 0.593859 0.019680 0.076 Uiso 1 1 calc GR . . H30C H 0.186138 0.632624 0.051790 0.076 Uiso 1 1 calc GR . . C22 C 0.61818(19) 0.7407(2) 0.12382(15) 0.0486(8) Uani 1 1 d . . . H22A H 0.619774 0.784868 0.098302 0.073 Uiso 1 1 calc GR . . H22B H 0.643059 0.695027 0.114814 0.073 Uiso 1 1 calc GR . . H22C H 0.642686 0.755781 0.165125 0.073 Uiso 1 1 calc GR . . C61 C 0.47899(19) 0.4324(2) 0.09969(16) 0.0519(9) Uani 1 1 d . . . H61A H 0.470272 0.489427 0.096512 0.078 Uiso 1 1 calc GR . . H61B H 0.441336 0.406744 0.111281 0.078 Uiso 1 1 calc GR . . H61C H 0.477174 0.411662 0.061538 0.078 Uiso 1 1 calc GR . . C34 C 0.16888(19) 0.7597(2) 0.1181(2) 0.0602(10) Uani 1 1 d . . . H34A H 0.194018 0.809607 0.118063 0.090 Uiso 1 1 calc GR . . H34B H 0.124138 0.769820 0.126250 0.090 Uiso 1 1 calc GR . . H34C H 0.156385 0.734332 0.079474 0.090 Uiso 1 1 calc GR . . C42 C 0.7756(2) 0.5750(2) 0.48486(15) 0.0544(9) Uani 1 1 d . . . H42 H 0.816251 0.608071 0.504149 0.065 Uiso 1 1 calc R . . C44 C 0.5879(2) 0.4225(3) 0.39803(17) 0.0732(14) Uani 1 1 d . . . H44 H 0.572127 0.432264 0.354658 0.088 Uiso 1 1 calc R . . C33 C 0.17978(19) 0.6237(2) 0.1691(2) 0.0550(9) Uani 1 1 d . . . H33A H 0.165810 0.597376 0.130713 0.083 Uiso 1 1 calc GR . . H33B H 0.135915 0.634775 0.178298 0.083 Uiso 1 1 calc GR . . H33C H 0.212483 0.589266 0.199510 0.083 Uiso 1 1 calc GR . . C17 C 0.4517(2) 0.9261(2) 0.10392(17) 0.0579(10) Uani 1 1 d . . . H17 H 0.443518 0.970500 0.078580 0.069 Uiso 1 1 calc R . . C24 C 0.3608(3) 0.9295(2) 0.2437(2) 0.0724(14) Uani 1 1 d . . . H24A H 0.377481 0.982813 0.239275 0.109 Uiso 1 1 calc GR . . H24B H 0.348762 0.926898 0.279513 0.109 Uiso 1 1 calc GR . . H24C H 0.317383 0.916729 0.209432 0.109 Uiso 1 1 calc GR . . C58 C 0.8154(2) 0.6584(2) 0.2246(2) 0.0608(11) Uani 1 1 d . . . H58A H 0.832723 0.664786 0.191671 0.091 Uiso 1 1 calc GR . . H58B H 0.852586 0.677869 0.260880 0.091 Uiso 1 1 calc GR . . H58C H 0.770132 0.688464 0.216673 0.091 Uiso 1 1 calc GR . . C47 C 0.8197(3) 0.5698(3) 0.39686(17) 0.0720(14) Uani 1 1 d . . . H47 H 0.797221 0.555752 0.354187 0.086 Uiso 1 1 calc R . . C25 C 0.4942(2) 0.8878(2) 0.30133(17) 0.0556(9) Uani 1 1 d . . . H25A H 0.531638 0.848669 0.302769 0.083 Uiso 1 1 calc GR . . H25B H 0.484188 0.885774 0.338082 0.083 Uiso 1 1 calc GR . . H25C H 0.511651 0.940514 0.296428 0.083 Uiso 1 1 calc GR . . C57 C 0.8714(2) 0.5210(3) 0.2416(2) 0.0828(16) Uani 1 1 d . . . H57A H 0.862340 0.465307 0.247119 0.124 Uiso 1 1 calc GR . . H57B H 0.910673 0.540680 0.276566 0.124 Uiso 1 1 calc GR . . H57C H 0.885893 0.526636 0.207041 0.124 Uiso 1 1 calc GR . . C60 C 0.5729(2) 0.3261(2) 0.1479(2) 0.0712(13) Uani 1 1 d . . . H60A H 0.573920 0.310195 0.109367 0.107 Uiso 1 1 calc GR . . H60B H 0.535155 0.296066 0.156500 0.107 Uiso 1 1 calc GR . . H60C H 0.620607 0.315586 0.178322 0.107 Uiso 1 1 calc GR . . C45 C 0.5208(2) 0.4383(4) 0.4160(2) 0.0858(17) Uani 1 1 d . . . H45A H 0.532703 0.424337 0.457531 0.129 Uiso 1 1 calc GR . . H45B H 0.479550 0.406230 0.391545 0.129 Uiso 1 1 calc GR . . H45C H 0.507711 0.494224 0.410312 0.129 Uiso 1 1 calc GR . . C46 C 0.6086(4) 0.3353(4) 0.4080(3) 0.111(2) Uani 1 1 d . . . H46A H 0.645055 0.322708 0.390290 0.167 Uiso 1 1 calc GR . . H46B H 0.564945 0.302803 0.389757 0.167 Uiso 1 1 calc GR . . H46C H 0.628856 0.324461 0.450396 0.167 Uiso 1 1 calc GR . . C49 C 0.8354(3) 0.6613(3) 0.4010(2) 0.0858(16) Uani 1 1 d . . . H49A H 0.789137 0.690089 0.384908 0.129 Uiso 1 1 calc GR . . H49B H 0.866428 0.674438 0.378268 0.129 Uiso 1 1 calc GR . . H49C H 0.860364 0.676212 0.442258 0.129 Uiso 1 1 calc GR . . C48 C 0.8915(3) 0.5218(4) 0.4232(3) 0.0999(19) Uani 1 1 d . . . H48A H 0.915315 0.535158 0.464970 0.150 Uiso 1 1 calc GR . . H48B H 0.924329 0.534604 0.402005 0.150 Uiso 1 1 calc GR . . H48C H 0.880286 0.465317 0.419362 0.150 Uiso 1 1 calc GR . . C74 C 0.4782(7) -0.0009(12) 0.5170(5) 0.246(7) Uani 1 1 d . . . C71 C 0.9277(10) 0.3369(5) 0.7065(8) 0.232(8) Uani 1 1 d . . . C72 C 0.5807(10) 0.0751(10) 0.4187(6) 0.279(9) Uani 1 1 d . . . C73 C 0.5428(7) 0.0658(9) 0.4568(5) 0.199(5) Uani 1 1 d . B 2 C70 C 0.8939(12) 0.3398(6) 0.6380(8) 0.305(13) Uani 1 1 d . . . C68 C 0.8813(14) 0.3475(7) 0.5447(11) 0.295(11) Uani 1 1 d . . . C69 C 0.8422(9) 0.3144(17) 0.6016(9) 0.342(13) Uani 1 1 d . . . C66 C 0.7736(11) 0.2026(12) 0.5135(6) 0.376(15) Uani 1 1 d . . . C67 C 0.8009(9) 0.2908(12) 0.5425(10) 0.341(14) Uani 1 1 d . . . H65 H 0.589(2) 0.632(2) 0.3925(16) 0.054(10) 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 Ti1 0.0197(2) 0.0230(2) 0.0236(2) 0.00297(17) 0.00657(18) 0.00111(17) S1 0.0369(4) 0.0377(4) 0.0354(4) -0.0021(3) 0.0106(3) -0.0122(3) N2 0.0223(11) 0.0258(11) 0.0301(11) 0.0046(9) 0.0099(9) -0.0008(9) N1 0.0198(10) 0.0243(10) 0.0259(11) 0.0041(8) 0.0053(9) -0.0005(8) N4 0.0235(11) 0.0274(11) 0.0251(11) -0.0008(9) 0.0068(9) -0.0004(9) N6 0.0337(13) 0.0263(11) 0.0280(11) -0.0033(9) 0.0100(10) 0.0051(9) N5 0.0329(12) 0.0274(11) 0.0261(11) 0.0010(9) 0.0055(10) 0.0084(10) N3 0.0209(11) 0.0259(11) 0.0407(13) 0.0059(10) 0.0069(10) -0.0015(9) C1 0.0223(13) 0.0235(12) 0.0295(13) -0.0001(10) 0.0082(11) -0.0004(10) C35 0.0247(13) 0.0235(12) 0.0265(13) -0.0024(10) 0.0066(10) 0.0003(10) C14 0.0191(12) 0.0265(13) 0.0288(13) 0.0058(10) 0.0005(10) -0.0020(10) C2 0.0223(13) 0.0309(14) 0.0360(14) 0.0076(11) 0.0113(11) 0.0000(11) C38 0.0388(16) 0.0305(14) 0.0249(13) 0.0024(11) 0.0079(12) 0.0104(12) C7 0.0282(14) 0.0304(14) 0.0396(15) 0.0068(12) 0.0122(12) -0.0022(11) C50 0.0366(15) 0.0281(13) 0.0264(13) -0.0037(11) 0.0116(12) 0.0072(11) C15 0.0307(15) 0.0340(15) 0.0301(14) 0.0062(11) 0.0066(12) -0.0024(12) C19 0.0207(13) 0.0274(13) 0.0421(16) 0.0054(12) 0.0047(12) 0.0009(10) C20 0.0389(16) 0.0410(16) 0.0282(14) 0.0007(12) 0.0121(12) -0.0032(13) C51 0.0419(17) 0.0326(15) 0.0380(16) -0.0066(12) 0.0174(14) 0.0005(13) C3 0.0314(15) 0.0359(15) 0.0389(16) 0.0056(12) 0.0152(13) 0.0002(12) C37 0.0461(18) 0.0297(14) 0.0368(16) -0.0018(12) 0.0117(14) 0.0147(13) C11 0.0334(15) 0.0301(14) 0.0419(16) 0.0018(12) 0.0135(13) -0.0077(12) C39 0.0406(17) 0.0509(19) 0.0313(15) 0.0116(13) 0.0106(13) 0.0094(14) C55 0.0387(16) 0.0343(15) 0.0319(15) -0.0081(12) 0.0120(13) 0.0029(12) C8 0.0412(17) 0.0388(16) 0.0400(16) -0.0021(13) 0.0237(14) -0.0054(13) C65 0.0348(16) 0.0394(16) 0.0334(15) 0.0067(13) 0.0151(13) 0.0074(13) C64 0.0439(18) 0.0543(19) 0.0249(14) 0.0059(13) 0.0095(13) 0.0107(15) C36 0.0439(17) 0.0304(15) 0.0374(16) 0.0026(12) 0.0096(14) 0.0167(13) C26 0.0234(14) 0.0251(13) 0.0478(17) 0.0069(12) 0.0034(12) -0.0027(11) C40 0.059(2) 0.066(2) 0.0317(16) 0.0128(16) 0.0210(16) 0.0171(19) C13 0.0382(17) 0.0409(17) 0.0477(18) -0.0004(14) 0.0120(14) -0.0072(14) C23 0.0281(15) 0.0295(14) 0.0563(19) -0.0021(13) 0.0184(14) -0.0022(12) C27 0.0285(15) 0.0363(15) 0.0394(16) 0.0051(13) -0.0036(13) -0.0055(12) C6 0.0388(17) 0.0371(16) 0.0518(19) 0.0058(14) 0.0189(15) -0.0119(13) C59 0.0430(18) 0.0526(19) 0.0316(15) -0.0065(14) 0.0102(14) -0.0073(15) C43 0.052(2) 0.0449(18) 0.0292(15) -0.0040(13) 0.0105(14) -0.0057(15) C4 0.0457(19) 0.0484(19) 0.0481(18) 0.0020(15) 0.0267(16) -0.0051(15) C54 0.0487(19) 0.0526(19) 0.0283(15) -0.0077(13) 0.0129(14) 0.0012(15) C5 0.0465(19) 0.0502(19) 0.056(2) 0.0062(16) 0.0314(17) -0.0119(16) C28 0.0366(16) 0.0379(16) 0.0330(15) 0.0017(12) 0.0041(13) -0.0038(13) C29 0.0391(17) 0.0427(17) 0.0383(17) 0.0104(14) -0.0058(14) -0.0044(14) C18 0.0461(19) 0.0317(16) 0.055(2) 0.0132(14) 0.0099(16) 0.0098(14) C32 0.0281(16) 0.0430(18) 0.079(3) -0.0004(17) 0.0219(16) 0.0047(14) C31 0.0213(14) 0.0382(17) 0.068(2) 0.0045(15) 0.0084(14) 0.0010(12) C56 0.048(2) 0.053(2) 0.0428(18) -0.0138(15) 0.0175(15) -0.0152(16) C62 0.0406(17) 0.0331(15) 0.0421(17) -0.0012(13) 0.0014(14) -0.0077(13) C52 0.057(2) 0.0437(18) 0.0437(18) -0.0064(14) 0.0267(16) -0.0065(16) C41 0.085(3) 0.0457(19) 0.0269(15) -0.0006(14) 0.0190(17) 0.0054(19) C9 0.052(2) 0.0427(18) 0.063(2) -0.0065(16) 0.0352(18) -0.0001(15) C53 0.065(2) 0.0492(19) 0.0321(16) -0.0055(14) 0.0232(16) 0.0015(17) C21 0.057(2) 0.056(2) 0.0313(16) -0.0025(15) 0.0150(15) -0.0100(17) C10 0.059(2) 0.058(2) 0.0396(18) -0.0040(15) 0.0259(16) -0.0076(17) C12 0.0479(19) 0.0423(18) 0.0470(19) 0.0012(15) 0.0146(16) 0.0078(15) C16 0.062(2) 0.0486(19) 0.0366(17) 0.0165(15) 0.0169(16) 0.0016(17) C63 0.059(2) 0.0403(17) 0.0342(16) -0.0102(14) -0.0001(15) -0.0081(16) C30 0.0385(18) 0.0480(19) 0.0489(19) 0.0016(15) -0.0059(15) -0.0119(15) C22 0.0440(19) 0.062(2) 0.0427(18) -0.0084(16) 0.0189(15) -0.0073(16) C61 0.0367(18) 0.070(2) 0.0467(19) -0.0139(17) 0.0114(15) -0.0056(17) C34 0.0294(17) 0.051(2) 0.086(3) 0.010(2) 0.0030(18) 0.0089(15) C42 0.077(3) 0.050(2) 0.0325(17) -0.0075(15) 0.0141(17) -0.0115(19) C44 0.055(2) 0.128(4) 0.0339(18) -0.001(2) 0.0124(17) -0.031(3) C33 0.0299(17) 0.050(2) 0.084(3) 0.0017(19) 0.0192(18) -0.0085(15) C17 0.074(3) 0.0415(19) 0.053(2) 0.0262(17) 0.0172(19) 0.0065(18) C24 0.073(3) 0.042(2) 0.129(4) 0.025(2) 0.068(3) 0.0246(19) C58 0.041(2) 0.048(2) 0.090(3) -0.026(2) 0.019(2) -0.0064(16) C47 0.072(3) 0.108(4) 0.0347(18) -0.021(2) 0.0181(19) -0.049(3) C25 0.052(2) 0.063(2) 0.057(2) -0.0187(18) 0.0255(18) -0.0130(18) C57 0.059(3) 0.050(2) 0.101(4) -0.012(2) -0.020(2) 0.005(2) C60 0.060(3) 0.048(2) 0.091(3) 0.013(2) 0.007(2) -0.0092(19) C45 0.048(2) 0.136(5) 0.069(3) 0.052(3) 0.015(2) 0.000(3) C46 0.108(5) 0.098(4) 0.160(6) -0.059(4) 0.087(5) -0.058(4) C49 0.050(2) 0.100(4) 0.094(4) 0.039(3) 0.009(2) -0.016(2) C48 0.079(4) 0.106(4) 0.142(5) -0.045(4) 0.073(4) -0.015(3) C74 0.162(10) 0.45(2) 0.147(9) 0.043(12) 0.076(7) -0.077(12) C71 0.38(2) 0.054(4) 0.374(19) -0.022(8) 0.266(18) -0.009(7) C72 0.36(2) 0.335(19) 0.242(14) -0.122(13) 0.226(15) -0.143(16) C73 0.172(10) 0.278(15) 0.179(10) 0.021(10) 0.100(8) -0.025(10) C70 0.44(3) 0.078(6) 0.229(15) -0.053(8) -0.084(17) 0.002(9) C68 0.50(3) 0.132(9) 0.42(3) -0.003(12) 0.37(3) -0.030(13) C69 0.174(13) 0.56(4) 0.238(18) -0.14(2) 0.009(12) -0.039(18) C66 0.45(3) 0.40(2) 0.175(11) -0.101(13) -0.025(13) 0.31(2) C67 0.231(16) 0.32(2) 0.33(2) -0.20(2) -0.072(16) 0.128(16) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 '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 S1 Ti1 C1 119.90(6) . . N2 Ti1 S1 148.39(7) . . N2 Ti1 N1 62.29(8) . . N2 Ti1 C1 31.18(8) . . N1 Ti1 S1 90.33(6) . . N1 Ti1 C1 31.12(8) . . N4 Ti1 S1 101.90(8) . . N4 Ti1 N2 106.80(9) . . N4 Ti1 N1 125.30(9) . . N4 Ti1 C1 120.82(9) . . N4 Ti1 C65 105.36(11) . . C65 Ti1 S1 86.84(10) . . C65 Ti1 N2 97.94(11) . . C65 Ti1 N1 128.63(10) . . C65 Ti1 C1 116.12(11) . . C62 S1 Ti1 112.42(12) . . C1 N2 Ti1 93.94(16) . . C1 N2 C2 120.8(2) . . C2 N2 Ti1 143.29(17) . . C1 N1 Ti1 92.63(15) . . C1 N1 C14 125.2(2) . . C14 N1 Ti1 140.32(17) . . C35 N4 Ti1 161.82(19) . . C35 N6 C50 126.7(2) . . C35 N6 C37 109.6(2) . . C37 N6 C50 122.9(2) . . C35 N5 C38 126.0(2) . . C35 N5 C36 109.3(2) . . C36 N5 C38 121.9(2) . . C26 N3 C1 140.2(3) . . N2 C1 Ti1 54.88(13) . . N2 C1 N3 119.2(2) . . N1 C1 Ti1 56.26(13) . . N1 C1 N2 111.1(2) . . N1 C1 N3 129.1(2) . . N3 C1 Ti1 170.2(2) . . N4 C35 N6 127.5(2) . . N4 C35 N5 127.7(2) . . N6 C35 N5 104.7(2) . . C15 C14 N1 119.0(2) . . C15 C14 C19 120.4(2) . . C19 C14 N1 120.4(2) . . C7 C2 N2 119.8(2) . . C7 C2 C3 120.3(3) . . C3 C2 N2 120.0(2) . . C39 C38 N5 120.4(3) . . C39 C38 C43 122.4(3) . . C43 C38 N5 117.1(3) . . C2 C7 C11 123.3(2) . . C6 C7 C2 118.4(3) . . C6 C7 C11 118.4(3) . . C51 C50 N6 118.3(3) . . C55 C50 N6 118.6(3) . . C55 C50 C51 122.9(3) . . C14 C15 C20 123.8(2) . . C16 C15 C14 117.9(3) . . C16 C15 C20 118.2(3) . . C14 C19 C23 122.1(2) . . C18 C19 C14 118.3(3) . . C18 C19 C23 119.5(3) . . C15 C20 C21 113.1(3) . . C15 C20 C22 110.7(3) . . C22 C20 C21 108.1(3) . . C50 C51 C56 122.4(3) . . C50 C51 C52 116.9(3) . . C52 C51 C56 120.6(3) . . C2 C3 C8 124.2(3) . . C4 C3 C2 118.5(3) . . C4 C3 C8 117.3(3) . . C36 C37 N6 108.2(2) . . C7 C11 C13 110.9(3) . . C7 C11 C12 112.5(3) . . C12 C11 C13 109.0(3) . . C38 C39 C40 117.4(3) . . C38 C39 C44 121.3(3) . . C40 C39 C44 121.3(3) . . C50 C55 C59 121.5(3) . . C50 C55 C54 117.6(3) . . C54 C55 C59 120.9(3) . . C3 C8 C9 112.9(3) . . C3 C8 C10 110.7(3) . . C9 C8 C10 108.8(3) . . C64 C65 Ti1 136.0(2) . . C65 C64 C63 127.3(3) . . C37 C36 N5 108.1(3) . . N3 C26 C27 124.4(3) . . N3 C26 C31 113.7(3) . . C27 C26 C31 121.9(2) . . C41 C40 C39 121.4(3) . . C19 C23 C24 113.7(3) . . C19 C23 C25 109.9(3) . . C24 C23 C25 111.9(3) . . C26 C27 C29 106.5(3) . . C28 C27 C26 112.3(2) . . C28 C27 C29 108.3(3) . . C28 C27 C30 105.6(3) . . C30 C27 C26 115.4(3) . . C30 C27 C29 108.5(2) . . C5 C6 C7 121.7(3) . . C55 C59 C61 113.1(3) . . C55 C59 C60 110.3(3) . . C60 C59 C61 109.7(3) . . C38 C43 C47 123.1(3) . . C42 C43 C38 117.1(3) . . C42 C43 C47 119.8(3) . . C5 C4 C3 121.6(3) . . C53 C54 C55 120.7(3) . . C4 C5 C6 119.6(3) . . C17 C18 C19 121.4(3) . . C32 C31 C26 110.3(3) . . C32 C31 C34 107.5(3) . . C32 C31 C33 106.1(3) . . C34 C31 C26 113.7(3) . . C34 C31 C33 110.2(3) . . C33 C31 C26 108.7(3) . . C51 C56 C58 112.2(3) . . C51 C56 C57 111.1(3) . . C58 C56 C57 109.5(3) . . C63 C62 S1 127.5(3) . . C53 C52 C51 121.4(3) . . C40 C41 C42 120.2(3) . . C52 C53 C54 120.4(3) . . C17 C16 C15 121.9(3) . . C62 C63 C64 125.8(3) . . C41 C42 C43 121.6(4) . . C39 C44 C45 114.3(4) . . C46 C44 C39 112.2(4) . . C46 C44 C45 109.0(4) . . C16 C17 C18 119.9(3) . . C43 C47 C49 111.3(4) . . C43 C47 C48 111.0(4) . . C48 C47 C49 111.3(4) . . C74 C74 C73 129(2) 3_656 3_656 C72 C73 C74 134.9(16) . 3_656 C69 C70 C71 136(3) . . C67 C68 C69 45.2(8) . . C70 C69 C68 89(2) . . C70 C69 C67 153(3) . . C67 C69 C68 65.3(15) . . C69 C67 C68 69.5(13) . . C69 C67 C66 131(2) . . C66 C67 C68 129.0(16) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ti1 S1 2.4052(9) . Ti1 N2 2.127(2) . Ti1 N1 2.159(2) . Ti1 N4 1.810(2) . Ti1 C1 2.594(3) . Ti1 C65 2.040(3) . S1 C62 1.721(3) . N2 C1 1.346(3) . N2 C2 1.441(3) . N1 C1 1.342(3) . N1 C14 1.422(3) . N4 C35 1.296(3) . N6 C35 1.383(3) . N6 C50 1.451(3) . N6 C37 1.394(4) . N5 C35 1.390(3) . N5 C38 1.450(3) . N5 C36 1.395(4) . N3 C1 1.377(3) . N3 C26 1.278(4) . C14 C15 1.411(4) . C14 C19 1.417(4) . C2 C7 1.410(4) . C2 C3 1.415(4) . C38 C39 1.383(4) . C38 C43 1.399(4) . C7 C11 1.525(4) . C7 C6 1.400(4) . C50 C51 1.397(4) . C50 C55 1.396(4) . C15 C20 1.519(4) . C15 C16 1.399(4) . C19 C23 1.515(4) . C19 C18 1.397(4) . C20 C21 1.541(4) . C20 C22 1.526(4) . C51 C56 1.521(4) . C51 C52 1.398(4) . C3 C8 1.524(4) . C3 C4 1.400(4) . C37 C36 1.328(4) . C11 C13 1.534(4) . C11 C12 1.529(4) . C39 C40 1.403(5) . C39 C44 1.509(5) . C55 C59 1.513(5) . C55 C54 1.398(4) . C8 C9 1.530(5) . C8 C10 1.539(5) . C65 C64 1.297(5) . C64 C63 1.459(5) . C26 C27 1.550(5) . C26 C31 1.569(4) . C40 C41 1.362(6) . C23 C24 1.527(4) . C23 C25 1.531(5) . C27 C28 1.526(4) . C27 C29 1.555(4) . C27 C30 1.549(4) . C6 C5 1.382(5) . C59 C61 1.525(5) . C59 C60 1.524(5) . C43 C42 1.397(4) . C43 C47 1.518(5) . C4 C5 1.372(5) . C54 C53 1.378(5) . C18 C17 1.374(5) . C32 C31 1.519(5) . C31 C34 1.542(5) . C31 C33 1.553(5) . C56 C58 1.526(5) . C56 C57 1.528(6) . C62 C63 1.348(5) . C52 C53 1.376(5) . C41 C42 1.363(5) . C16 C17 1.368(5) . C44 C45 1.517(6) . C44 C46 1.499(8) . C47 C49 1.546(7) . C47 C48 1.521(8) . C74 C74 1.352(19) 3_656 C74 C73 1.377(17) 3_656 C71 C70 1.526(18) . C72 C73 1.355(14) . C70 C69 1.141(19) . C68 C69 1.85(2) . C68 C67 1.79(3) . C69 C67 1.40(2) . C66 C67 1.63(2) .