Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email HAGADORN@STRIPE.COLORADO.EDU _publ_contact_author_name 'John R. Hagadorn' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0186 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name J.Hagadorn E.L.Fillis C.Ives data_bc404 _database_code_CSD 196425 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (2,6-Mes2C6H3CS2)Li(Et2O)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H45 Li O2 S2' _chemical_formula_weight 544.75 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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' _cell_length_a 11.5924(13) _cell_length_b 11.5958(12) _cell_length_c 24.140(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.241(2) _cell_angle_gamma 90.00 _cell_volume 3239.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 184(2) _cell_measurement_reflns_used 7123 _cell_measurement_theta_min 2.437 _cell_measurement_theta_max 28.206 _exptl_crystal_description block _exptl_crystal_colour gold _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.117 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.190 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9417 _exptl_absorpt_correction_T_max 0.9523 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 184(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26733 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 26.38 _reflns_number_total 6640 _reflns_number_gt 4537 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1003P)^2^+2.5183P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6640 _refine_ls_number_parameters 334 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1013 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.2027 _refine_ls_wR_factor_gt 0.1793 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.5788(5) 0.2488(6) 0.0582(2) 0.0558(14) Uani 1 1 d . . . S1 S 0.45957(8) 0.15827(7) 0.12760(3) 0.0495(2) Uani 1 1 d . A . S2 S 0.44801(7) 0.40175(7) 0.08959(3) 0.0491(2) Uani 1 1 d . A . C1 C 0.4080(2) 0.2937(2) 0.13049(11) 0.0357(6) Uani 1 1 d . . . C2 C 0.3215(2) 0.3193(2) 0.17277(11) 0.0329(6) Uani 1 1 d . A . C3 C 0.2023(2) 0.3146(2) 0.15811(11) 0.0351(6) Uani 1 1 d . . . C4 C 0.1234(2) 0.3381(3) 0.19808(12) 0.0419(7) Uani 1 1 d . A . H4 H 0.0430 0.3356 0.1881 0.050 Uiso 1 1 calc R . . C5 C 0.1601(3) 0.3651(3) 0.25186(13) 0.0462(7) Uani 1 1 d . . . H5 H 0.1053 0.3803 0.2787 0.055 Uiso 1 1 calc R A . C6 C 0.2768(3) 0.3699(3) 0.26642(12) 0.0414(7) Uani 1 1 d . A . H6 H 0.3017 0.3881 0.3036 0.050 Uiso 1 1 calc R . . C7 C 0.3590(2) 0.3484(2) 0.22754(11) 0.0347(6) Uani 1 1 d . . . C8 C 0.1577(2) 0.2869(2) 0.10011(11) 0.0355(6) Uani 1 1 d . A . C9 C 0.1352(3) 0.1735(3) 0.08413(12) 0.0404(7) Uani 1 1 d . . . C10 C 0.0938(3) 0.1504(3) 0.02983(12) 0.0432(7) Uani 1 1 d . A . H10 H 0.0799 0.0728 0.0188 0.052 Uiso 1 1 calc R . . C11 C 0.0726(3) 0.2382(3) -0.00844(12) 0.0439(7) Uani 1 1 d . . . C12 C 0.0918(3) 0.3509(3) 0.00890(12) 0.0421(7) Uani 1 1 d . A . H12 H 0.0760 0.4119 -0.0167 0.050 Uiso 1 1 calc R . . C13 C 0.1334(2) 0.3775(2) 0.06256(12) 0.0378(6) Uani 1 1 d . . . C14 C 0.1522(3) 0.0752(3) 0.12504(14) 0.0538(8) Uani 1 1 d . A . H14A H 0.2304 0.0787 0.1425 0.065 Uiso 1 1 calc R . . H14B H 0.1414 0.0016 0.1055 0.065 Uiso 1 1 calc R . . H14C H 0.0956 0.0817 0.1536 0.065 Uiso 1 1 calc R . . C15 C 0.0295(3) 0.2115(3) -0.06733(14) 0.0590(9) Uani 1 1 d . A . H15A H -0.0460 0.2480 -0.0750 0.071 Uiso 1 1 calc R . . H15B H 0.0221 0.1279 -0.0720 0.071 Uiso 1 1 calc R . . H15C H 0.0844 0.2415 -0.0932 0.071 Uiso 1 1 calc R . . C16 C 0.1508(3) 0.5010(3) 0.07999(14) 0.0496(8) Uani 1 1 d . A . H16A H 0.1386 0.5514 0.0476 0.060 Uiso 1 1 calc R . . H16B H 0.2297 0.5112 0.0960 0.060 Uiso 1 1 calc R . . H16C H 0.0955 0.5210 0.1077 0.060 Uiso 1 1 calc R . . C17 C 0.4841(2) 0.3595(2) 0.24539(11) 0.0346(6) Uani 1 1 d . A . C18 C 0.5395(3) 0.4657(3) 0.24053(12) 0.0413(7) Uani 1 1 d . . . C19 C 0.6563(3) 0.4740(3) 0.25795(13) 0.0503(8) Uani 1 1 d . A . H19 H 0.6946 0.5459 0.2545 0.060 Uiso 1 1 calc R . . C20 C 0.7180(3) 0.3813(3) 0.27994(13) 0.0517(8) Uani 1 1 d . . . C21 C 0.6595(3) 0.2780(3) 0.28615(13) 0.0484(8) Uani 1 1 d . A . H21 H 0.7001 0.2139 0.3022 0.058 Uiso 1 1 calc R . . C22 C 0.5433(3) 0.2653(3) 0.26965(12) 0.0408(7) Uani 1 1 d . . . C23 C 0.4762(3) 0.5705(3) 0.21741(15) 0.0545(8) Uani 1 1 d . A . H23A H 0.4077 0.5844 0.2384 0.065 Uiso 1 1 calc R . . H23B H 0.4526 0.5572 0.1783 0.065 Uiso 1 1 calc R . . H23C H 0.5273 0.6378 0.2205 0.065 Uiso 1 1 calc R . . C24 C 0.8452(3) 0.3925(4) 0.29628(18) 0.0747(12) Uani 1 1 d . A . H24A H 0.8653 0.3405 0.3274 0.090 Uiso 1 1 calc R . . H24B H 0.8625 0.4722 0.3074 0.090 Uiso 1 1 calc R . . H24C H 0.8905 0.3719 0.2647 0.090 Uiso 1 1 calc R . . C25 C 0.4837(3) 0.1533(2) 0.27867(12) 0.0524(8) Uani 1 1 d . A . H25A H 0.4298 0.1622 0.3082 0.063 Uiso 1 1 calc R . . H25B H 0.5411 0.0942 0.2894 0.063 Uiso 1 1 calc R . . H25C H 0.4410 0.1299 0.2443 0.063 Uiso 1 1 calc R . . O1 O 0.7399(3) 0.2769(2) 0.07584(12) 0.0522(12) Uiso 0.778(10) 1 d PR A 1 C26 C 0.7896(3) 0.0795(2) 0.09228(15) 0.091(3) Uiso 0.778(10) 1 d PR A 1 H26D H 0.7095 0.0610 0.0998 0.109 Uiso 0.778(10) 1 calc PR A 1 H26E H 0.8420 0.0287 0.1142 0.109 Uiso 0.778(10) 1 calc PR A 1 H26F H 0.8011 0.0684 0.0527 0.109 Uiso 0.778(10) 1 calc PR A 1 C27 C 0.8141(6) 0.2012(5) 0.1076(3) 0.0778(18) Uiso 0.778(10) 1 d P A 1 H27C H 0.8028 0.2125 0.1476 0.093 Uiso 0.778(10) 1 calc PR A 1 H27D H 0.8956 0.2195 0.1009 0.093 Uiso 0.778(10) 1 calc PR A 1 C28 C 0.7826(5) 0.3911(5) 0.0722(2) 0.0689(17) Uiso 0.778(10) 1 d P A 1 H28C H 0.7355 0.4330 0.0432 0.083 Uiso 0.778(10) 1 calc PR A 1 H28D H 0.8629 0.3881 0.0604 0.083 Uiso 0.778(10) 1 calc PR A 1 C29 C 0.7811(6) 0.4564(6) 0.1245(3) 0.085(2) Uiso 0.778(10) 1 d P A 1 H29D H 0.7022 0.4589 0.1369 0.102 Uiso 0.778(10) 1 calc PR A 1 H29E H 0.8085 0.5352 0.1185 0.102 Uiso 0.778(10) 1 calc PR A 1 H29F H 0.8318 0.4186 0.1528 0.102 Uiso 0.778(10) 1 calc PR A 1 O1' O 0.739(3) 0.280(2) 0.0880(13) 0.136(10) Uiso 0.222(10) 1 d P A 2 C26' C 0.803(3) 0.091(2) 0.0907(9) 0.26(4) Uiso 0.222(10) 1 d P A 2 H26A H 0.7744 0.1113 0.0529 0.311 Uiso 0.222(10) 1 calc PR A 2 H26B H 0.7569 0.0268 0.1042 0.311 Uiso 0.222(10) 1 calc PR A 2 H26C H 0.8840 0.0678 0.0905 0.311 Uiso 0.222(10) 1 calc PR A 2 C27' C 0.792(3) 0.190(2) 0.1271(9) 0.153(16) Uiso 0.222(10) 1 d PR A 2 H27A H 0.8685 0.2158 0.1430 0.183 Uiso 0.222(10) 1 calc PR A 2 H27B H 0.7413 0.1732 0.1577 0.183 Uiso 0.222(10) 1 calc PR A 2 C28' C 0.780(2) 0.394(2) 0.1278(9) 0.152(15) Uiso 0.222(10) 1 d PR A 2 H28A H 0.7415 0.3940 0.1633 0.183 Uiso 0.222(10) 1 calc PR A 2 H28B H 0.8651 0.3945 0.1356 0.183 Uiso 0.222(10) 1 calc PR A 2 C29' C 0.741(2) 0.493(2) 0.0911(9) 0.153(14) Uiso 0.222(10) 1 d PR A 2 H29A H 0.7361 0.4676 0.0523 0.184 Uiso 0.222(10) 1 calc PR A 2 H29B H 0.7966 0.5562 0.0956 0.184 Uiso 0.222(10) 1 calc PR A 2 H29C H 0.6650 0.5191 0.1016 0.184 Uiso 0.222(10) 1 calc PR A 2 O2 O 0.5529(6) 0.1818(7) -0.0135(3) 0.0635(19) Uiso 0.523(8) 1 d P A 1 C30 C 0.7050(12) 0.2175(14) -0.0685(8) 0.155(6) Uiso 0.523(8) 1 d PD A 1 H30A H 0.6779 0.2894 -0.0862 0.186 Uiso 0.523(8) 1 calc PR A 1 H30B H 0.7572 0.1777 -0.0927 0.186 Uiso 0.523(8) 1 calc PR A 1 H30C H 0.7462 0.2351 -0.0329 0.186 Uiso 0.523(8) 1 calc PR A 1 C31 C 0.6088(11) 0.1456(11) -0.0592(6) 0.127(5) Uiso 0.523(8) 1 d PD A 1 H31A H 0.5544 0.1472 -0.0923 0.152 Uiso 0.523(8) 1 calc PR A 1 H31B H 0.6355 0.0652 -0.0535 0.152 Uiso 0.523(8) 1 calc PR A 1 C32 C 0.4553(10) 0.1390(11) -0.0334(5) 0.098(3) Uiso 0.523(8) 1 d P A 1 H32A H 0.4280 0.0818 -0.0065 0.118 Uiso 0.523(8) 1 calc PR A 1 H32B H 0.4693 0.0972 -0.0681 0.118 Uiso 0.523(8) 1 calc PR A 1 C33 C 0.3651(15) 0.2216(16) -0.0448(8) 0.148(7) Uiso 0.523(8) 1 d P A 1 H33A H 0.3579 0.2712 -0.0123 0.178 Uiso 0.523(8) 1 calc PR A 1 H33B H 0.2919 0.1813 -0.0531 0.178 Uiso 0.523(8) 1 calc PR A 1 H33C H 0.3839 0.2689 -0.0767 0.178 Uiso 0.523(8) 1 calc PR A 1 O2' O 0.5403(6) 0.2179(7) -0.0188(3) 0.062(2) Uiso 0.477(8) 1 d P A 2 C30' C 0.6580(12) 0.2175(10) -0.0999(5) 0.099(4) Uiso 0.477(8) 1 d PD A 2 H30D H 0.7003 0.1491 -0.0862 0.119 Uiso 0.477(8) 1 calc PR A 2 H30E H 0.7116 0.2705 -0.1170 0.119 Uiso 0.477(8) 1 calc PR A 2 H30F H 0.5974 0.1942 -0.1276 0.119 Uiso 0.477(8) 1 calc PR A 2 C31' C 0.6073(12) 0.2734(12) -0.0553(5) 0.122(5) Uiso 0.477(8) 1 d PD A 2 H31C H 0.6714 0.3099 -0.0328 0.146 Uiso 0.477(8) 1 calc PR A 2 H31D H 0.5597 0.3370 -0.0716 0.146 Uiso 0.477(8) 1 calc PR A 2 C32' C 0.4069(12) 0.1952(11) -0.0299(5) 0.079(3) Uiso 0.477(8) 1 d P A 2 H32C H 0.3918 0.1249 -0.0524 0.095 Uiso 0.477(8) 1 calc PR A 2 H32D H 0.3667 0.1893 0.0051 0.095 Uiso 0.477(8) 1 calc PR A 2 C33' C 0.3728(9) 0.3032(9) -0.0618(4) 0.080(3) Uiso 0.477(8) 1 d P A 2 H33D H 0.3981 0.3712 -0.0402 0.096 Uiso 0.477(8) 1 calc PR A 2 H33E H 0.2886 0.3053 -0.0684 0.096 Uiso 0.477(8) 1 calc PR A 2 H33F H 0.4094 0.3033 -0.0974 0.096 Uiso 0.477(8) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.042(3) 0.073(4) 0.053(3) -0.004(3) 0.007(2) 0.005(3) S1 0.0574(5) 0.0424(4) 0.0498(5) -0.0009(4) 0.0139(4) 0.0115(4) S2 0.0544(5) 0.0462(4) 0.0479(5) 0.0056(4) 0.0149(4) 0.0016(4) C1 0.0338(14) 0.0409(15) 0.0320(14) -0.0016(12) -0.0022(11) 0.0013(12) C2 0.0341(14) 0.0305(13) 0.0340(14) -0.0018(11) 0.0016(11) 0.0021(11) C3 0.0347(14) 0.0352(14) 0.0351(14) 0.0003(11) 0.0000(11) 0.0005(11) C4 0.0320(14) 0.0502(17) 0.0436(16) -0.0026(14) 0.0021(12) 0.0012(13) C5 0.0403(16) 0.0576(19) 0.0414(16) -0.0080(14) 0.0086(13) -0.0004(14) C6 0.0428(16) 0.0469(17) 0.0346(15) -0.0070(13) 0.0026(12) -0.0007(13) C7 0.0361(14) 0.0340(14) 0.0340(14) -0.0012(11) 0.0014(11) -0.0013(11) C8 0.0298(13) 0.0403(15) 0.0360(14) -0.0009(12) -0.0011(11) 0.0006(11) C9 0.0403(16) 0.0392(15) 0.0412(16) -0.0002(13) -0.0001(12) -0.0009(12) C10 0.0458(17) 0.0402(16) 0.0429(16) -0.0032(13) -0.0048(13) -0.0042(13) C11 0.0417(16) 0.0510(18) 0.0381(15) -0.0029(14) -0.0050(12) 0.0020(14) C12 0.0436(16) 0.0420(16) 0.0400(16) 0.0044(13) -0.0036(12) 0.0048(13) C13 0.0367(14) 0.0370(15) 0.0392(15) -0.0021(12) -0.0010(12) 0.0019(12) C14 0.069(2) 0.0414(17) 0.0491(19) 0.0069(15) -0.0083(16) -0.0074(16) C15 0.073(2) 0.059(2) 0.0431(18) -0.0054(16) -0.0146(16) 0.0021(18) C16 0.060(2) 0.0361(16) 0.0521(19) 0.0004(14) -0.0073(15) 0.0054(14) C17 0.0357(14) 0.0389(15) 0.0287(13) -0.0027(11) -0.0012(11) -0.0005(12) C18 0.0459(16) 0.0423(16) 0.0356(15) -0.0013(13) 0.0023(12) -0.0059(13) C19 0.0461(18) 0.057(2) 0.0477(18) -0.0047(15) 0.0027(14) -0.0152(15) C20 0.0384(16) 0.075(2) 0.0413(17) -0.0038(16) -0.0022(13) -0.0037(16) C21 0.0427(17) 0.059(2) 0.0429(16) 0.0011(15) -0.0030(13) 0.0077(15) C22 0.0437(16) 0.0457(16) 0.0327(14) 0.0003(13) -0.0015(12) 0.0001(13) C23 0.066(2) 0.0373(17) 0.060(2) -0.0001(15) -0.0004(17) -0.0049(15) C24 0.0417(19) 0.111(3) 0.070(3) -0.003(2) -0.0062(18) -0.011(2) C25 0.063(2) 0.0426(17) 0.0505(19) 0.0072(15) -0.0044(16) -0.0006(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O2 1.905(9) . ? Li1 O1 1.919(7) . ? Li1 O2' 1.919(9) . ? Li1 O1' 1.98(3) . ? Li1 S1 2.467(6) . ? Li1 S2 2.480(6) . ? S1 C1 1.684(3) . ? S2 C1 1.676(3) . ? C1 C2 1.501(4) . ? C2 C3 1.408(4) . ? C2 C7 1.409(4) . ? C3 C4 1.393(4) . ? C3 C8 1.500(4) . ? C4 C5 1.379(4) . ? C5 C6 1.379(4) . ? C6 C7 1.397(4) . ? C7 C17 1.495(4) . ? C8 C9 1.391(4) . ? C8 C13 1.405(4) . ? C9 C10 1.396(4) . ? C9 C14 1.514(4) . ? C10 C11 1.387(4) . ? C11 C12 1.387(4) . ? C11 C15 1.512(4) . ? C12 C13 1.391(4) . ? C13 C16 1.503(4) . ? C17 C18 1.397(4) . ? C17 C22 1.401(4) . ? C18 C19 1.398(4) . ? C18 C23 1.510(4) . ? C19 C20 1.380(5) . ? C20 C21 1.390(5) . ? C20 C24 1.511(4) . ? C21 C22 1.390(4) . ? C22 C25 1.493(4) . ? O1 C28 1.419(6) . ? O1 C27 1.422(8) . ? C26 C27 1.482(7) . ? C28 C29 1.472(8) . ? O1' C27' 1.51(4) . ? O1' C28' 1.69(3) . ? C26' C27' 1.4603 . ? C28' C29' 1.506(6) . ? O2 C32 1.302(12) . ? O2 C31 1.377(14) . ? C30 C31 1.420(5) . ? C32 C33 1.433(18) . ? O2' C31' 1.368(14) . ? O2' C32' 1.577(14) . ? C30' C31' 1.414(5) . ? C32' C33' 1.511(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Li1 O1 111.9(3) . . ? O2 Li1 O2' 13.8(3) . . ? O1 Li1 O2' 114.7(3) . . ? O2 Li1 O1' 120.0(10) . . ? O1 Li1 O1' 8.5(10) . . ? O2' Li1 O1' 123.2(10) . . ? O2 Li1 S1 112.2(3) . . ? O1 Li1 S1 119.8(3) . . ? O2' Li1 S1 118.0(4) . . ? O1' Li1 S1 112.2(9) . . ? O2 Li1 S2 120.1(4) . . ? O1 Li1 S2 114.5(3) . . ? O2' Li1 S2 108.5(4) . . ? O1' Li1 S2 109.5(9) . . ? S1 Li1 S2 73.77(15) . . ? C1 S1 Li1 81.07(17) . . ? C1 S2 Li1 80.80(17) . . ? C2 C1 S2 118.1(2) . . ? C2 C1 S1 117.7(2) . . ? S2 C1 S1 124.21(17) . . ? C3 C2 C7 119.4(2) . . ? C3 C2 C1 120.4(2) . . ? C7 C2 C1 120.2(2) . . ? C4 C3 C2 119.4(3) . . ? C4 C3 C8 118.9(2) . . ? C2 C3 C8 121.7(2) . . ? C5 C4 C3 121.1(3) . . ? C6 C5 C4 119.7(3) . . ? C5 C6 C7 121.2(3) . . ? C6 C7 C2 119.2(3) . . ? C6 C7 C17 118.6(2) . . ? C2 C7 C17 122.3(2) . . ? C9 C8 C13 120.0(3) . . ? C9 C8 C3 120.7(3) . . ? C13 C8 C3 119.2(2) . . ? C8 C9 C10 119.4(3) . . ? C8 C9 C14 121.0(3) . . ? C10 C9 C14 119.6(3) . . ? C11 C10 C9 121.5(3) . . ? C12 C11 C10 118.1(3) . . ? C12 C11 C15 121.0(3) . . ? C10 C11 C15 120.9(3) . . ? C11 C12 C13 122.1(3) . . ? C12 C13 C8 118.8(3) . . ? C12 C13 C16 120.4(3) . . ? C8 C13 C16 120.9(3) . . ? C18 C17 C22 120.4(3) . . ? C18 C17 C7 119.6(3) . . ? C22 C17 C7 119.9(2) . . ? C17 C18 C19 118.5(3) . . ? C17 C18 C23 121.6(3) . . ? C19 C18 C23 119.9(3) . . ? C20 C19 C18 122.3(3) . . ? C19 C20 C21 117.9(3) . . ? C19 C20 C24 120.7(3) . . ? C21 C20 C24 121.4(3) . . ? C20 C21 C22 122.1(3) . . ? C21 C22 C17 118.7(3) . . ? C21 C22 C25 119.9(3) . . ? C17 C22 C25 121.3(3) . . ? C28 O1 C27 114.0(4) . . ? C28 O1 Li1 118.9(4) . . ? C27 O1 Li1 124.5(4) . . ? O1 C27 C26 110.5(5) . . ? O1 C28 C29 114.0(5) . . ? C27' O1' C28' 94.9(19) . . ? C27' O1' Li1 116.4(19) . . ? C28' O1' Li1 126(2) . . ? C26' C27' O1' 102.2(13) . . ? C29' C28' O1' 101.2(13) . . ? C32 O2 C31 91.6(8) . . ? C32 O2 Li1 125.4(7) . . ? C31 O2 Li1 142.6(7) . . ? O2 C31 C30 110.9(12) . . ? O2 C32 C33 115.1(12) . . ? C31' O2' C32' 123.8(10) . . ? C31' O2' Li1 115.2(7) . . ? C32' O2' Li1 111.6(6) . . ? O2' C31' C30' 123.4(12) . . ? C33' C32' O2' 100.0(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.712 _refine_diff_density_min -0.478 _refine_diff_density_rms 0.057 #===END data_bc397 _database_code_CSD 196426 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (2,6-Mes2C6H3CS2)TiCl2(thf)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H51 Cl2 O3 S2 Ti' _chemical_formula_weight 726.70 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.553(6) _cell_length_b 15.809(6) _cell_length_c 16.514(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.35(4) _cell_angle_gamma 90.00 _cell_volume 3711(2) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 8414 _cell_measurement_theta_min 2.466 _cell_measurement_theta_max 30.381 _exptl_crystal_description diamond _exptl_crystal_colour green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1540 _exptl_absorpt_coefficient_mu 0.521 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8895 _exptl_absorpt_correction_T_max 0.8895 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51, 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD area detector' _diffrn_measurement_method ' \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36233 _diffrn_reflns_av_R_equivalents 0.0747 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 29.00 _reflns_number_total 9861 _reflns_number_gt 6815 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0922P)^2^+0.1335P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9861 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0900 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1561 _refine_ls_wR_factor_gt 0.1376 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.24055(3) 0.50364(3) 0.43548(3) 0.02097(12) Uani 1 1 d . . . S1 S 0.18108(5) 0.41487(4) 0.30581(4) 0.02427(15) Uani 1 1 d . . . S2 S 0.31590(4) 0.54862(4) 0.31603(4) 0.02392(14) Uani 1 1 d . . . Cl1 Cl 0.14596(5) 0.42579(4) 0.50507(4) 0.03185(16) Uani 1 1 d . . . Cl2 Cl 0.32279(5) 0.60862(4) 0.52030(4) 0.03155(16) Uani 1 1 d . . . O1 O 0.35050(13) 0.42036(12) 0.48124(10) 0.0285(4) Uani 1 1 d . . . O2 O 0.13052(12) 0.59002(11) 0.40110(10) 0.0242(4) Uani 1 1 d . . . C1 C 0.25195(17) 0.47181(15) 0.25875(14) 0.0212(5) Uani 1 1 d . . . C2 C 0.26333(17) 0.46041(15) 0.17155(14) 0.0216(5) Uani 1 1 d . . . C3 C 0.21035(18) 0.51134(15) 0.10771(15) 0.0232(5) Uani 1 1 d . . . C4 C 0.23461(19) 0.51148(17) 0.03054(16) 0.0284(6) Uani 1 1 d . . . H4 H 0.2009 0.5469 -0.0121 0.034 Uiso 1 1 calc R . . C5 C 0.3059(2) 0.46185(18) 0.01440(16) 0.0314(6) Uani 1 1 d . . . H5 H 0.3228 0.4648 -0.0380 0.038 Uiso 1 1 calc R . . C6 C 0.3531(2) 0.40730(18) 0.07511(16) 0.0310(6) Uani 1 1 d . . . H6 H 0.4007 0.3713 0.0631 0.037 Uiso 1 1 calc R . . C7 C 0.33172(17) 0.40452(16) 0.15387(15) 0.0232(5) Uani 1 1 d . . . C8 C 0.37923(18) 0.33814(16) 0.21272(15) 0.0237(5) Uani 1 1 d . . . C9 C 0.33219(18) 0.26176(16) 0.21968(15) 0.0260(5) Uani 1 1 d . . . C10 C 0.37873(19) 0.19778(17) 0.26999(16) 0.0290(6) Uani 1 1 d . . . H10 H 0.3459 0.1470 0.2758 0.035 Uiso 1 1 calc R . . C11 C 0.47207(19) 0.20582(17) 0.31218(15) 0.0284(6) Uani 1 1 d . . . C12 C 0.51845(19) 0.28158(17) 0.30375(16) 0.0281(6) Uani 1 1 d . . . H12 H 0.5822 0.2881 0.3318 0.034 Uiso 1 1 calc R . . C13 C 0.47349(18) 0.34826(16) 0.25494(15) 0.0261(5) Uani 1 1 d . . . C14 C 0.23232(19) 0.24743(18) 0.17168(18) 0.0327(6) Uani 1 1 d . . . H14A H 0.2136 0.1890 0.1796 0.039 Uiso 1 1 calc R . . H14B H 0.2290 0.2577 0.1126 0.039 Uiso 1 1 calc R . . H14C H 0.1898 0.2864 0.1918 0.039 Uiso 1 1 calc R . . C15 C 0.5218(2) 0.13542(19) 0.36511(19) 0.0386(7) Uani 1 1 d . . . H15A H 0.5611 0.1040 0.3341 0.046 Uiso 1 1 calc R . . H15B H 0.4753 0.0971 0.3803 0.046 Uiso 1 1 calc R . . H15C H 0.5615 0.1592 0.4155 0.046 Uiso 1 1 calc R . . C16 C 0.52614(19) 0.42960(17) 0.24977(18) 0.0317(6) Uani 1 1 d . . . H16A H 0.5864 0.4281 0.2899 0.038 Uiso 1 1 calc R . . H16B H 0.4887 0.4774 0.2624 0.038 Uiso 1 1 calc R . . H16C H 0.5375 0.4361 0.1937 0.038 Uiso 1 1 calc R . . C17 C 0.12652(18) 0.56175(15) 0.11781(14) 0.0225(5) Uani 1 1 d . . . C18 C 0.04056(18) 0.52024(16) 0.11440(14) 0.0242(5) Uani 1 1 d . . . C19 C -0.03953(19) 0.56824(17) 0.11642(15) 0.0269(6) Uani 1 1 d . . . H19 H -0.0971 0.5399 0.1163 0.032 Uiso 1 1 calc R . . C20 C -0.03776(19) 0.65593(17) 0.11852(15) 0.0291(6) Uani 1 1 d . . . C21 C 0.0479(2) 0.69560(16) 0.12104(15) 0.0285(6) Uani 1 1 d . . . H21 H 0.0503 0.7556 0.1226 0.034 Uiso 1 1 calc R . . C22 C 0.13042(19) 0.65102(16) 0.12136(14) 0.0256(5) Uani 1 1 d . . . C23 C 0.03032(19) 0.42558(15) 0.10468(16) 0.0262(5) Uani 1 1 d . . . H23A H -0.0314 0.4083 0.1137 0.031 Uiso 1 1 calc R . . H23B H 0.0799 0.3976 0.1454 0.031 Uiso 1 1 calc R . . H23C H 0.0358 0.4094 0.0486 0.031 Uiso 1 1 calc R . . C24 C -0.1267(2) 0.70611(19) 0.11592(19) 0.0389(7) Uani 1 1 d . . . H24A H -0.1392 0.7095 0.1718 0.047 Uiso 1 1 calc R . . H24B H -0.1795 0.6781 0.0789 0.047 Uiso 1 1 calc R . . H24C H -0.1190 0.7633 0.0954 0.047 Uiso 1 1 calc R . . C25 C 0.22171(19) 0.69721(17) 0.12526(17) 0.0326(6) Uani 1 1 d . . . H25A H 0.2113 0.7582 0.1287 0.039 Uiso 1 1 calc R . . H25B H 0.2455 0.6848 0.0753 0.039 Uiso 1 1 calc R . . H25C H 0.2679 0.6787 0.1743 0.039 Uiso 1 1 calc R . . C26 C 0.40903(19) 0.37281(17) 0.43604(16) 0.0285(6) Uani 1 1 d . . . H26A H 0.4602 0.4087 0.4239 0.034 Uiso 1 1 calc R . . H26B H 0.3711 0.3509 0.3832 0.034 Uiso 1 1 calc R . . C27 C 0.4482(2) 0.30163(18) 0.49305(17) 0.0381(7) Uani 1 1 d . . . H27A H 0.5085 0.2811 0.4819 0.046 Uiso 1 1 calc R . . H27B H 0.4033 0.2539 0.4878 0.046 Uiso 1 1 calc R . . C28 C 0.4622(2) 0.34245(19) 0.57773(16) 0.0337(6) Uani 1 1 d . . . H28A H 0.4626 0.2995 0.6214 0.040 Uiso 1 1 calc R . . H28B H 0.5218 0.3747 0.5908 0.040 Uiso 1 1 calc R . . C29 C 0.3789(2) 0.4003(2) 0.56990(17) 0.0449(8) Uani 1 1 d . . . H29A H 0.3271 0.3719 0.5895 0.054 Uiso 1 1 calc R . . H29B H 0.3964 0.4524 0.6028 0.054 Uiso 1 1 calc R . . C30 C 0.10086(19) 0.63458(17) 0.32252(16) 0.0288(6) Uani 1 1 d . . . H30A H 0.0831 0.5940 0.2762 0.035 Uiso 1 1 calc R . . H30B H 0.1520 0.6712 0.3116 0.035 Uiso 1 1 calc R . . C31 C 0.0174(2) 0.68680(19) 0.33200(17) 0.0356(7) Uani 1 1 d . . . H31A H -0.0417 0.6541 0.3162 0.043 Uiso 1 1 calc R . . H31B H 0.0122 0.7388 0.2978 0.043 Uiso 1 1 calc R . . C32 C 0.0392(2) 0.70805(18) 0.42446(17) 0.0351(7) Uani 1 1 d . . . H32A H 0.0836 0.7561 0.4370 0.042 Uiso 1 1 calc R . . H32B H -0.0188 0.7217 0.4440 0.042 Uiso 1 1 calc R . . C33 C 0.0831(2) 0.62740(18) 0.46258(16) 0.0301(6) Uani 1 1 d . . . H33A H 0.1289 0.6393 0.5149 0.036 Uiso 1 1 calc R . . H33B H 0.0343 0.5886 0.4745 0.036 Uiso 1 1 calc R . . O1S O 0.23028(17) 0.56136(14) -0.18634(14) 0.0490(6) Uani 1 1 d . . . C1S C 0.3100(3) 0.6789(3) -0.1148(2) 0.0626(11) Uani 1 1 d . . . H1S1 H 0.2760 0.6724 -0.0700 0.075 Uiso 1 1 calc R . . H1S2 H 0.3242 0.7389 -0.1210 0.075 Uiso 1 1 calc R . . H1S3 H 0.3688 0.6467 -0.1015 0.075 Uiso 1 1 calc R . . C2S C 0.2507(2) 0.6468(2) -0.1938(2) 0.0470(8) Uani 1 1 d . . . H2S1 H 0.1914 0.6796 -0.2075 0.056 Uiso 1 1 calc R . . H2S2 H 0.2844 0.6545 -0.2394 0.056 Uiso 1 1 calc R . . C3S C 0.1896(3) 0.5210(2) -0.2635(2) 0.0566(10) Uani 1 1 d . . . H3S1 H 0.1896 0.4591 -0.2544 0.068 Uiso 1 1 calc R . . H3S2 H 0.2301 0.5325 -0.3034 0.068 Uiso 1 1 calc R . . C4S C 0.0915(3) 0.5484(2) -0.3016(2) 0.0485(8) Uani 1 1 d . . . H4S1 H 0.0523 0.5443 -0.2603 0.058 Uiso 1 1 calc R . . H4S2 H 0.0657 0.5117 -0.3489 0.058 Uiso 1 1 calc R . . H4S3 H 0.0923 0.6070 -0.3207 0.058 Uiso 1 1 calc R . . 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 0.0244(2) 0.0216(2) 0.0167(2) -0.00035(16) 0.00399(16) 0.00078(17) S1 0.0292(3) 0.0238(3) 0.0198(3) -0.0012(2) 0.0052(2) -0.0040(2) S2 0.0283(3) 0.0248(3) 0.0187(3) -0.0026(2) 0.0051(2) -0.0042(2) Cl1 0.0354(4) 0.0320(4) 0.0309(3) 0.0061(3) 0.0133(3) 0.0008(3) Cl2 0.0322(3) 0.0326(3) 0.0276(3) -0.0081(3) 0.0014(3) -0.0026(3) O1 0.0355(10) 0.0353(10) 0.0149(8) 0.0027(7) 0.0060(7) 0.0117(8) O2 0.0291(9) 0.0255(9) 0.0184(8) -0.0013(7) 0.0056(7) 0.0064(7) C1 0.0222(12) 0.0217(12) 0.0193(11) -0.0004(9) 0.0036(9) 0.0017(9) C2 0.0253(13) 0.0227(12) 0.0165(11) -0.0022(9) 0.0034(9) -0.0022(10) C3 0.0290(13) 0.0203(12) 0.0195(11) -0.0014(9) 0.0035(10) -0.0021(10) C4 0.0350(15) 0.0313(14) 0.0183(12) 0.0012(10) 0.0041(10) -0.0003(11) C5 0.0389(16) 0.0382(16) 0.0184(12) -0.0011(11) 0.0090(11) -0.0005(12) C6 0.0366(15) 0.0310(14) 0.0262(13) -0.0057(11) 0.0083(11) 0.0037(12) C7 0.0258(13) 0.0241(12) 0.0193(11) -0.0034(9) 0.0039(9) -0.0011(10) C8 0.0265(13) 0.0243(13) 0.0205(12) -0.0040(9) 0.0053(10) 0.0023(10) C9 0.0289(13) 0.0265(13) 0.0228(12) -0.0070(10) 0.0062(10) 0.0012(10) C10 0.0375(15) 0.0233(13) 0.0280(13) -0.0030(10) 0.0112(11) 0.0008(11) C11 0.0343(14) 0.0294(14) 0.0215(12) -0.0025(10) 0.0059(10) 0.0088(11) C12 0.0302(14) 0.0288(14) 0.0239(13) -0.0040(10) 0.0031(10) 0.0040(11) C13 0.0296(13) 0.0264(13) 0.0233(12) -0.0049(10) 0.0077(10) 0.0010(10) C14 0.0315(15) 0.0290(14) 0.0359(15) -0.0066(11) 0.0038(12) -0.0036(11) C15 0.0436(17) 0.0324(15) 0.0375(16) 0.0015(13) 0.0035(13) 0.0081(13) C16 0.0296(14) 0.0303(15) 0.0346(15) -0.0015(11) 0.0050(12) -0.0008(11) C17 0.0281(13) 0.0212(12) 0.0168(11) 0.0012(9) 0.0018(9) 0.0012(10) C18 0.0321(14) 0.0218(12) 0.0165(11) -0.0002(9) 0.0005(9) 0.0014(10) C19 0.0295(14) 0.0296(14) 0.0200(12) 0.0005(10) 0.0014(10) -0.0003(11) C20 0.0357(15) 0.0309(14) 0.0189(12) 0.0005(10) 0.0016(10) 0.0068(11) C21 0.0441(16) 0.0201(12) 0.0202(12) 0.0002(9) 0.0041(11) 0.0043(11) C22 0.0385(15) 0.0228(12) 0.0144(11) 0.0009(9) 0.0029(10) -0.0017(11) C23 0.0308(14) 0.0217(12) 0.0240(12) -0.0015(10) 0.0015(10) -0.0020(10) C24 0.0435(17) 0.0352(16) 0.0358(16) -0.0019(12) 0.0036(13) 0.0130(13) C25 0.0388(16) 0.0272(14) 0.0317(14) 0.0004(11) 0.0077(12) -0.0056(12) C26 0.0315(14) 0.0337(15) 0.0214(12) 0.0020(10) 0.0078(10) 0.0107(11) C27 0.0492(18) 0.0320(15) 0.0322(15) 0.0057(12) 0.0068(13) 0.0117(13) C28 0.0340(15) 0.0440(17) 0.0222(13) 0.0068(12) 0.0039(11) 0.0058(13) C29 0.057(2) 0.060(2) 0.0169(13) 0.0088(13) 0.0067(13) 0.0271(16) C30 0.0348(15) 0.0280(14) 0.0222(12) 0.0041(10) 0.0032(10) 0.0075(11) C31 0.0389(16) 0.0364(16) 0.0283(14) 0.0002(12) 0.0002(12) 0.0104(13) C32 0.0441(17) 0.0329(15) 0.0279(14) -0.0042(11) 0.0066(12) 0.0117(13) C33 0.0317(14) 0.0350(15) 0.0247(13) -0.0027(11) 0.0086(11) 0.0069(11) O1S 0.0631(15) 0.0372(12) 0.0420(13) 0.0022(10) 0.0011(11) -0.0037(11) C1S 0.083(3) 0.057(2) 0.050(2) -0.0116(18) 0.019(2) -0.018(2) C2S 0.055(2) 0.0367(17) 0.0486(19) -0.0004(15) 0.0103(16) 0.0013(15) C3S 0.062(2) 0.049(2) 0.057(2) -0.0157(17) 0.0073(18) 0.0057(18) C4S 0.061(2) 0.0430(19) 0.0422(18) 0.0032(15) 0.0116(16) -0.0042(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 2.0851(19) . ? Ti1 O2 2.0886(18) . ? Ti1 Cl1 2.3254(10) . ? Ti1 Cl2 2.3305(10) . ? Ti1 S1 2.5517(11) . ? Ti1 S2 2.5542(11) . ? S1 C1 1.679(3) . ? S2 C1 1.691(3) . ? O1 C26 1.456(3) . ? O1 C29 1.469(3) . ? O2 C30 1.458(3) . ? O2 C33 1.469(3) . ? C1 C2 1.495(3) . ? C2 C7 1.407(3) . ? C2 C3 1.417(3) . ? C3 C4 1.393(4) . ? C3 C17 1.496(4) . ? C4 C5 1.371(4) . ? C5 C6 1.388(4) . ? C6 C7 1.401(4) . ? C7 C8 1.495(3) . ? C8 C9 1.405(4) . ? C8 C13 1.409(4) . ? C9 C10 1.390(4) . ? C9 C14 1.516(4) . ? C10 C11 1.394(4) . ? C11 C12 1.396(4) . ? C11 C15 1.502(4) . ? C12 C13 1.401(4) . ? C13 C16 1.509(4) . ? C17 C18 1.403(4) . ? C17 C22 1.413(3) . ? C18 C19 1.397(4) . ? C18 C23 1.509(3) . ? C19 C20 1.387(4) . ? C20 C21 1.389(4) . ? C20 C24 1.511(4) . ? C21 C22 1.391(4) . ? C22 C25 1.505(4) . ? C26 C27 1.499(4) . ? C27 C28 1.514(4) . ? C28 C29 1.501(4) . ? C30 C31 1.504(4) . ? C31 C32 1.529(4) . ? C32 C33 1.502(4) . ? O1S C2S 1.395(4) . ? O1S C3S 1.435(4) . ? C1S C2S 1.491(5) . ? C3S C4S 1.495(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 O2 174.66(7) . . ? O1 Ti1 Cl1 88.64(6) . . ? O2 Ti1 Cl1 88.85(6) . . ? O1 Ti1 Cl2 88.63(7) . . ? O2 Ti1 Cl2 87.89(6) . . ? Cl1 Ti1 Cl2 111.23(4) . . ? O1 Ti1 S1 93.05(6) . . ? O2 Ti1 S1 91.65(6) . . ? Cl1 Ti1 S1 89.61(4) . . ? Cl2 Ti1 S1 159.14(3) . . ? O1 Ti1 S2 91.88(6) . . ? O2 Ti1 S2 92.23(6) . . ? Cl1 Ti1 S2 157.87(3) . . ? Cl2 Ti1 S2 90.91(3) . . ? S1 Ti1 S2 68.26(3) . . ? C1 S1 Ti1 87.81(9) . . ? C1 S2 Ti1 87.49(9) . . ? C26 O1 C29 109.19(19) . . ? C26 O1 Ti1 128.90(14) . . ? C29 O1 Ti1 121.90(16) . . ? C30 O2 C33 109.10(19) . . ? C30 O2 Ti1 128.42(15) . . ? C33 O2 Ti1 121.45(14) . . ? C2 C1 S1 125.91(18) . . ? C2 C1 S2 117.66(18) . . ? S1 C1 S2 116.43(14) . . ? C7 C2 C3 119.9(2) . . ? C7 C2 C1 120.3(2) . . ? C3 C2 C1 119.6(2) . . ? C4 C3 C2 118.5(2) . . ? C4 C3 C17 118.3(2) . . ? C2 C3 C17 123.1(2) . . ? C5 C4 C3 121.8(2) . . ? C4 C5 C6 119.6(3) . . ? C5 C6 C7 121.1(3) . . ? C6 C7 C2 118.7(2) . . ? C6 C7 C8 117.5(2) . . ? C2 C7 C8 123.7(2) . . ? C9 C8 C13 119.8(2) . . ? C9 C8 C7 119.4(2) . . ? C13 C8 C7 120.5(2) . . ? C10 C9 C8 119.4(2) . . ? C10 C9 C14 119.6(2) . . ? C8 C9 C14 121.0(2) . . ? C9 C10 C11 122.1(3) . . ? C10 C11 C12 117.9(2) . . ? C10 C11 C15 121.3(3) . . ? C12 C11 C15 120.7(2) . . ? C11 C12 C13 121.8(2) . . ? C12 C13 C8 119.0(2) . . ? C12 C13 C16 119.6(2) . . ? C8 C13 C16 121.4(2) . . ? C18 C17 C22 119.8(2) . . ? C18 C17 C3 119.2(2) . . ? C22 C17 C3 120.7(2) . . ? C19 C18 C17 119.1(2) . . ? C19 C18 C23 118.5(2) . . ? C17 C18 C23 122.3(2) . . ? C20 C19 C18 122.2(3) . . ? C19 C20 C21 117.6(2) . . ? C19 C20 C24 120.9(3) . . ? C21 C20 C24 121.5(3) . . ? C20 C21 C22 122.7(2) . . ? C21 C22 C17 118.6(2) . . ? C21 C22 C25 120.5(2) . . ? C17 C22 C25 120.9(2) . . ? O1 C26 C27 104.5(2) . . ? C26 C27 C28 102.6(2) . . ? C29 C28 C27 103.5(2) . . ? O1 C29 C28 105.5(2) . . ? O2 C30 C31 105.3(2) . . ? C30 C31 C32 103.0(2) . . ? C33 C32 C31 102.2(2) . . ? O2 C33 C32 105.8(2) . . ? C2S O1S C3S 114.0(3) . . ? O1S C2S C1S 110.3(3) . . ? O1S C3S C4S 114.9(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.448 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.088 #===END data_bc411 _database_code_CSD 196427 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (2,6-Trip2C6H3CS2)2TiCl2(py)2a2py _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C83 H113 Cl2 N O S4 Ti' _chemical_formula_weight 1387.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7871(7) _cell_length_b 16.9214(9) _cell_length_c 20.3901(11) _cell_angle_alpha 80.0020(10) _cell_angle_beta 78.0300(10) _cell_angle_gamma 68.3500(10) _cell_volume 3988.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 135(2) _cell_measurement_reflns_used 8316 _cell_measurement_theta_min 2.315 _cell_measurement_theta_max 30.899 _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1492 _exptl_absorpt_coefficient_mu 0.322 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.822 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51, 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 135(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56179 _diffrn_reflns_av_R_equivalents 0.053 _diffrn_reflns_av_sigmaI/netI 0.0661 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.48 _reflns_number_total 18248 _reflns_number_gt 13638 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+4.0850P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18248 _refine_ls_number_parameters 780 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1722 _refine_ls_wR_factor_gt 0.1628 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.45774(4) 0.12900(3) 0.28786(2) 0.02441(11) Uani 1 1 d . . . Cl1 Cl 0.28501(6) 0.15603(4) 0.35814(3) 0.03380(15) Uani 1 1 d . . . Cl2 Cl 0.63185(6) 0.09999(5) 0.22085(4) 0.03683(16) Uani 1 1 d . . . S1 S 0.47689(6) -0.02914(4) 0.30832(3) 0.03106(16) Uani 1 1 d . . . S2 S 0.38899(7) 0.08358(4) 0.19771(3) 0.03181(16) Uani 1 1 d . . . C1 C 0.4215(2) -0.01555(16) 0.23791(13) 0.0260(5) Uani 1 1 d . . . C2 C 0.4045(2) -0.08320(16) 0.20766(12) 0.0249(5) Uani 1 1 d . . . C3 C 0.4988(2) -0.14355(16) 0.17424(13) 0.0265(5) Uani 1 1 d . . . C4 C 0.4804(2) -0.20003(18) 0.13869(13) 0.0307(6) Uani 1 1 d . . . H4 H 0.5434 -0.2410 0.1152 0.037 Uiso 1 1 calc R . . C5 C 0.3702(3) -0.19626(19) 0.13779(14) 0.0340(6) Uani 1 1 d . . . H5 H 0.3582 -0.2331 0.1121 0.041 Uiso 1 1 calc R . . C6 C 0.2781(2) -0.13941(18) 0.17395(14) 0.0314(6) Uani 1 1 d . . . H6 H 0.2035 -0.1388 0.1738 0.038 Uiso 1 1 calc R . . C7 C 0.2927(2) -0.08270(17) 0.21077(13) 0.0265(5) Uani 1 1 d . . . C8 C 0.6176(2) -0.14981(16) 0.17764(13) 0.0275(5) Uani 1 1 d . . . C9 C 0.6751(2) -0.10600(17) 0.12726(13) 0.0287(5) Uani 1 1 d . . . C10 C 0.7828(2) -0.10966(18) 0.13473(14) 0.0316(6) Uani 1 1 d . . . H10 H 0.8222 -0.0800 0.1010 0.038 Uiso 1 1 calc R . . C11 C 0.8343(2) -0.15558(18) 0.19023(14) 0.0315(6) Uani 1 1 d . . . C12 C 0.7766(3) -0.19954(19) 0.23858(15) 0.0350(6) Uani 1 1 d . . . H12 H 0.8115 -0.2316 0.2762 0.042 Uiso 1 1 calc R . . C13 C 0.6687(2) -0.19806(18) 0.23359(14) 0.0313(6) Uani 1 1 d . . . C14 C 0.6228(3) -0.05748(19) 0.06491(14) 0.0331(6) Uani 1 1 d . . . H14 H 0.5388 -0.0455 0.0756 0.040 Uiso 1 1 calc R . . C15 C 0.6417(3) 0.0277(2) 0.04306(16) 0.0443(8) Uani 1 1 d . . . H15A H 0.6175 0.0612 0.0817 0.053 Uiso 1 1 calc R . . H15B H 0.5971 0.0595 0.0072 0.053 Uiso 1 1 calc R . . H15C H 0.7227 0.0173 0.0263 0.053 Uiso 1 1 calc R . . C16 C 0.6707(3) -0.1139(2) 0.00680(15) 0.0473(8) Uani 1 1 d . . . H16A H 0.7541 -0.1349 0.0007 0.057 Uiso 1 1 calc R . . H16B H 0.6449 -0.0803 -0.0348 0.057 Uiso 1 1 calc R . . H16C H 0.6437 -0.1625 0.0174 0.057 Uiso 1 1 calc R . . C17 C 0.9475(2) -0.15333(19) 0.20001(15) 0.0350(6) Uani 1 1 d . . . H17 H 0.9831 -0.1308 0.1559 0.042 Uiso 1 1 calc R . . C18 C 0.9288(3) -0.0916(2) 0.25165(16) 0.0399(7) Uani 1 1 d . . . H18A H 0.8786 -0.0346 0.2365 0.048 Uiso 1 1 calc R . . H18B H 1.0022 -0.0888 0.2560 0.048 Uiso 1 1 calc R . . H18C H 0.8935 -0.1120 0.2954 0.048 Uiso 1 1 calc R . . C19 C 1.0297(3) -0.2422(2) 0.2200(2) 0.0497(8) Uani 1 1 d . . . H19A H 1.0094 -0.2587 0.2681 0.060 Uiso 1 1 calc R . . H19B H 1.1076 -0.2415 0.2111 0.060 Uiso 1 1 calc R . . H19C H 1.0247 -0.2836 0.1936 0.060 Uiso 1 1 calc R . . C20 C 0.6088(3) -0.2487(2) 0.28717(15) 0.0385(7) Uani 1 1 d . . . H20 H 0.5249 -0.2177 0.2898 0.046 Uiso 1 1 calc R . . C21 C 0.6385(3) -0.2570(2) 0.35750(16) 0.0484(8) Uani 1 1 d . . . H21A H 0.7212 -0.2833 0.3558 0.058 Uiso 1 1 calc R . . H21B H 0.6010 -0.2929 0.3888 0.058 Uiso 1 1 calc R . . H21C H 0.6124 -0.2002 0.3730 0.058 Uiso 1 1 calc R . . C22 C 0.6346(4) -0.3377(2) 0.2666(2) 0.0554(9) Uani 1 1 d . . . H22A H 0.7173 -0.3660 0.2559 0.067 Uiso 1 1 calc R . . H22B H 0.5996 -0.3321 0.2268 0.067 Uiso 1 1 calc R . . H22C H 0.6036 -0.3719 0.3038 0.067 Uiso 1 1 calc R . . C23 C 0.1957(2) -0.03191(18) 0.25869(13) 0.0298(6) Uani 1 1 d . . . C24 C 0.1798(2) -0.06878(18) 0.32616(14) 0.0308(6) Uani 1 1 d . . . C25 C 0.0910(2) -0.02249(19) 0.37194(14) 0.0347(6) Uani 1 1 d . . . H25 H 0.0803 -0.0474 0.4172 0.042 Uiso 1 1 calc R . . C26 C 0.0178(3) 0.05833(19) 0.35396(14) 0.0352(6) Uani 1 1 d . . . C27 C 0.0320(3) 0.0929(2) 0.28717(15) 0.0384(7) Uani 1 1 d . . . H27 H -0.0190 0.1479 0.2739 0.046 Uiso 1 1 calc R . . C28 C 0.1199(2) 0.04882(19) 0.23895(14) 0.0328(6) Uani 1 1 d . . . C29 C 0.2528(3) -0.15991(19) 0.34880(14) 0.0336(6) Uani 1 1 d . . . H29 H 0.3170 -0.1803 0.3113 0.040 Uiso 1 1 calc R . . C30 C 0.3045(3) -0.1659(2) 0.41165(15) 0.0428(7) Uani 1 1 d . . . H30A H 0.3606 -0.1370 0.4005 0.051 Uiso 1 1 calc R . . H30B H 0.3418 -0.2261 0.4273 0.051 Uiso 1 1 calc R . . H30C H 0.2440 -0.1384 0.4473 0.051 Uiso 1 1 calc R . . C31 C 0.1838(3) -0.2197(2) 0.36162(19) 0.0505(8) Uani 1 1 d . . . H31A H 0.2277 -0.2754 0.3830 0.061 Uiso 1 1 calc R . . H31B H 0.1675 -0.2272 0.3187 0.061 Uiso 1 1 calc R . . H31C H 0.1120 -0.1949 0.3914 0.061 Uiso 1 1 calc R . . C32 C -0.0719(3) 0.1080(2) 0.40846(16) 0.0426(7) Uani 1 1 d . . . H32 H -0.0925 0.0651 0.4439 0.051 Uiso 1 1 calc R . . C33 C -0.0184(4) 0.1550(3) 0.4415(2) 0.0619(11) Uani 1 1 d . . . H33A H 0.0362 0.1135 0.4691 0.074 Uiso 1 1 calc R . . H33B H -0.0781 0.1954 0.4701 0.074 Uiso 1 1 calc R . . H33C H 0.0212 0.1862 0.4064 0.074 Uiso 1 1 calc R . . C34 C -0.1804(3) 0.1671(3) 0.38334(19) 0.0633(11) Uani 1 1 d . . . H34A H -0.2367 0.1923 0.4214 0.076 Uiso 1 1 calc R . . H34B H -0.2105 0.1347 0.3615 0.076 Uiso 1 1 calc R . . H34C H -0.1643 0.2127 0.3508 0.076 Uiso 1 1 calc R . . C35 C 0.1294(3) 0.0867(2) 0.16525(14) 0.0371(6) Uani 1 1 d . . . H35 H 0.2095 0.0588 0.1432 0.045 Uiso 1 1 calc R . . C36 C 0.1050(3) 0.1830(2) 0.15656(18) 0.0497(8) Uani 1 1 d . . . H36A H 0.0260 0.2124 0.1764 0.060 Uiso 1 1 calc R . . H36B H 0.1165 0.2030 0.1084 0.060 Uiso 1 1 calc R . . H36C H 0.1567 0.1955 0.1793 0.060 Uiso 1 1 calc R . . C37 C 0.0507(3) 0.0659(3) 0.12880(18) 0.0573(10) Uani 1 1 d . . . H37A H 0.0618 0.0048 0.1384 0.069 Uiso 1 1 calc R . . H37B H 0.0688 0.0802 0.0801 0.069 Uiso 1 1 calc R . . H37C H -0.0288 0.0994 0.1446 0.069 Uiso 1 1 calc R . . S3 S 0.36538(6) 0.26226(4) 0.21394(3) 0.03211(16) Uani 1 1 d . . . S4 S 0.48419(6) 0.26037(4) 0.31672(3) 0.02895(15) Uani 1 1 d . . . C38 C 0.4086(2) 0.31812(16) 0.25604(12) 0.0249(5) Uani 1 1 d . . . C39 C 0.3786(2) 0.41257(16) 0.24045(12) 0.0249(5) Uani 1 1 d . . . C40 C 0.2980(2) 0.46634(16) 0.28634(13) 0.0285(5) Uani 1 1 d . . . C41 C 0.2678(3) 0.55491(17) 0.27027(15) 0.0363(6) Uani 1 1 d . . . H41 H 0.2126 0.5923 0.3005 0.044 Uiso 1 1 calc R . . C42 C 0.3180(3) 0.58849(18) 0.21045(16) 0.0426(7) Uani 1 1 d . . . H42 H 0.2971 0.6487 0.2000 0.051 Uiso 1 1 calc R . . C43 C 0.3983(3) 0.53480(18) 0.16602(15) 0.0365(6) Uani 1 1 d . . . H43 H 0.4320 0.5588 0.1253 0.044 Uiso 1 1 calc R . . C44 C 0.4306(2) 0.44626(17) 0.17978(13) 0.0276(5) Uani 1 1 d . . . C45 C 0.2436(2) 0.43173(17) 0.35202(13) 0.0304(6) Uani 1 1 d . A . C46 C 0.1442(3) 0.41430(18) 0.35513(15) 0.0353(6) Uani 1 1 d . . . C47 C 0.0951(3) 0.3850(2) 0.41848(17) 0.0435(7) Uani 1 1 d . A . H47 H 0.0274 0.3728 0.4216 0.052 Uiso 1 1 calc R . . C48 C 0.1419(3) 0.37333(19) 0.47664(15) 0.0413(7) Uani 1 1 d D . . C49 C 0.2401(3) 0.39093(19) 0.47163(15) 0.0397(7) Uani 1 1 d . A . H49 H 0.2728 0.3830 0.5111 0.048 Uiso 1 1 calc R . . C50 C 0.2927(3) 0.41990(17) 0.41092(14) 0.0350(6) Uani 1 1 d . . . C51 C 0.0874(3) 0.4295(2) 0.29335(18) 0.0432(7) Uani 1 1 d . . . H51 H 0.1456 0.4313 0.2525 0.052 Uiso 1 1 calc R . . C52 C -0.0097(3) 0.5170(2) 0.2923(2) 0.0624(10) Uani 1 1 d . . . H52A H -0.0699 0.5159 0.3307 0.075 Uiso 1 1 calc R . . H52B H -0.0411 0.5288 0.2502 0.075 Uiso 1 1 calc R . . H52C H 0.0200 0.5617 0.2953 0.075 Uiso 1 1 calc R . . C53 C 0.0427(3) 0.3585(2) 0.2892(2) 0.0579(10) Uani 1 1 d . . . H53A H 0.1028 0.3028 0.2955 0.069 Uiso 1 1 calc R . . H53B H 0.0199 0.3656 0.2449 0.069 Uiso 1 1 calc R . . H53C H -0.0232 0.3616 0.3245 0.069 Uiso 1 1 calc R . . C54 C 0.0916(3) 0.3394(2) 0.54554(17) 0.0328(9) Uiso 0.846(8) 1 d P A 1 C55 C 0.1401(4) 0.2405(2) 0.5519(2) 0.0369(10) Uiso 0.846(8) 1 d P A 1 C56 C -0.0388(3) 0.3730(3) 0.5578(2) 0.0431(11) Uiso 0.846(8) 1 d P A 1 C54' C 0.0590(9) 0.3297(7) 0.5183(5) 0.030(5) Uiso 0.154(8) 1 d PD A 2 C55' C 0.1175(13) 0.2345(6) 0.5392(7) 0.012(3) Uiso 0.154(8) 1 d PD A 2 C56' C 0.0093(15) 0.3787(8) 0.5803(8) 0.032(5) Uiso 0.154(8) 1 d PD A 2 C57 C 0.3997(3) 0.4401(2) 0.40930(16) 0.0430(7) Uani 1 1 d . A . H57 H 0.4409 0.4383 0.3619 0.052 Uiso 1 1 calc R . . C58 C 0.4819(3) 0.3763(2) 0.45473(18) 0.0523(9) Uani 1 1 d . . . H58A H 0.4458 0.3799 0.5020 0.063 Uiso 1 1 calc R A . H58B H 0.5516 0.3901 0.4481 0.063 Uiso 1 1 calc R . . H58C H 0.5008 0.3183 0.4432 0.063 Uiso 1 1 calc R . . C59 C 0.3702(4) 0.5305(3) 0.4285(3) 0.0718(12) Uani 1 1 d . . . H59A H 0.3269 0.5726 0.3956 0.086 Uiso 1 1 calc R A . H59B H 0.4406 0.5409 0.4287 0.086 Uiso 1 1 calc R . . H59C H 0.3243 0.5357 0.4735 0.086 Uiso 1 1 calc R . . C60 C 0.5261(2) 0.39077(17) 0.13346(13) 0.0307(6) Uani 1 1 d . B . C61 C 0.6383(3) 0.36942(19) 0.14505(16) 0.0382(7) Uani 1 1 d . . . C62 C 0.7282(3) 0.3232(2) 0.0997(2) 0.0542(9) Uani 1 1 d . B . H62 H 0.8038 0.3088 0.1081 0.065 Uiso 1 1 calc R . . C63 C 0.7122(3) 0.2977(2) 0.0434(2) 0.0597(10) Uani 1 1 d . . . C64 C 0.6011(4) 0.3173(3) 0.03364(19) 0.0593(10) Uani 1 1 d . B . H64 H 0.5885 0.2983 -0.0042 0.071 Uiso 1 1 calc R . . C65 C 0.5055(3) 0.36431(19) 0.07727(15) 0.0382(7) Uani 1 1 d . . . C66 C 0.6650(3) 0.3994(2) 0.20330(18) 0.0478(8) Uani 1 1 d . . . H66 H 0.5922 0.4215 0.2349 0.057 Uiso 1 1 calc R . . C67 C 0.7482(4) 0.3270(3) 0.2424(2) 0.0758(14) Uani 1 1 d . . . H67A H 0.7222 0.2779 0.2533 0.091 Uiso 1 1 calc R . . H67B H 0.7520 0.3463 0.2842 0.091 Uiso 1 1 calc R . . H67C H 0.8239 0.3103 0.2149 0.091 Uiso 1 1 calc R . . C68 C 0.7105(5) 0.4732(3) 0.1786(2) 0.0744(13) Uani 1 1 d . . . H68A H 0.7889 0.4509 0.1551 0.089 Uiso 1 1 calc R . . H68B H 0.7091 0.5011 0.2172 0.089 Uiso 1 1 calc R . . H68C H 0.6626 0.5149 0.1475 0.089 Uiso 1 1 calc R . . C69 C 0.8039(5) 0.2549(4) -0.0174(3) 0.0423(15) Uiso 0.613(9) 1 d P B 1 C70 C 0.8227(5) 0.1576(4) -0.0024(3) 0.0397(14) Uiso 0.613(9) 1 d P B 1 C71 C 0.9167(6) 0.2690(4) -0.0197(3) 0.059(2) Uiso 0.613(9) 1 d P B 1 C69' C 0.8292(8) 0.2371(6) 0.0135(5) 0.048(3) Uiso 0.387(9) 1 d P B 2 C70' C 0.8372(10) 0.1416(8) 0.0243(7) 0.061(3) Uiso 0.387(9) 1 d P B 2 C71' C 0.8373(8) 0.2794(6) -0.0577(5) 0.053(3) Uiso 0.387(9) 1 d P B 2 C72 C 0.3854(3) 0.3885(2) 0.06223(16) 0.0454(8) Uani 1 1 d . B . H72 H 0.3323 0.4000 0.1058 0.054 Uiso 1 1 calc R . . C73 C 0.3678(5) 0.3155(3) 0.0350(2) 0.0763(14) Uani 1 1 d . . . H73A H 0.4094 0.3087 -0.0109 0.092 Uiso 1 1 calc R B . H73B H 0.2864 0.3293 0.0347 0.092 Uiso 1 1 calc R . . H73C H 0.3964 0.2621 0.0641 0.092 Uiso 1 1 calc R . . C74 C 0.3528(4) 0.4711(3) 0.0138(2) 0.0712(13) Uani 1 1 d . . . H74A H 0.3695 0.5155 0.0304 0.085 Uiso 1 1 calc R B . H74B H 0.2713 0.4903 0.0113 0.085 Uiso 1 1 calc R . . H74C H 0.3969 0.4600 -0.0312 0.085 Uiso 1 1 calc R . . N1 N 0.5466(2) 0.08009(14) 0.38033(11) 0.0291(5) Uani 1 1 d . . . C75 C 0.4988(3) 0.11350(18) 0.43942(14) 0.0330(6) Uani 1 1 d . . . H75 H 0.4265 0.1579 0.4422 0.040 Uiso 1 1 calc R . . C76 C 0.5518(3) 0.0851(2) 0.49633(15) 0.0426(7) Uani 1 1 d . . . H76 H 0.5162 0.1100 0.5372 0.051 Uiso 1 1 calc R . . C77 C 0.6563(3) 0.0202(2) 0.49309(17) 0.0479(8) Uani 1 1 d . . . H77 H 0.6936 -0.0004 0.5316 0.058 Uiso 1 1 calc R . . C78 C 0.7055(3) -0.0139(2) 0.43296(18) 0.0478(8) Uani 1 1 d . . . H78 H 0.7776 -0.0585 0.4294 0.057 Uiso 1 1 calc R . . C79 C 0.6492(3) 0.01726(18) 0.37769(16) 0.0384(7) Uani 1 1 d . . . H79 H 0.6842 -0.0066 0.3363 0.046 Uiso 1 1 calc R . . 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 0.0319(3) 0.0200(2) 0.0235(2) -0.00115(17) -0.00805(18) -0.01005(18) Cl1 0.0347(4) 0.0328(3) 0.0327(3) -0.0021(3) -0.0033(3) -0.0120(3) Cl2 0.0380(4) 0.0356(4) 0.0370(4) -0.0101(3) -0.0026(3) -0.0118(3) S1 0.0472(4) 0.0237(3) 0.0287(3) 0.0003(2) -0.0164(3) -0.0154(3) S2 0.0482(4) 0.0248(3) 0.0289(3) 0.0018(3) -0.0169(3) -0.0163(3) C1 0.0309(13) 0.0254(12) 0.0243(12) -0.0015(10) -0.0064(10) -0.0123(11) C2 0.0319(13) 0.0234(12) 0.0237(12) 0.0030(9) -0.0099(10) -0.0139(11) C3 0.0338(14) 0.0253(13) 0.0247(12) 0.0006(10) -0.0095(11) -0.0141(11) C4 0.0373(15) 0.0320(14) 0.0260(13) -0.0082(11) -0.0025(11) -0.0147(12) C5 0.0441(16) 0.0402(16) 0.0285(13) -0.0089(12) -0.0049(12) -0.0252(13) C6 0.0336(14) 0.0396(15) 0.0287(13) -0.0055(11) -0.0056(11) -0.0202(12) C7 0.0319(14) 0.0269(13) 0.0234(12) -0.0003(10) -0.0075(10) -0.0128(11) C8 0.0314(14) 0.0255(13) 0.0295(13) -0.0035(10) -0.0084(11) -0.0122(11) C9 0.0355(14) 0.0280(13) 0.0266(13) -0.0021(10) -0.0086(11) -0.0139(11) C10 0.0343(15) 0.0339(14) 0.0299(13) -0.0020(11) -0.0050(11) -0.0161(12) C11 0.0315(14) 0.0323(14) 0.0341(14) -0.0048(11) -0.0076(11) -0.0130(12) C12 0.0386(16) 0.0347(15) 0.0346(15) 0.0052(12) -0.0150(12) -0.0151(13) C13 0.0385(15) 0.0295(14) 0.0288(13) 0.0017(11) -0.0096(12) -0.0151(12) C14 0.0385(16) 0.0395(16) 0.0266(13) 0.0036(11) -0.0089(12) -0.0205(13) C15 0.055(2) 0.0437(18) 0.0395(17) 0.0096(14) -0.0161(15) -0.0252(16) C16 0.062(2) 0.056(2) 0.0285(15) -0.0024(14) -0.0120(15) -0.0234(17) C17 0.0307(14) 0.0369(15) 0.0403(16) -0.0023(12) -0.0103(12) -0.0132(12) C18 0.0337(16) 0.0456(18) 0.0465(17) -0.0107(14) -0.0072(13) -0.0175(14) C19 0.0427(18) 0.0407(18) 0.071(2) -0.0063(16) -0.0236(17) -0.0121(15) C20 0.0389(16) 0.0400(17) 0.0378(16) 0.0107(13) -0.0112(13) -0.0188(14) C21 0.0465(19) 0.057(2) 0.0397(17) 0.0165(15) -0.0143(15) -0.0207(16) C22 0.068(2) 0.0398(19) 0.066(2) 0.0107(17) -0.020(2) -0.0289(18) C23 0.0335(14) 0.0343(14) 0.0272(13) -0.0038(11) -0.0071(11) -0.0166(12) C24 0.0348(15) 0.0321(14) 0.0286(13) -0.0030(11) -0.0068(11) -0.0145(12) C25 0.0369(15) 0.0409(16) 0.0281(14) -0.0028(12) -0.0048(12) -0.0163(13) C26 0.0364(16) 0.0382(16) 0.0314(14) -0.0062(12) -0.0011(12) -0.0144(13) C27 0.0371(16) 0.0352(16) 0.0387(16) -0.0020(13) -0.0072(13) -0.0078(13) C28 0.0334(15) 0.0362(15) 0.0295(14) -0.0005(11) -0.0068(11) -0.0132(12) C29 0.0387(16) 0.0351(15) 0.0282(13) 0.0005(11) -0.0085(12) -0.0140(13) C30 0.0486(18) 0.0501(19) 0.0344(16) 0.0028(14) -0.0159(14) -0.0209(15) C31 0.067(2) 0.0402(18) 0.055(2) 0.0002(15) -0.0239(18) -0.0250(17) C32 0.0448(18) 0.0431(18) 0.0345(16) -0.0038(13) 0.0023(13) -0.0136(14) C33 0.070(3) 0.072(3) 0.051(2) -0.0276(19) 0.0160(19) -0.038(2) C34 0.056(2) 0.065(3) 0.044(2) -0.0033(18) 0.0045(17) 0.0014(19) C35 0.0384(16) 0.0394(16) 0.0289(14) 0.0032(12) -0.0073(12) -0.0101(13) C36 0.052(2) 0.0397(18) 0.0435(18) 0.0083(14) -0.0023(15) -0.0077(15) C37 0.063(2) 0.075(3) 0.0389(18) 0.0084(17) -0.0212(17) -0.030(2) S3 0.0463(4) 0.0231(3) 0.0317(3) 0.0017(3) -0.0169(3) -0.0138(3) S4 0.0394(4) 0.0206(3) 0.0298(3) -0.0012(2) -0.0124(3) -0.0108(3) C38 0.0312(13) 0.0204(12) 0.0231(12) -0.0014(9) -0.0041(10) -0.0097(10) C39 0.0289(13) 0.0221(12) 0.0219(12) -0.0006(9) -0.0037(10) -0.0076(10) C40 0.0341(14) 0.0221(12) 0.0251(12) -0.0015(10) -0.0004(11) -0.0077(11) C41 0.0430(17) 0.0225(13) 0.0336(15) -0.0039(11) 0.0053(13) -0.0059(12) C42 0.0495(19) 0.0201(13) 0.0446(17) 0.0025(12) 0.0047(14) -0.0052(13) C43 0.0404(16) 0.0269(14) 0.0321(14) 0.0035(11) 0.0060(12) -0.0092(12) C44 0.0316(14) 0.0253(13) 0.0234(12) -0.0017(10) -0.0024(10) -0.0085(11) C45 0.0369(15) 0.0219(12) 0.0263(13) -0.0012(10) 0.0013(11) -0.0069(11) C46 0.0356(15) 0.0267(14) 0.0365(15) -0.0006(11) -0.0004(12) -0.0067(12) C47 0.0351(16) 0.0339(16) 0.0526(19) -0.0031(14) 0.0079(14) -0.0102(13) C48 0.0473(18) 0.0266(14) 0.0339(15) 0.0003(12) 0.0054(13) -0.0020(13) C49 0.0492(18) 0.0322(15) 0.0284(14) -0.0015(12) -0.0009(13) -0.0071(13) C50 0.0467(17) 0.0235(13) 0.0294(14) -0.0038(11) -0.0031(12) -0.0071(12) C51 0.0387(17) 0.0399(17) 0.0497(19) -0.0020(14) -0.0095(14) -0.0119(14) C52 0.055(2) 0.045(2) 0.080(3) -0.0031(19) -0.026(2) -0.0022(17) C53 0.051(2) 0.054(2) 0.076(3) -0.0062(19) -0.0187(19) -0.0211(18) C57 0.058(2) 0.0368(16) 0.0377(16) -0.0023(13) -0.0153(15) -0.0172(15) C58 0.063(2) 0.052(2) 0.0453(19) -0.0049(16) -0.0217(17) -0.0172(18) C59 0.088(3) 0.046(2) 0.092(3) -0.012(2) -0.030(3) -0.026(2) C60 0.0382(15) 0.0229(13) 0.0262(13) -0.0015(10) 0.0011(11) -0.0088(11) C61 0.0383(16) 0.0279(14) 0.0420(16) -0.0006(12) -0.0041(13) -0.0066(12) C62 0.0371(18) 0.0384(18) 0.074(3) -0.0097(17) 0.0017(17) -0.0016(14) C63 0.047(2) 0.047(2) 0.081(3) -0.033(2) 0.0201(19) -0.0166(17) C64 0.069(3) 0.065(2) 0.051(2) -0.0328(19) 0.0206(18) -0.035(2) C65 0.0501(18) 0.0355(16) 0.0291(14) -0.0073(12) 0.0029(13) -0.0179(14) C66 0.0412(18) 0.055(2) 0.0460(18) -0.0012(15) -0.0125(15) -0.0144(16) C67 0.061(3) 0.086(3) 0.085(3) 0.025(3) -0.040(2) -0.031(2) C68 0.114(4) 0.064(3) 0.065(3) 0.001(2) -0.029(3) -0.048(3) C72 0.061(2) 0.055(2) 0.0277(15) -0.0004(14) -0.0061(14) -0.0310(17) C73 0.103(4) 0.104(4) 0.053(2) -0.026(2) -0.007(2) -0.066(3) C74 0.070(3) 0.093(3) 0.053(2) 0.032(2) -0.023(2) -0.041(3) N1 0.0393(13) 0.0218(11) 0.0291(11) -0.0026(9) -0.0124(10) -0.0102(10) C75 0.0451(17) 0.0302(14) 0.0285(13) -0.0021(11) -0.0110(12) -0.0161(13) C76 0.065(2) 0.0411(17) 0.0316(15) -0.0019(13) -0.0173(15) -0.0255(16) C77 0.071(2) 0.0374(17) 0.0440(18) 0.0057(14) -0.0321(17) -0.0212(17) C78 0.057(2) 0.0276(15) 0.061(2) -0.0012(14) -0.0338(18) -0.0054(14) C79 0.0478(18) 0.0259(14) 0.0444(17) -0.0057(12) -0.0208(14) -0.0080(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N1 2.277(2) . ? Ti1 Cl2 2.2867(9) . ? Ti1 Cl1 2.3045(8) . ? Ti1 S3 2.5190(8) . ? Ti1 S2 2.5302(8) . ? Ti1 S4 2.5484(8) . ? Ti1 S1 2.5624(8) . ? S1 C1 1.674(3) . ? S2 C1 1.676(3) . ? C1 C2 1.491(3) . ? C2 C3 1.398(4) . ? C2 C7 1.415(4) . ? C3 C4 1.405(4) . ? C3 C8 1.499(4) . ? C4 C5 1.391(4) . ? C5 C6 1.380(4) . ? C6 C7 1.400(4) . ? C7 C23 1.495(4) . ? C8 C9 1.403(4) . ? C8 C13 1.409(4) . ? C9 C10 1.395(4) . ? C9 C14 1.524(4) . ? C10 C11 1.394(4) . ? C11 C12 1.385(4) . ? C11 C17 1.516(4) . ? C12 C13 1.396(4) . ? C13 C20 1.526(4) . ? C14 C15 1.525(4) . ? C14 C16 1.533(4) . ? C17 C19 1.527(4) . ? C17 C18 1.533(4) . ? C20 C21 1.529(4) . ? C20 C22 1.532(5) . ? C23 C28 1.401(4) . ? C23 C24 1.415(4) . ? C24 C25 1.390(4) . ? C24 C29 1.527(4) . ? C25 C26 1.380(4) . ? C26 C27 1.389(4) . ? C26 C32 1.530(4) . ? C27 C28 1.401(4) . ? C28 C35 1.527(4) . ? C29 C31 1.530(4) . ? C29 C30 1.532(4) . ? C32 C34 1.510(5) . ? C32 C33 1.527(5) . ? C35 C36 1.527(5) . ? C35 C37 1.533(5) . ? S3 C38 1.673(2) . ? S4 C38 1.673(3) . ? C38 C39 1.491(3) . ? C39 C40 1.403(4) . ? C39 C44 1.412(4) . ? C40 C41 1.399(4) . ? C40 C45 1.504(4) . ? C41 C42 1.388(4) . ? C42 C43 1.382(4) . ? C43 C44 1.393(4) . ? C44 C60 1.500(4) . ? C45 C46 1.394(4) . ? C45 C50 1.419(4) . ? C46 C47 1.407(4) . ? C46 C51 1.520(4) . ? C47 C48 1.389(5) . ? C48 C49 1.373(5) . ? C48 C54 1.528(4) . ? C48 C54' 1.542(5) . ? C49 C50 1.383(4) . ? C50 C57 1.520(5) . ? C51 C53 1.529(5) . ? C51 C52 1.542(5) . ? C54 C56 1.530(5) . ? C54 C55 1.548(5) . ? C54' C56' 1.526(5) . ? C54' C55' 1.529(5) . ? C57 C58 1.532(5) . ? C57 C59 1.535(5) . ? C60 C61 1.404(4) . ? C60 C65 1.405(4) . ? C61 C62 1.391(5) . ? C61 C66 1.514(5) . ? C62 C63 1.372(6) . ? C63 C64 1.383(6) . ? C63 C69' 1.539(10) . ? C63 C69 1.588(7) . ? C64 C65 1.413(5) . ? C65 C72 1.518(5) . ? C66 C67 1.522(5) . ? C66 C68 1.533(5) . ? C69 C71 1.537(9) . ? C69 C70 1.557(8) . ? C69' C71' 1.504(15) . ? C69' C70' 1.560(15) . ? C72 C74 1.537(5) . ? C72 C73 1.543(5) . ? N1 C79 1.347(4) . ? N1 C75 1.349(4) . ? C75 C76 1.389(4) . ? C76 C77 1.379(5) . ? C77 C78 1.375(5) . ? C78 C79 1.385(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ti1 Cl2 89.36(7) . . ? N1 Ti1 Cl1 88.93(7) . . ? Cl2 Ti1 Cl1 178.27(3) . . ? N1 Ti1 S3 143.44(6) . . ? Cl2 Ti1 S3 93.77(3) . . ? Cl1 Ti1 S3 87.79(3) . . ? N1 Ti1 S2 143.77(6) . . ? Cl2 Ti1 S2 88.03(3) . . ? Cl1 Ti1 S2 93.17(3) . . ? S3 Ti1 S2 72.79(2) . . ? N1 Ti1 S4 76.07(6) . . ? Cl2 Ti1 S4 87.83(3) . . ? Cl1 Ti1 S4 92.05(3) . . ? S3 Ti1 S4 67.68(2) . . ? S2 Ti1 S4 139.85(3) . . ? N1 Ti1 S1 76.71(6) . . ? Cl2 Ti1 S1 92.26(3) . . ? Cl1 Ti1 S1 87.05(3) . . ? S3 Ti1 S1 139.36(3) . . ? S2 Ti1 S1 67.30(2) . . ? S4 Ti1 S1 152.78(3) . . ? C1 S1 Ti1 88.42(9) . . ? C1 S2 Ti1 89.48(9) . . ? C2 C1 S1 126.16(19) . . ? C2 C1 S2 118.97(18) . . ? S1 C1 S2 114.80(14) . . ? C3 C2 C7 121.3(2) . . ? C3 C2 C1 119.3(2) . . ? C7 C2 C1 119.3(2) . . ? C2 C3 C4 118.7(2) . . ? C2 C3 C8 120.9(2) . . ? C4 C3 C8 120.4(2) . . ? C5 C4 C3 120.2(3) . . ? C6 C5 C4 120.5(2) . . ? C5 C6 C7 121.1(2) . . ? C6 C7 C2 117.8(2) . . ? C6 C7 C23 120.7(2) . . ? C2 C7 C23 121.0(2) . . ? C9 C8 C13 120.8(2) . . ? C9 C8 C3 120.5(2) . . ? C13 C8 C3 118.6(2) . . ? C10 C9 C8 118.3(2) . . ? C10 C9 C14 120.6(2) . . ? C8 C9 C14 121.1(2) . . ? C11 C10 C9 122.0(3) . . ? C12 C11 C10 118.5(3) . . ? C12 C11 C17 120.4(3) . . ? C10 C11 C17 121.1(3) . . ? C11 C12 C13 121.9(3) . . ? C12 C13 C8 118.4(2) . . ? C12 C13 C20 120.4(2) . . ? C8 C13 C20 121.2(2) . . ? C9 C14 C15 113.4(2) . . ? C9 C14 C16 109.5(2) . . ? C15 C14 C16 110.0(3) . . ? C11 C17 C19 112.1(2) . . ? C11 C17 C18 110.3(2) . . ? C19 C17 C18 111.2(3) . . ? C13 C20 C21 113.6(2) . . ? C13 C20 C22 110.5(3) . . ? C21 C20 C22 109.8(3) . . ? C28 C23 C24 119.6(3) . . ? C28 C23 C7 122.6(2) . . ? C24 C23 C7 117.8(2) . . ? C25 C24 C23 118.9(3) . . ? C25 C24 C29 119.2(2) . . ? C23 C24 C29 121.7(3) . . ? C26 C25 C24 122.3(3) . . ? C25 C26 C27 118.3(3) . . ? C25 C26 C32 119.2(3) . . ? C27 C26 C32 122.5(3) . . ? C26 C27 C28 121.7(3) . . ? C23 C28 C27 119.2(3) . . ? C23 C28 C35 120.5(3) . . ? C27 C28 C35 120.3(3) . . ? C24 C29 C31 110.7(2) . . ? C24 C29 C30 113.0(2) . . ? C31 C29 C30 109.6(2) . . ? C34 C32 C33 112.3(3) . . ? C34 C32 C26 113.7(3) . . ? C33 C32 C26 108.9(3) . . ? C28 C35 C36 113.3(3) . . ? C28 C35 C37 110.5(3) . . ? C36 C35 C37 110.2(3) . . ? C38 S3 Ti1 89.16(9) . . ? C38 S4 Ti1 88.18(9) . . ? C39 C38 S4 123.66(18) . . ? C39 C38 S3 121.36(18) . . ? S4 C38 S3 114.97(14) . . ? C40 C39 C44 121.2(2) . . ? C40 C39 C38 119.1(2) . . ? C44 C39 C38 119.6(2) . . ? C41 C40 C39 118.7(2) . . ? C41 C40 C45 119.2(2) . . ? C39 C40 C45 122.1(2) . . ? C42 C41 C40 120.4(3) . . ? C43 C42 C41 120.4(3) . . ? C42 C43 C44 121.3(3) . . ? C43 C44 C39 118.1(2) . . ? C43 C44 C60 119.2(2) . . ? C39 C44 C60 122.5(2) . . ? C46 C45 C50 120.7(3) . . ? C46 C45 C40 120.2(2) . . ? C50 C45 C40 119.1(3) . . ? C45 C46 C47 117.5(3) . . ? C45 C46 C51 121.8(3) . . ? C47 C46 C51 120.6(3) . . ? C48 C47 C46 122.5(3) . . ? C49 C48 C47 118.4(3) . . ? C49 C48 C54 118.4(3) . . ? C47 C48 C54 123.2(3) . . ? C49 C48 C54' 148.0(5) . . ? C47 C48 C54' 92.6(5) . . ? C54 C48 C54' 31.3(5) . . ? C48 C49 C50 122.1(3) . . ? C49 C50 C45 118.8(3) . . ? C49 C50 C57 119.3(3) . . ? C45 C50 C57 121.8(3) . . ? C46 C51 C53 112.8(3) . . ? C46 C51 C52 109.9(3) . . ? C53 C51 C52 110.4(3) . . ? C48 C54 C56 112.9(3) . . ? C48 C54 C55 108.5(3) . . ? C56 C54 C55 111.5(3) . . ? C56' C54' C55' 110.5(5) . . ? C56' C54' C48 103.6(10) . . ? C55' C54' C48 113.2(9) . . ? C50 C57 C58 113.9(3) . . ? C50 C57 C59 111.3(3) . . ? C58 C57 C59 108.7(3) . . ? C61 C60 C65 120.1(3) . . ? C61 C60 C44 118.6(2) . . ? C65 C60 C44 121.2(3) . . ? C62 C61 C60 119.2(3) . . ? C62 C61 C66 118.6(3) . . ? C60 C61 C66 122.0(3) . . ? C63 C62 C61 122.6(3) . . ? C62 C63 C64 117.4(3) . . ? C62 C63 C69' 106.3(5) . . ? C64 C63 C69' 135.0(5) . . ? C62 C63 C69 129.1(4) . . ? C64 C63 C69 113.2(4) . . ? C69' C63 C69 27.1(4) . . ? C63 C64 C65 123.2(3) . . ? C60 C65 C64 117.4(3) . . ? C60 C65 C72 121.4(3) . . ? C64 C65 C72 121.2(3) . . ? C61 C66 C67 112.2(3) . . ? C61 C66 C68 110.7(3) . . ? C67 C66 C68 110.6(3) . . ? C71 C69 C70 109.6(5) . . ? C71 C69 C63 110.8(5) . . ? C70 C69 C63 105.2(4) . . ? C71' C69' C63 99.5(7) . . ? C71' C69' C70' 117.6(9) . . ? C63 C69' C70' 112.9(7) . . ? C65 C72 C74 111.6(3) . . ? C65 C72 C73 112.4(3) . . ? C74 C72 C73 110.7(3) . . ? C79 N1 C75 117.8(2) . . ? C79 N1 Ti1 121.05(19) . . ? C75 N1 Ti1 121.17(18) . . ? N1 C75 C76 122.2(3) . . ? C77 C76 C75 119.5(3) . . ? C78 C77 C76 118.6(3) . . ? C77 C78 C79 119.5(3) . . ? N1 C79 C78 122.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ti1 S1 C1 -175.95(11) . . . . ? Cl2 Ti1 S1 C1 -87.14(10) . . . . ? Cl1 Ti1 S1 C1 94.45(10) . . . . ? S3 Ti1 S1 C1 11.31(11) . . . . ? S2 Ti1 S1 C1 -0.23(9) . . . . ? S4 Ti1 S1 C1 -176.79(11) . . . . ? N1 Ti1 S2 C1 7.28(15) . . . . ? Cl2 Ti1 S2 C1 93.51(10) . . . . ? Cl1 Ti1 S2 C1 -85.24(10) . . . . ? S3 Ti1 S2 C1 -171.93(10) . . . . ? S4 Ti1 S2 C1 177.79(10) . . . . ? S1 Ti1 S2 C1 0.23(9) . . . . ? Ti1 S1 C1 C2 177.4(2) . . . . ? Ti1 S1 C1 S2 0.35(15) . . . . ? Ti1 S2 C1 C2 -177.7(2) . . . . ? Ti1 S2 C1 S1 -0.36(15) . . . . ? S1 C1 C2 C3 -74.1(3) . . . . ? S2 C1 C2 C3 102.8(3) . . . . ? S1 C1 C2 C7 108.6(3) . . . . ? S2 C1 C2 C7 -74.4(3) . . . . ? C7 C2 C3 C4 5.2(4) . . . . ? C1 C2 C3 C4 -172.0(2) . . . . ? C7 C2 C3 C8 -173.2(2) . . . . ? C1 C2 C3 C8 9.7(4) . . . . ? C2 C3 C4 C5 -0.9(4) . . . . ? C8 C3 C4 C5 177.5(2) . . . . ? C3 C4 C5 C6 -2.6(4) . . . . ? C4 C5 C6 C7 1.8(4) . . . . ? C5 C6 C7 C2 2.4(4) . . . . ? C5 C6 C7 C23 -169.7(3) . . . . ? C3 C2 C7 C6 -5.9(4) . . . . ? C1 C2 C7 C6 171.2(2) . . . . ? C3 C2 C7 C23 166.2(2) . . . . ? C1 C2 C7 C23 -16.7(4) . . . . ? C2 C3 C8 C9 -94.1(3) . . . . ? C4 C3 C8 C9 87.6(3) . . . . ? C2 C3 C8 C13 83.7(3) . . . . ? C4 C3 C8 C13 -94.6(3) . . . . ? C13 C8 C9 C10 -1.5(4) . . . . ? C3 C8 C9 C10 176.2(2) . . . . ? C13 C8 C9 C14 176.9(3) . . . . ? C3 C8 C9 C14 -5.4(4) . . . . ? C8 C9 C10 C11 0.3(4) . . . . ? C14 C9 C10 C11 -178.1(3) . . . . ? C9 C10 C11 C12 0.9(4) . . . . ? C9 C10 C11 C17 -175.4(3) . . . . ? C10 C11 C12 C13 -0.8(4) . . . . ? C17 C11 C12 C13 175.4(3) . . . . ? C11 C12 C13 C8 -0.3(4) . . . . ? C11 C12 C13 C20 178.8(3) . . . . ? C9 C8 C13 C12 1.6(4) . . . . ? C3 C8 C13 C12 -176.2(3) . . . . ? C9 C8 C13 C20 -177.6(3) . . . . ? C3 C8 C13 C20 4.7(4) . . . . ? C10 C9 C14 C15 -41.6(4) . . . . ? C8 C9 C14 C15 140.0(3) . . . . ? C10 C9 C14 C16 81.6(3) . . . . ? C8 C9 C14 C16 -96.8(3) . . . . ? C12 C11 C17 C19 48.9(4) . . . . ? C10 C11 C17 C19 -135.0(3) . . . . ? C12 C11 C17 C18 -75.7(3) . . . . ? C10 C11 C17 C18 100.5(3) . . . . ? C12 C13 C20 C21 31.3(4) . . . . ? C8 C13 C20 C21 -149.6(3) . . . . ? C12 C13 C20 C22 -92.6(3) . . . . ? C8 C13 C20 C22 86.5(3) . . . . ? C6 C7 C23 C28 -89.3(3) . . . . ? C2 C7 C23 C28 98.8(3) . . . . ? C6 C7 C23 C24 89.2(3) . . . . ? C2 C7 C23 C24 -82.6(3) . . . . ? C28 C23 C24 C25 -2.1(4) . . . . ? C7 C23 C24 C25 179.3(2) . . . . ? C28 C23 C24 C29 174.1(2) . . . . ? C7 C23 C24 C29 -4.5(4) . . . . ? C23 C24 C25 C26 -0.1(4) . . . . ? C29 C24 C25 C26 -176.4(3) . . . . ? C24 C25 C26 C27 2.0(4) . . . . ? C24 C25 C26 C32 -175.2(3) . . . . ? C25 C26 C27 C28 -1.7(4) . . . . ? C32 C26 C27 C28 175.4(3) . . . . ? C24 C23 C28 C27 2.4(4) . . . . ? C7 C23 C28 C27 -179.1(3) . . . . ? C24 C23 C28 C35 -175.0(3) . . . . ? C7 C23 C28 C35 3.6(4) . . . . ? C26 C27 C28 C23 -0.5(4) . . . . ? C26 C27 C28 C35 176.9(3) . . . . ? C25 C24 C29 C31 68.8(3) . . . . ? C23 C24 C29 C31 -107.4(3) . . . . ? C25 C24 C29 C30 -54.6(4) . . . . ? C23 C24 C29 C30 129.2(3) . . . . ? C25 C26 C32 C34 -148.4(3) . . . . ? C27 C26 C32 C34 34.5(4) . . . . ? C25 C26 C32 C33 85.6(4) . . . . ? C27 C26 C32 C33 -91.5(4) . . . . ? C23 C28 C35 C36 -142.1(3) . . . . ? C27 C28 C35 C36 40.5(4) . . . . ? C23 C28 C35 C37 93.7(3) . . . . ? C27 C28 C35 C37 -83.6(4) . . . . ? N1 Ti1 S3 C38 7.15(15) . . . . ? Cl2 Ti1 S3 C38 -86.87(9) . . . . ? Cl1 Ti1 S3 C38 92.36(9) . . . . ? S2 Ti1 S3 C38 -173.63(10) . . . . ? S4 Ti1 S3 C38 -0.77(9) . . . . ? S1 Ti1 S3 C38 175.23(10) . . . . ? N1 Ti1 S4 C38 -174.37(11) . . . . ? Cl2 Ti1 S4 C38 95.74(9) . . . . ? Cl1 Ti1 S4 C38 -85.99(9) . . . . ? S3 Ti1 S4 C38 0.77(9) . . . . ? S2 Ti1 S4 C38 11.39(11) . . . . ? S1 Ti1 S4 C38 -173.53(11) . . . . ? Ti1 S4 C38 C39 177.6(2) . . . . ? Ti1 S4 C38 S3 -1.19(14) . . . . ? Ti1 S3 C38 C39 -177.6(2) . . . . ? Ti1 S3 C38 S4 1.20(14) . . . . ? S4 C38 C39 C40 -70.7(3) . . . . ? S3 C38 C39 C40 107.9(3) . . . . ? S4 C38 C39 C44 109.8(3) . . . . ? S3 C38 C39 C44 -71.5(3) . . . . ? C44 C39 C40 C41 1.4(4) . . . . ? C38 C39 C40 C41 -178.0(3) . . . . ? C44 C39 C40 C45 -178.5(3) . . . . ? C38 C39 C40 C45 2.0(4) . . . . ? C39 C40 C41 C42 -0.9(5) . . . . ? C45 C40 C41 C42 179.0(3) . . . . ? C40 C41 C42 C43 0.1(5) . . . . ? C41 C42 C43 C44 0.1(5) . . . . ? C42 C43 C44 C39 0.3(4) . . . . ? C42 C43 C44 C60 -174.0(3) . . . . ? C40 C39 C44 C43 -1.1(4) . . . . ? C38 C39 C44 C43 178.3(3) . . . . ? C40 C39 C44 C60 173.0(3) . . . . ? C38 C39 C44 C60 -7.6(4) . . . . ? C41 C40 C45 C46 91.5(3) . . . . ? C39 C40 C45 C46 -88.6(3) . . . . ? C41 C40 C45 C50 -86.4(3) . . . . ? C39 C40 C45 C50 93.5(3) . . . . ? C50 C45 C46 C47 0.2(4) . . . . ? C40 C45 C46 C47 -177.7(3) . . . . ? C50 C45 C46 C51 177.7(3) . . . . ? C40 C45 C46 C51 -0.2(4) . . . . ? C45 C46 C47 C48 0.0(4) . . . . ? C51 C46 C47 C48 -177.6(3) . . . . ? C46 C47 C48 C49 -0.2(5) . . . . ? C46 C47 C48 C54 -178.4(3) . . . . ? C46 C47 C48 C54' -171.6(5) . . . . ? C47 C48 C49 C50 0.2(5) . . . . ? C54 C48 C49 C50 178.4(3) . . . . ? C54' C48 C49 C50 163.8(9) . . . . ? C48 C49 C50 C45 0.0(4) . . . . ? C48 C49 C50 C57 178.6(3) . . . . ? C46 C45 C50 C49 -0.2(4) . . . . ? C40 C45 C50 C49 177.7(3) . . . . ? C46 C45 C50 C57 -178.7(3) . . . . ? C40 C45 C50 C57 -0.8(4) . . . . ? C45 C46 C51 C53 139.6(3) . . . . ? C47 C46 C51 C53 -43.0(4) . . . . ? C45 C46 C51 C52 -96.8(4) . . . . ? C47 C46 C51 C52 80.7(4) . . . . ? C49 C48 C54 C56 143.9(3) . . . . ? C47 C48 C54 C56 -38.0(4) . . . . ? C54' C48 C54 C56 -51.1(9) . . . . ? C49 C48 C54 C55 -92.0(4) . . . . ? C47 C48 C54 C55 86.2(4) . . . . ? C54' C48 C54 C55 73.1(9) . . . . ? C49 C48 C54' C56' 65.6(13) . . . . ? C47 C48 C54' C56' -128.8(8) . . . . ? C54 C48 C54' C56' 40.3(8) . . . . ? C49 C48 C54' C55' -54.1(14) . . . . ? C47 C48 C54' C55' 111.5(8) . . . . ? C54 C48 C54' C55' -79.5(10) . . . . ? C49 C50 C57 C58 39.9(4) . . . . ? C45 C50 C57 C58 -141.5(3) . . . . ? C49 C50 C57 C59 -83.4(4) . . . . ? C45 C50 C57 C59 95.2(4) . . . . ? C43 C44 C60 C61 87.0(3) . . . . ? C39 C44 C60 C61 -87.1(3) . . . . ? C43 C44 C60 C65 -89.5(3) . . . . ? C39 C44 C60 C65 96.5(3) . . . . ? C65 C60 C61 C62 1.1(4) . . . . ? C44 C60 C61 C62 -175.4(3) . . . . ? C65 C60 C61 C66 177.6(3) . . . . ? C44 C60 C61 C66 1.1(4) . . . . ? C60 C61 C62 C63 0.3(5) . . . . ? C66 C61 C62 C63 -176.2(3) . . . . ? C61 C62 C63 C64 -2.0(6) . . . . ? C61 C62 C63 C69' -171.2(5) . . . . ? C61 C62 C63 C69 172.0(4) . . . . ? C62 C63 C64 C65 2.2(6) . . . . ? C69' C63 C64 C65 167.5(7) . . . . ? C69 C63 C64 C65 -172.7(4) . . . . ? C61 C60 C65 C64 -0.8(4) . . . . ? C44 C60 C65 C64 175.5(3) . . . . ? C61 C60 C65 C72 -178.2(3) . . . . ? C44 C60 C65 C72 -1.8(4) . . . . ? C63 C64 C65 C60 -0.9(5) . . . . ? C63 C64 C65 C72 176.5(4) . . . . ? C62 C61 C66 C67 -51.3(4) . . . . ? C60 C61 C66 C67 132.2(3) . . . . ? C62 C61 C66 C68 72.7(4) . . . . ? C60 C61 C66 C68 -103.7(4) . . . . ? C62 C63 C69 C71 -18.2(7) . . . . ? C64 C63 C69 C71 155.9(5) . . . . ? C69' C63 C69 C71 -55.8(9) . . . . ? C62 C63 C69 C70 100.1(5) . . . . ? C64 C63 C69 C70 -85.8(5) . . . . ? C69' C63 C69 C70 62.5(9) . . . . ? C62 C63 C69' C71' -127.0(6) . . . . ? C64 C63 C69' C71' 66.7(9) . . . . ? C69 C63 C69' C71' 23.5(7) . . . . ? C62 C63 C69' C70' 107.5(8) . . . . ? C64 C63 C69' C70' -58.8(11) . . . . ? C69 C63 C69' C70' -102.0(12) . . . . ? C60 C65 C72 C74 92.9(4) . . . . ? C64 C65 C72 C74 -84.3(4) . . . . ? C60 C65 C72 C73 -142.0(3) . . . . ? C64 C65 C72 C73 40.7(4) . . . . ? Cl2 Ti1 N1 C79 -31.6(2) . . . . ? Cl1 Ti1 N1 C79 148.1(2) . . . . ? S3 Ti1 N1 C79 -127.09(19) . . . . ? S2 Ti1 N1 C79 54.2(3) . . . . ? S4 Ti1 N1 C79 -119.5(2) . . . . ? S1 Ti1 N1 C79 60.9(2) . . . . ? Cl2 Ti1 N1 C75 147.8(2) . . . . ? Cl1 Ti1 N1 C75 -32.5(2) . . . . ? S3 Ti1 N1 C75 52.3(3) . . . . ? S2 Ti1 N1 C75 -126.39(18) . . . . ? S4 Ti1 N1 C75 59.90(19) . . . . ? S1 Ti1 N1 C75 -119.7(2) . . . . ? C79 N1 C75 C76 -0.1(4) . . . . ? Ti1 N1 C75 C76 -179.6(2) . . . . ? N1 C75 C76 C77 -0.4(5) . . . . ? C75 C76 C77 C78 0.5(5) . . . . ? C76 C77 C78 C79 -0.2(5) . . . . ? C75 N1 C79 C78 0.5(4) . . . . ? Ti1 N1 C79 C78 180.0(2) . . . . ? C77 C78 C79 N1 -0.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.823 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.072 #===END data_bc417 _database_code_CSD 196428 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (2,6-Trip2C6H3CS2)2VCl(py)2a2py _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C94 H118 Cl N4 S4 V' _chemical_formula_weight 1518.55 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.648(2) _cell_length_b 13.5721(13) _cell_length_c 29.404(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.288(2) _cell_angle_gamma 90.00 _cell_volume 8718.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 135(2) _cell_measurement_reflns_used 5363 _cell_measurement_theta_min 2.354 _cell_measurement_theta_max 24.658 _exptl_crystal_description ? _exptl_crystal_colour purple _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3256 _exptl_absorpt_coefficient_mu 0.286 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.846 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51, 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 135(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD detector' _diffrn_measurement_method '/w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 85590 _diffrn_reflns_av_R_equivalents 0.117 _diffrn_reflns_av_sigmaI/netI 0.0906 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 26.37 _reflns_number_total 17808 _reflns_number_gt 10633 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17808 _refine_ls_number_parameters 850 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1042 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1456 _refine_ls_wR_factor_gt 0.1300 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.979 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.20372(2) 0.48974(3) 0.025656(16) 0.02371(12) Uani 1 1 d . . . S1 S 0.23330(3) 0.43875(5) -0.04859(3) 0.02758(17) Uani 1 1 d . . . S2 S 0.15476(3) 0.59762(5) -0.04525(2) 0.02739(17) Uani 1 1 d . . . S3 S 0.30007(3) 0.38506(5) 0.05270(3) 0.02948(17) Uani 1 1 d . . . S4 S 0.21452(3) 0.41104(5) 0.10574(3) 0.03065(17) Uani 1 1 d . . . Cl1 Cl 0.13289(3) 0.58391(5) 0.05638(3) 0.03126(17) Uani 1 1 d . . . N1 N 0.13481(10) 0.37826(16) 0.00191(8) 0.0273(5) Uani 1 1 d . . . N2 N 0.26801(11) 0.60916(16) 0.04930(9) 0.0304(6) Uani 1 1 d . . . C1 C 0.18677(11) 0.52652(19) -0.07851(10) 0.0233(6) Uani 1 1 d . . . C2 C 0.17424(12) 0.54169(18) -0.13014(10) 0.0226(6) Uani 1 1 d . . . C3 C 0.11863(12) 0.50929(19) -0.16079(10) 0.0248(6) Uani 1 1 d . . . C4 C 0.10688(13) 0.5306(2) -0.20870(10) 0.0295(7) Uani 1 1 d . . . H4 H 0.0692 0.5099 -0.2294 0.035 Uiso 1 1 calc R . . C5 C 0.14845(13) 0.5810(2) -0.22703(10) 0.0313(7) Uani 1 1 d . . . H5 H 0.1391 0.5964 -0.2597 0.038 Uiso 1 1 calc R . . C6 C 0.20379(13) 0.6087(2) -0.19703(10) 0.0296(7) Uani 1 1 d . . . H6 H 0.2330 0.6417 -0.2096 0.036 Uiso 1 1 calc R . . C7 C 0.21788(12) 0.58950(19) -0.14887(10) 0.0251(6) Uani 1 1 d . . . C8 C 0.07327(12) 0.44264(19) -0.14683(9) 0.0240(6) Uani 1 1 d . . . C9 C 0.08026(12) 0.3404(2) -0.15112(10) 0.0277(6) Uani 1 1 d . . . C10 C 0.03285(13) 0.2777(2) -0.14696(10) 0.0314(7) Uani 1 1 d . . . H10 H 0.0375 0.2086 -0.1498 0.038 Uiso 1 1 calc R . . C11 C -0.02070(13) 0.3136(2) -0.13881(10) 0.0293(6) Uani 1 1 d . . . C12 C -0.02562(13) 0.4150(2) -0.13330(10) 0.0283(6) Uani 1 1 d . . . H12 H -0.0614 0.4404 -0.1264 0.034 Uiso 1 1 calc R . . C13 C 0.01979(12) 0.4803(2) -0.13758(9) 0.0249(6) Uani 1 1 d . . . C14 C 0.13652(13) 0.2964(2) -0.16223(11) 0.0335(7) Uani 1 1 d . . . H14 H 0.1679 0.3498 -0.1583 0.040 Uiso 1 1 calc R . . C15 C 0.16505(14) 0.2119(2) -0.12918(13) 0.0452(9) Uani 1 1 d . . . H15A H 0.1755 0.2352 -0.0965 0.068 Uiso 1 1 calc R . . H15B H 0.2022 0.1890 -0.1370 0.068 Uiso 1 1 calc R . . H15C H 0.1357 0.1575 -0.1329 0.068 Uiso 1 1 calc R . . C16 C 0.12092(16) 0.2628(3) -0.21355(12) 0.0479(9) Uani 1 1 d . . . H16A H 0.0931 0.2063 -0.2178 0.072 Uiso 1 1 calc R . . H16B H 0.1585 0.2437 -0.2218 0.072 Uiso 1 1 calc R . . H16C H 0.1011 0.3169 -0.2340 0.072 Uiso 1 1 calc R . . C17 C -0.07307(13) 0.2466(2) -0.13445(11) 0.0339(7) Uani 1 1 d . . . H17 H -0.0778 0.2555 -0.1018 0.041 Uiso 1 1 calc R . . C18 C -0.06097(15) 0.1376(2) -0.14008(13) 0.0440(8) Uani 1 1 d . . . H18A H -0.0556 0.1257 -0.1716 0.066 Uiso 1 1 calc R . . H18B H -0.0958 0.0989 -0.1360 0.066 Uiso 1 1 calc R . . H18C H -0.0238 0.1178 -0.1163 0.066 Uiso 1 1 calc R . . C19 C -0.13400(14) 0.2760(2) -0.16844(13) 0.0454(9) Uani 1 1 d . . . H19A H -0.1316 0.2671 -0.2010 0.068 Uiso 1 1 calc R . . H19B H -0.1427 0.3452 -0.1633 0.068 Uiso 1 1 calc R . . H19C H -0.1668 0.2344 -0.1628 0.068 Uiso 1 1 calc R . . C20 C 0.01025(13) 0.5901(2) -0.13388(10) 0.0289(6) Uani 1 1 d . . . H20 H 0.0510 0.6226 -0.1295 0.035 Uiso 1 1 calc R . . C21 C -0.01378(14) 0.6185(2) -0.09197(11) 0.0344(7) Uani 1 1 d . . . H21A H -0.0543 0.5892 -0.0956 0.052 Uiso 1 1 calc R . . H21B H -0.0168 0.6904 -0.0905 0.052 Uiso 1 1 calc R . . H21C H 0.0143 0.5942 -0.0629 0.052 Uiso 1 1 calc R . . C22 C -0.03207(14) 0.6301(2) -0.17963(12) 0.0397(8) Uani 1 1 d . . . H22A H -0.0145 0.6157 -0.2060 0.060 Uiso 1 1 calc R . . H22B H -0.0365 0.7015 -0.1769 0.060 Uiso 1 1 calc R . . H22C H -0.0723 0.5986 -0.1853 0.060 Uiso 1 1 calc R . . C23 C 0.28078(12) 0.6189(2) -0.12010(10) 0.0272(6) Uani 1 1 d . . . C24 C 0.29240(13) 0.7172(2) -0.10540(10) 0.0306(7) Uani 1 1 d . . . C25 C 0.35218(14) 0.7440(2) -0.08215(11) 0.0380(8) Uani 1 1 d . . . H25 H 0.3603 0.8106 -0.0726 0.046 Uiso 1 1 calc R . . C26 C 0.39961(14) 0.6779(3) -0.07260(11) 0.0399(8) Uani 1 1 d . . . C27 C 0.38714(13) 0.5810(2) -0.08746(11) 0.0395(8) Uani 1 1 d . . . H27 H 0.4197 0.5346 -0.0809 0.047 Uiso 1 1 calc R . . C28 C 0.32873(13) 0.5496(2) -0.11162(10) 0.0305(7) Uani 1 1 d . . . C29 C 0.24228(14) 0.7946(2) -0.11580(11) 0.0344(7) Uani 1 1 d . . . H29 H 0.2021 0.7592 -0.1250 0.041 Uiso 1 1 calc R . . C30 C 0.24240(18) 0.8586(3) -0.07309(12) 0.0519(9) Uani 1 1 d . . . H30A H 0.2387 0.8166 -0.0469 0.078 Uiso 1 1 calc R . . H30B H 0.2078 0.9045 -0.0812 0.078 Uiso 1 1 calc R . . H30C H 0.2808 0.8959 -0.0638 0.078 Uiso 1 1 calc R . . C31 C 0.24605(17) 0.8600(3) -0.15740(12) 0.0509(9) Uani 1 1 d . . . H31A H 0.2856 0.8940 -0.1499 0.076 Uiso 1 1 calc R . . H31B H 0.2129 0.9086 -0.1634 0.076 Uiso 1 1 calc R . . H31C H 0.2420 0.8190 -0.1855 0.076 Uiso 1 1 calc R . . C32 C 0.46383(15) 0.7107(3) -0.04672(14) 0.0568(10) Uani 1 1 d . . . H32 H 0.4586 0.7792 -0.0359 0.068 Uiso 1 1 calc R . . C33 C 0.4900(2) 0.6555(4) -0.00343(17) 0.0948(17) Uani 1 1 d . . . H33A H 0.4948 0.5863 -0.0112 0.142 Uiso 1 1 calc R . . H33B H 0.4627 0.6601 0.0174 0.142 Uiso 1 1 calc R . . H33C H 0.5301 0.6832 0.0126 0.142 Uiso 1 1 calc R . . C34 C 0.50437(16) 0.7217(3) -0.07897(15) 0.0656(12) Uani 1 1 d . . . H34A H 0.5459 0.7387 -0.0606 0.098 Uiso 1 1 calc R . . H34B H 0.4885 0.7741 -0.1018 0.098 Uiso 1 1 calc R . . H34C H 0.5054 0.6596 -0.0957 0.098 Uiso 1 1 calc R . . C35 C 0.31799(13) 0.4449(2) -0.13059(11) 0.0352(7) Uani 1 1 d . . . H35 H 0.2743 0.4282 -0.1329 0.042 Uiso 1 1 calc R . . C36 C 0.35737(15) 0.3682(3) -0.09888(13) 0.0509(9) Uani 1 1 d . . . H36A H 0.4000 0.3757 -0.0999 0.076 Uiso 1 1 calc R . . H36B H 0.3428 0.3021 -0.1098 0.076 Uiso 1 1 calc R . . H36C H 0.3546 0.3773 -0.0664 0.076 Uiso 1 1 calc R . . C37 C 0.32669(15) 0.4386(2) -0.18029(12) 0.0436(8) Uani 1 1 d . . . H37A H 0.2994 0.4857 -0.2008 0.065 Uiso 1 1 calc R . . H37B H 0.3170 0.3717 -0.1926 0.065 Uiso 1 1 calc R . . H37C H 0.3693 0.4542 -0.1793 0.065 Uiso 1 1 calc R . . C38 C 0.28004(13) 0.35994(19) 0.10260(10) 0.0271(6) Uani 1 1 d . . . C39 C 0.32024(12) 0.29758(19) 0.13960(10) 0.0263(6) Uani 1 1 d . . . C40 C 0.35937(13) 0.3415(2) 0.17958(10) 0.0299(7) Uani 1 1 d . . . C41 C 0.40199(14) 0.2826(2) 0.21091(12) 0.0404(8) Uani 1 1 d . . . H41 H 0.4291 0.3119 0.2377 0.049 Uiso 1 1 calc R . . C42 C 0.40535(15) 0.1825(2) 0.20356(12) 0.0452(9) Uani 1 1 d . . . H42 H 0.4360 0.1440 0.2243 0.054 Uiso 1 1 calc R . . C43 C 0.36414(14) 0.1388(2) 0.16617(12) 0.0399(8) Uani 1 1 d . . . H43 H 0.3653 0.0694 0.1622 0.048 Uiso 1 1 calc R . . C44 C 0.32071(13) 0.1942(2) 0.13400(10) 0.0302(7) Uani 1 1 d . . . C45 C 0.35749(13) 0.4490(2) 0.19144(10) 0.0316(7) Uani 1 1 d . . . C46 C 0.31724(14) 0.4806(2) 0.21757(10) 0.0351(7) Uani 1 1 d . . . C47 C 0.32092(15) 0.5775(2) 0.23314(11) 0.0404(8) Uani 1 1 d . . . H47 H 0.2936 0.5993 0.2506 0.049 Uiso 1 1 calc R . . C48 C 0.36320(17) 0.6438(2) 0.22402(12) 0.0459(9) Uani 1 1 d . A . C49 C 0.40127(15) 0.6115(2) 0.19760(11) 0.0379(8) Uani 1 1 d . . . H49 H 0.4300 0.6561 0.1907 0.046 Uiso 1 1 calc R . . C50 C 0.39904(13) 0.5154(2) 0.18075(10) 0.0331(7) Uani 1 1 d . . . C51 C 0.27242(13) 0.4106(2) 0.23124(11) 0.0359(7) Uani 1 1 d . . . H51 H 0.2657 0.3538 0.2088 0.043 Uiso 1 1 calc R . . C52 C 0.30013(17) 0.3694(3) 0.28113(13) 0.0545(10) Uani 1 1 d . . . H52A H 0.3396 0.3383 0.2825 0.082 Uiso 1 1 calc R . . H52B H 0.2722 0.3205 0.2886 0.082 Uiso 1 1 calc R . . H52C H 0.3062 0.4233 0.3041 0.082 Uiso 1 1 calc R . . C53 C 0.21015(15) 0.4562(2) 0.22861(12) 0.0444(8) Uani 1 1 d . . . H53A H 0.2145 0.5064 0.2532 0.067 Uiso 1 1 calc R . . H53B H 0.1819 0.4048 0.2333 0.067 Uiso 1 1 calc R . . H53C H 0.1939 0.4867 0.1976 0.067 Uiso 1 1 calc R . . C54 C 0.3661(2) 0.7495(3) 0.24363(14) 0.0662(12) Uani 1 1 d . . . C55 C 0.4018(4) 0.7379(6) 0.3000(3) 0.070(2) Uiso 0.627(9) 1 d P A 1 C56 C 0.3085(3) 0.7984(4) 0.2314(2) 0.056(2) Uiso 0.627(9) 1 d P A 1 C55' C 0.3766(5) 0.7584(6) 0.2949(3) 0.029(2) Uiso 0.373(9) 1 d P A 2 C56' C 0.3904(5) 0.8303(8) 0.2212(4) 0.060(4) Uiso 0.373(9) 1 d P A 2 C57 C 0.44322(14) 0.4838(2) 0.15288(11) 0.0370(7) Uani 1 1 d . . . H57 H 0.4307 0.4166 0.1400 0.044 Uiso 1 1 calc R . . C58 C 0.50861(16) 0.4766(3) 0.18432(14) 0.0619(11) Uani 1 1 d . . . H58A H 0.5222 0.5418 0.1973 0.093 Uiso 1 1 calc R . . H58B H 0.5358 0.4530 0.1657 0.093 Uiso 1 1 calc R . . H58C H 0.5098 0.4305 0.2102 0.093 Uiso 1 1 calc R . . C59 C 0.44109(16) 0.5526(3) 0.11081(12) 0.0474(9) Uani 1 1 d . . . H59A H 0.3994 0.5542 0.0901 0.071 Uiso 1 1 calc R . . H59B H 0.4692 0.5281 0.0931 0.071 Uiso 1 1 calc R . . H59C H 0.4533 0.6191 0.1224 0.071 Uiso 1 1 calc R . . C60 C 0.27260(12) 0.13858(19) 0.09815(10) 0.0277(6) Uani 1 1 d . . . C61 C 0.28265(13) 0.1037(2) 0.05611(11) 0.0310(7) Uani 1 1 d . . . C62 C 0.23990(13) 0.0400(2) 0.02796(11) 0.0320(7) Uani 1 1 d . . . H62 H 0.2469 0.0160 -0.0005 0.038 Uiso 1 1 calc R . . C63 C 0.18715(13) 0.01034(19) 0.04024(11) 0.0297(7) Uani 1 1 d . . . C64 C 0.17800(13) 0.0475(2) 0.08175(11) 0.0312(7) Uani 1 1 d . . . H64 H 0.1421 0.0287 0.0906 0.037 Uiso 1 1 calc R . . C65 C 0.21896(13) 0.11088(19) 0.11090(10) 0.0297(7) Uani 1 1 d . . . C66 C 0.33995(14) 0.1304(2) 0.04142(12) 0.0377(8) Uani 1 1 d . . . H66 H 0.3599 0.1871 0.0613 0.045 Uiso 1 1 calc R . . C67 C 0.38524(15) 0.0443(3) 0.05067(14) 0.0533(10) Uani 1 1 d . . . H67A H 0.3963 0.0279 0.0843 0.080 Uiso 1 1 calc R . . H67B H 0.4221 0.0630 0.0413 0.080 Uiso 1 1 calc R . . H67C H 0.3663 -0.0131 0.0323 0.080 Uiso 1 1 calc R . . C68 C 0.32638(16) 0.1621(2) -0.01002(12) 0.0452(8) Uani 1 1 d . . . H68A H 0.3103 0.1059 -0.0304 0.068 Uiso 1 1 calc R . . H68B H 0.3641 0.1857 -0.0167 0.068 Uiso 1 1 calc R . . H68C H 0.2960 0.2152 -0.0160 0.068 Uiso 1 1 calc R . . C69 C 0.14441(14) -0.0644(2) 0.01014(12) 0.0356(7) Uani 1 1 d . . . H69 H 0.1489 -0.0591 -0.0227 0.043 Uiso 1 1 calc R . . C70 C 0.16294(17) -0.1686(2) 0.02772(13) 0.0500(9) Uani 1 1 d . . . H70A H 0.2057 -0.1802 0.0278 0.075 Uiso 1 1 calc R . . H70B H 0.1366 -0.2164 0.0068 0.075 Uiso 1 1 calc R . . H70C H 0.1584 -0.1761 0.0598 0.075 Uiso 1 1 calc R . . C71 C 0.07679(15) -0.0490(2) 0.00786(14) 0.0524(10) Uani 1 1 d . . . H71A H 0.0699 -0.0641 0.0386 0.079 Uiso 1 1 calc R . . H71B H 0.0517 -0.0927 -0.0161 0.079 Uiso 1 1 calc R . . H71C H 0.0655 0.0197 -0.0004 0.079 Uiso 1 1 calc R . . C72 C 0.20647(15) 0.1453(2) 0.15680(11) 0.0385(8) Uani 1 1 d . . . H72 H 0.2345 0.2016 0.1692 0.046 Uiso 1 1 calc R . . C73 C 0.22120(18) 0.0619(3) 0.19328(12) 0.0547(10) Uani 1 1 d . . . H73A H 0.1958 0.0044 0.1811 0.082 Uiso 1 1 calc R . . H73B H 0.2127 0.0840 0.2227 0.082 Uiso 1 1 calc R . . H73C H 0.2645 0.0440 0.1994 0.082 Uiso 1 1 calc R . . C74 C 0.14101(16) 0.1808(3) 0.15005(13) 0.0526(9) Uani 1 1 d . . . H74A H 0.1315 0.2312 0.1253 0.079 Uiso 1 1 calc R . . H74B H 0.1365 0.2088 0.1797 0.079 Uiso 1 1 calc R . . H74C H 0.1128 0.1251 0.1408 0.079 Uiso 1 1 calc R . . C75 C 0.15067(13) 0.2839(2) -0.00144(11) 0.0343(7) Uani 1 1 d . . . H75 H 0.1930 0.2678 0.0064 0.041 Uiso 1 1 calc R . . C76 C 0.10891(15) 0.2093(2) -0.01564(12) 0.0446(9) Uani 1 1 d . . . H76 H 0.1221 0.1437 -0.0183 0.053 Uiso 1 1 calc R . . C77 C 0.04715(15) 0.2318(2) -0.02595(12) 0.0443(9) Uani 1 1 d . . . H77 H 0.0172 0.1815 -0.0350 0.053 Uiso 1 1 calc R . . C78 C 0.03004(14) 0.3279(2) -0.02290(11) 0.0373(7) Uani 1 1 d . . . H78 H -0.0120 0.3454 -0.0299 0.045 Uiso 1 1 calc R . . C79 C 0.07476(13) 0.3990(2) -0.00949(10) 0.0324(7) Uani 1 1 d . . . H79 H 0.0625 0.4656 -0.0083 0.039 Uiso 1 1 calc R . . C80 C 0.27430(16) 0.6508(2) 0.09162(11) 0.0409(8) Uani 1 1 d . . . H80 H 0.2530 0.6231 0.1124 0.049 Uiso 1 1 calc R . . C81 C 0.31076(19) 0.7328(2) 0.10599(13) 0.0572(11) Uani 1 1 d . . . H81 H 0.3146 0.7602 0.1364 0.069 Uiso 1 1 calc R . . C82 C 0.34104(18) 0.7740(3) 0.07665(13) 0.0573(11) Uani 1 1 d . . . H82 H 0.3651 0.8316 0.0858 0.069 Uiso 1 1 calc R . . C83 C 0.33632(15) 0.7310(2) 0.03338(13) 0.0482(9) Uani 1 1 d . . . H83 H 0.3579 0.7570 0.0124 0.058 Uiso 1 1 calc R . . C84 C 0.29949(13) 0.6492(2) 0.02137(11) 0.0354(7) Uani 1 1 d . . . H84 H 0.2963 0.6196 -0.0085 0.042 Uiso 1 1 calc R . . 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 V1 0.0237(2) 0.0260(2) 0.0216(3) 0.0003(2) 0.0063(2) -0.00009(19) S1 0.0273(4) 0.0317(4) 0.0237(4) 0.0023(3) 0.0067(3) 0.0046(3) S2 0.0285(4) 0.0315(4) 0.0221(4) -0.0001(3) 0.0065(3) 0.0029(3) S3 0.0258(4) 0.0348(4) 0.0270(4) 0.0041(3) 0.0055(3) 0.0007(3) S4 0.0312(4) 0.0341(4) 0.0272(4) 0.0040(3) 0.0087(3) 0.0033(3) Cl1 0.0352(4) 0.0319(4) 0.0303(4) 0.0022(3) 0.0150(3) 0.0067(3) N1 0.0254(13) 0.0307(12) 0.0259(13) 0.0019(10) 0.0067(11) 0.0004(10) N2 0.0340(14) 0.0273(12) 0.0281(14) 0.0029(11) 0.0051(12) -0.0006(10) C1 0.0147(13) 0.0305(14) 0.0255(15) 0.0007(12) 0.0064(12) -0.0045(11) C2 0.0192(14) 0.0256(13) 0.0236(15) -0.0006(11) 0.0065(12) 0.0010(11) C3 0.0223(14) 0.0265(14) 0.0257(15) 0.0018(12) 0.0065(13) 0.0033(11) C4 0.0229(15) 0.0363(16) 0.0279(16) -0.0025(13) 0.0041(13) 0.0011(12) C5 0.0325(16) 0.0401(16) 0.0226(16) 0.0017(13) 0.0096(14) 0.0028(13) C6 0.0274(15) 0.0358(16) 0.0278(16) 0.0012(13) 0.0108(14) -0.0020(13) C7 0.0230(14) 0.0291(14) 0.0238(15) -0.0008(12) 0.0071(12) 0.0005(12) C8 0.0207(14) 0.0310(14) 0.0185(14) -0.0027(12) 0.0023(12) -0.0029(11) C9 0.0240(15) 0.0342(15) 0.0240(16) -0.0031(12) 0.0047(13) -0.0024(12) C10 0.0334(17) 0.0294(15) 0.0298(17) -0.0036(13) 0.0057(14) -0.0019(13) C11 0.0275(15) 0.0355(16) 0.0248(16) -0.0014(13) 0.0068(13) -0.0036(13) C12 0.0224(14) 0.0365(15) 0.0263(16) -0.0013(13) 0.0070(13) -0.0006(12) C13 0.0216(14) 0.0337(15) 0.0179(14) -0.0028(12) 0.0027(12) -0.0010(12) C14 0.0276(16) 0.0316(15) 0.0420(19) -0.0074(14) 0.0107(15) 0.0008(13) C15 0.0325(18) 0.0444(19) 0.057(2) -0.0014(17) 0.0096(17) 0.0047(15) C16 0.047(2) 0.056(2) 0.044(2) -0.0112(17) 0.0181(18) 0.0096(17) C17 0.0291(16) 0.0398(17) 0.0341(18) -0.0047(14) 0.0107(15) -0.0090(13) C18 0.0390(19) 0.0405(18) 0.051(2) -0.0035(16) 0.0086(17) -0.0137(15) C19 0.0311(17) 0.0490(19) 0.054(2) -0.0003(17) 0.0080(17) -0.0111(15) C20 0.0226(15) 0.0319(15) 0.0329(17) -0.0009(13) 0.0086(13) 0.0015(12) C21 0.0311(16) 0.0355(16) 0.0375(18) -0.0057(14) 0.0108(15) 0.0036(13) C22 0.0297(17) 0.0435(18) 0.043(2) 0.0026(15) 0.0049(16) 0.0053(14) C23 0.0230(15) 0.0374(16) 0.0218(15) 0.0003(12) 0.0071(13) -0.0060(12) C24 0.0299(16) 0.0396(16) 0.0246(16) -0.0009(13) 0.0108(14) -0.0080(13) C25 0.0373(18) 0.0450(18) 0.0318(19) -0.0029(14) 0.0093(16) -0.0128(15) C26 0.0293(17) 0.059(2) 0.0300(18) -0.0010(16) 0.0051(15) -0.0169(16) C27 0.0219(16) 0.061(2) 0.0351(19) 0.0034(16) 0.0072(14) -0.0028(15) C28 0.0248(15) 0.0423(17) 0.0251(16) 0.0017(13) 0.0078(13) -0.0033(13) C29 0.0374(17) 0.0369(16) 0.0322(18) 0.0008(14) 0.0149(15) -0.0035(14) C30 0.068(2) 0.049(2) 0.043(2) -0.0085(17) 0.022(2) 0.0017(18) C31 0.063(2) 0.050(2) 0.046(2) 0.0101(17) 0.024(2) 0.0009(18) C32 0.0319(19) 0.081(3) 0.052(2) 0.001(2) 0.0012(18) -0.0162(18) C33 0.050(3) 0.149(5) 0.068(3) 0.022(3) -0.017(2) -0.032(3) C34 0.0310(19) 0.095(3) 0.073(3) -0.008(2) 0.016(2) -0.024(2) C35 0.0225(15) 0.0427(17) 0.0415(19) 0.0004(15) 0.0101(14) 0.0038(13) C36 0.0370(19) 0.055(2) 0.060(2) 0.0080(18) 0.0111(18) 0.0110(16) C37 0.0426(19) 0.0496(19) 0.040(2) -0.0070(16) 0.0139(17) -0.0004(16) C38 0.0268(15) 0.0258(14) 0.0266(16) -0.0032(12) 0.0030(13) -0.0065(12) C39 0.0215(14) 0.0301(14) 0.0256(16) 0.0040(12) 0.0033(13) -0.0034(12) C40 0.0245(15) 0.0356(16) 0.0278(17) 0.0058(13) 0.0035(13) -0.0037(13) C41 0.0307(17) 0.0493(19) 0.0331(19) 0.0069(15) -0.0061(15) -0.0042(15) C42 0.0392(19) 0.0458(19) 0.039(2) 0.0161(16) -0.0094(16) 0.0041(16) C43 0.0379(18) 0.0378(17) 0.039(2) 0.0061(15) 0.0020(16) 0.0005(14) C44 0.0294(16) 0.0334(15) 0.0262(16) 0.0044(13) 0.0045(14) 0.0013(13) C45 0.0262(15) 0.0409(16) 0.0228(16) -0.0020(13) -0.0024(13) -0.0052(13) C46 0.0354(17) 0.0416(17) 0.0258(17) -0.0005(14) 0.0038(14) -0.0094(14) C47 0.048(2) 0.0409(17) 0.0346(19) -0.0078(14) 0.0154(16) -0.0119(15) C48 0.058(2) 0.0475(19) 0.0321(19) -0.0085(15) 0.0116(18) -0.0161(17) C49 0.0402(18) 0.0402(17) 0.0330(18) -0.0022(14) 0.0089(16) -0.0137(14) C50 0.0297(16) 0.0430(17) 0.0252(16) 0.0026(14) 0.0049(14) -0.0080(14) C51 0.0320(17) 0.0436(17) 0.0313(18) -0.0012(14) 0.0070(15) -0.0093(14) C52 0.050(2) 0.061(2) 0.054(2) 0.0185(19) 0.0171(19) -0.0089(18) C53 0.0404(19) 0.0500(19) 0.044(2) -0.0005(16) 0.0137(17) -0.0081(16) C54 0.108(4) 0.045(2) 0.052(2) -0.0129(18) 0.033(3) -0.034(2) C57 0.0321(17) 0.0416(17) 0.0377(19) 0.0024(15) 0.0098(15) -0.0047(14) C58 0.036(2) 0.098(3) 0.049(2) 0.011(2) 0.0068(19) 0.001(2) C59 0.048(2) 0.055(2) 0.042(2) 0.0034(17) 0.0163(18) -0.0030(17) C60 0.0242(15) 0.0251(14) 0.0314(17) 0.0050(12) 0.0029(13) -0.0012(12) C61 0.0274(15) 0.0301(15) 0.0373(18) 0.0041(13) 0.0117(14) -0.0004(12) C62 0.0340(17) 0.0308(15) 0.0332(18) -0.0013(13) 0.0121(15) -0.0018(13) C63 0.0307(16) 0.0231(14) 0.0367(18) 0.0007(13) 0.0112(14) 0.0003(12) C64 0.0280(16) 0.0304(15) 0.0379(18) 0.0072(13) 0.0132(15) -0.0003(12) C65 0.0323(16) 0.0261(14) 0.0306(17) 0.0052(13) 0.0079(14) 0.0003(12) C66 0.0301(16) 0.0358(16) 0.050(2) -0.0003(15) 0.0163(16) -0.0070(13) C67 0.0344(19) 0.056(2) 0.073(3) 0.006(2) 0.0210(19) 0.0028(16) C68 0.047(2) 0.0484(19) 0.047(2) -0.0012(16) 0.0257(18) -0.0080(16) C69 0.0362(17) 0.0311(16) 0.0412(19) -0.0040(14) 0.0133(16) -0.0053(13) C70 0.064(2) 0.0288(17) 0.055(2) -0.0050(16) 0.013(2) -0.0055(16) C71 0.0369(19) 0.0421(19) 0.079(3) -0.0077(18) 0.016(2) -0.0130(15) C72 0.0437(19) 0.0407(17) 0.0346(19) -0.0029(14) 0.0165(16) -0.0060(15) C73 0.059(2) 0.069(2) 0.038(2) 0.0118(18) 0.0179(19) -0.005(2) C74 0.055(2) 0.057(2) 0.054(2) -0.0077(18) 0.029(2) 0.0037(18) C75 0.0263(16) 0.0315(16) 0.041(2) 0.0058(14) 0.0022(14) -0.0014(13) C76 0.0404(19) 0.0316(16) 0.054(2) 0.0072(15) -0.0010(17) -0.0050(14) C77 0.0359(19) 0.0469(19) 0.044(2) 0.0099(16) -0.0002(16) -0.0161(15) C78 0.0234(16) 0.059(2) 0.0280(18) -0.0003(15) 0.0042(14) -0.0035(15) C79 0.0262(16) 0.0439(17) 0.0276(17) 0.0008(14) 0.0077(14) 0.0020(14) C80 0.057(2) 0.0340(16) 0.0265(18) -0.0005(14) 0.0017(16) -0.0029(15) C81 0.092(3) 0.0383(19) 0.030(2) -0.0039(16) -0.004(2) -0.0095(19) C82 0.073(3) 0.0406(19) 0.044(2) 0.0034(17) -0.011(2) -0.0234(18) C83 0.0414(19) 0.052(2) 0.042(2) 0.0084(17) -0.0041(17) -0.0183(17) C84 0.0329(17) 0.0381(17) 0.0309(18) -0.0001(14) 0.0009(15) -0.0049(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 N1 2.154(2) . ? V1 N2 2.167(2) . ? V1 Cl1 2.4056(8) . ? V1 S4 2.5380(9) . ? V1 S1 2.5425(9) . ? V1 S3 2.5489(9) . ? V1 S2 2.5498(8) . ? S1 C1 1.678(3) . ? S2 C1 1.669(3) . ? S3 C38 1.681(3) . ? S4 C38 1.662(3) . ? N1 C75 1.341(3) . ? N1 C79 1.342(4) . ? N2 C84 1.337(4) . ? N2 C80 1.339(4) . ? C1 C2 1.483(4) . ? C2 C7 1.410(4) . ? C2 C3 1.412(4) . ? C3 C4 1.393(4) . ? C3 C8 1.505(4) . ? C4 C5 1.383(4) . ? C5 C6 1.381(4) . ? C6 C7 1.392(4) . ? C7 C23 1.506(4) . ? C8 C13 1.406(4) . ? C8 C9 1.406(4) . ? C9 C10 1.400(4) . ? C9 C14 1.518(4) . ? C10 C11 1.385(4) . ? C11 C12 1.394(4) . ? C11 C17 1.527(4) . ? C12 C13 1.388(4) . ? C13 C20 1.514(4) . ? C14 C16 1.526(4) . ? C14 C15 1.532(4) . ? C17 C18 1.522(4) . ? C17 C19 1.528(4) . ? C20 C21 1.522(4) . ? C20 C22 1.531(4) . ? C23 C24 1.405(4) . ? C23 C28 1.409(4) . ? C24 C25 1.395(4) . ? C24 C29 1.518(4) . ? C25 C26 1.370(4) . ? C26 C27 1.391(4) . ? C26 C32 1.519(4) . ? C27 C28 1.393(4) . ? C28 C35 1.522(4) . ? C29 C30 1.526(4) . ? C29 C31 1.532(4) . ? C32 C33 1.461(6) . ? C32 C34 1.491(5) . ? C35 C36 1.520(4) . ? C35 C37 1.528(4) . ? C38 C39 1.485(4) . ? C39 C40 1.404(4) . ? C39 C44 1.413(4) . ? C40 C41 1.396(4) . ? C40 C45 1.504(4) . ? C41 C42 1.381(4) . ? C42 C43 1.375(4) . ? C43 C44 1.391(4) . ? C44 C60 1.504(4) . ? C45 C50 1.397(4) . ? C45 C46 1.405(4) . ? C46 C47 1.388(4) . ? C46 C51 1.520(4) . ? C47 C48 1.390(4) . ? C48 C49 1.376(5) . ? C48 C54 1.541(5) . ? C49 C50 1.391(4) . ? C50 C57 1.513(4) . ? C51 C53 1.523(4) . ? C51 C52 1.540(5) . ? C54 C56 1.423(7) . ? C54 C56' 1.460(11) . ? C54 C55' 1.468(9) . ? C54 C55 1.647(9) . ? C57 C58 1.528(5) . ? C57 C59 1.540(4) . ? C60 C61 1.397(4) . ? C60 C65 1.413(4) . ? C61 C62 1.396(4) . ? C61 C66 1.516(4) . ? C62 C63 1.395(4) . ? C63 C64 1.386(4) . ? C63 C69 1.516(4) . ? C64 C65 1.384(4) . ? C65 C72 1.524(4) . ? C66 C68 1.524(4) . ? C66 C67 1.531(4) . ? C69 C70 1.526(4) . ? C69 C71 1.530(4) . ? C72 C74 1.521(5) . ? C72 C73 1.534(5) . ? C75 C76 1.373(4) . ? C76 C77 1.385(4) . ? C77 C78 1.371(4) . ? C78 C79 1.378(4) . ? C80 C81 1.384(4) . ? C81 C82 1.356(5) . ? C82 C83 1.378(5) . ? C83 C84 1.378(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 V1 N2 176.05(9) . . ? N1 V1 Cl1 89.83(6) . . ? N2 V1 Cl1 86.58(7) . . ? N1 V1 S4 83.65(6) . . ? N2 V1 S4 97.17(7) . . ? Cl1 V1 S4 77.64(3) . . ? N1 V1 S1 82.12(7) . . ? N2 V1 S1 99.92(7) . . ? Cl1 V1 S1 145.06(3) . . ? S4 V1 S1 134.37(3) . . ? N1 V1 S3 101.37(6) . . ? N2 V1 S3 82.49(7) . . ? Cl1 V1 S3 141.24(3) . . ? S4 V1 S3 67.10(3) . . ? S1 V1 S3 73.65(3) . . ? N1 V1 S2 90.95(6) . . ? N2 V1 S2 86.76(6) . . ? Cl1 V1 S2 79.21(3) . . ? S4 V1 S2 156.22(3) . . ? S1 V1 S2 67.07(3) . . ? S3 V1 S2 136.64(3) . . ? C1 S1 V1 89.19(10) . . ? C1 S2 V1 89.12(10) . . ? C38 S3 V1 88.83(10) . . ? C38 S4 V1 89.62(10) . . ? C75 N1 C79 117.1(2) . . ? C75 N1 V1 120.63(18) . . ? C79 N1 V1 122.27(19) . . ? C84 N2 C80 117.1(3) . . ? C84 N2 V1 121.9(2) . . ? C80 N2 V1 120.8(2) . . ? C2 C1 S2 121.6(2) . . ? C2 C1 S1 124.0(2) . . ? S2 C1 S1 114.39(16) . . ? C7 C2 C3 119.6(2) . . ? C7 C2 C1 119.9(2) . . ? C3 C2 C1 120.5(2) . . ? C4 C3 C2 118.7(2) . . ? C4 C3 C8 116.0(2) . . ? C2 C3 C8 124.8(2) . . ? C5 C4 C3 121.9(3) . . ? C6 C5 C4 118.8(3) . . ? C5 C6 C7 121.7(3) . . ? C6 C7 C2 119.2(2) . . ? C6 C7 C23 116.8(2) . . ? C2 C7 C23 124.0(2) . . ? C13 C8 C9 120.0(2) . . ? C13 C8 C3 121.3(2) . . ? C9 C8 C3 117.9(2) . . ? C10 C9 C8 119.0(3) . . ? C10 C9 C14 119.1(2) . . ? C8 C9 C14 121.9(2) . . ? C11 C10 C9 121.9(3) . . ? C10 C11 C12 117.9(3) . . ? C10 C11 C17 122.7(3) . . ? C12 C11 C17 119.4(3) . . ? C13 C12 C11 122.4(3) . . ? C12 C13 C8 118.8(2) . . ? C12 C13 C20 119.9(2) . . ? C8 C13 C20 121.2(2) . . ? C9 C14 C16 110.0(2) . . ? C9 C14 C15 113.3(3) . . ? C16 C14 C15 110.6(3) . . ? C18 C17 C11 113.8(2) . . ? C18 C17 C19 109.9(3) . . ? C11 C17 C19 112.2(3) . . ? C13 C20 C21 113.3(2) . . ? C13 C20 C22 110.7(2) . . ? C21 C20 C22 110.3(2) . . ? C24 C23 C28 120.4(3) . . ? C24 C23 C7 119.8(2) . . ? C28 C23 C7 119.5(2) . . ? C25 C24 C23 118.5(3) . . ? C25 C24 C29 119.7(3) . . ? C23 C24 C29 121.7(3) . . ? C26 C25 C24 122.5(3) . . ? C25 C26 C27 118.1(3) . . ? C25 C26 C32 120.4(3) . . ? C27 C26 C32 121.5(3) . . ? C26 C27 C28 122.5(3) . . ? C27 C28 C23 118.0(3) . . ? C27 C28 C35 120.8(3) . . ? C23 C28 C35 121.2(2) . . ? C24 C29 C30 112.9(3) . . ? C24 C29 C31 111.5(3) . . ? C30 C29 C31 109.8(3) . . ? C33 C32 C34 115.4(4) . . ? C33 C32 C26 113.7(3) . . ? C34 C32 C26 112.3(3) . . ? C36 C35 C28 113.8(3) . . ? C36 C35 C37 110.2(3) . . ? C28 C35 C37 110.8(3) . . ? C39 C38 S4 125.5(2) . . ? C39 C38 S3 120.0(2) . . ? S4 C38 S3 114.45(17) . . ? C40 C39 C44 119.8(3) . . ? C40 C39 C38 120.1(2) . . ? C44 C39 C38 120.2(2) . . ? C41 C40 C39 118.9(3) . . ? C41 C40 C45 117.3(3) . . ? C39 C40 C45 123.7(2) . . ? C42 C41 C40 121.1(3) . . ? C43 C42 C41 119.7(3) . . ? C42 C43 C44 121.3(3) . . ? C43 C44 C39 118.8(3) . . ? C43 C44 C60 117.2(2) . . ? C39 C44 C60 123.6(2) . . ? C50 C45 C46 120.0(3) . . ? C50 C45 C40 120.8(3) . . ? C46 C45 C40 119.0(3) . . ? C47 C46 C45 118.6(3) . . ? C47 C46 C51 119.4(3) . . ? C45 C46 C51 121.9(3) . . ? C46 C47 C48 122.3(3) . . ? C49 C48 C47 118.0(3) . . ? C49 C48 C54 122.4(3) . . ? C47 C48 C54 119.6(3) . . ? C48 C49 C50 122.0(3) . . ? C49 C50 C45 119.2(3) . . ? C49 C50 C57 119.4(3) . . ? C45 C50 C57 121.3(3) . . ? C46 C51 C53 114.0(3) . . ? C46 C51 C52 110.2(3) . . ? C53 C51 C52 109.6(3) . . ? C56 C54 C56' 87.9(5) . . ? C56 C54 C55' 96.3(6) . . ? C56' C54 C55' 115.0(6) . . ? C56 C54 C48 113.2(4) . . ? C56' C54 C48 121.0(5) . . ? C55' C54 C48 116.1(4) . . ? C56 C54 C55 118.1(5) . . ? C56' C54 C55 112.5(6) . . ? C55' C54 C55 21.9(4) . . ? C48 C54 C55 104.4(4) . . ? C50 C57 C58 111.4(3) . . ? C50 C57 C59 112.2(3) . . ? C58 C57 C59 110.2(3) . . ? C61 C60 C65 119.8(3) . . ? C61 C60 C44 122.2(2) . . ? C65 C60 C44 117.5(3) . . ? C62 C61 C60 119.0(3) . . ? C62 C61 C66 119.4(3) . . ? C60 C61 C66 121.5(3) . . ? C63 C62 C61 122.2(3) . . ? C64 C63 C62 117.4(3) . . ? C64 C63 C69 122.5(3) . . ? C62 C63 C69 120.0(3) . . ? C65 C64 C63 122.7(3) . . ? C64 C65 C60 118.9(3) . . ? C64 C65 C72 119.2(3) . . ? C60 C65 C72 121.8(3) . . ? C61 C66 C68 112.7(3) . . ? C61 C66 C67 110.5(2) . . ? C68 C66 C67 110.0(3) . . ? C63 C69 C70 110.3(3) . . ? C63 C69 C71 114.3(2) . . ? C70 C69 C71 108.9(3) . . ? C74 C72 C65 112.6(3) . . ? C74 C72 C73 110.5(3) . . ? C65 C72 C73 109.7(3) . . ? N1 C75 C76 123.4(3) . . ? C75 C76 C77 118.6(3) . . ? C78 C77 C76 118.8(3) . . ? C77 C78 C79 119.0(3) . . ? N1 C79 C78 123.0(3) . . ? N2 C80 C81 122.1(3) . . ? C82 C81 C80 119.9(3) . . ? C81 C82 C83 118.9(3) . . ? C84 C83 C82 118.2(3) . . ? N2 C84 C83 123.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 V1 S1 C1 91.48(11) . . . . ? N2 V1 S1 C1 -85.09(11) . . . . ? Cl1 V1 S1 C1 13.22(11) . . . . ? S4 V1 S1 C1 164.53(9) . . . . ? S3 V1 S1 C1 -164.16(9) . . . . ? S2 V1 S1 C1 -2.92(9) . . . . ? N1 V1 S2 C1 -78.09(11) . . . . ? N2 V1 S2 C1 105.13(11) . . . . ? Cl1 V1 S2 C1 -167.74(9) . . . . ? S4 V1 S2 C1 -154.42(11) . . . . ? S1 V1 S2 C1 2.94(9) . . . . ? S3 V1 S2 C1 29.65(10) . . . . ? N1 V1 S3 C38 -78.54(11) . . . . ? N2 V1 S3 C38 100.58(11) . . . . ? Cl1 V1 S3 C38 25.67(11) . . . . ? S4 V1 S3 C38 -0.51(9) . . . . ? S1 V1 S3 C38 -156.73(9) . . . . ? S2 V1 S3 C38 177.71(9) . . . . ? N1 V1 S4 C38 105.72(11) . . . . ? N2 V1 S4 C38 -78.17(11) . . . . ? Cl1 V1 S4 C38 -163.06(10) . . . . ? S1 V1 S4 C38 33.29(10) . . . . ? S3 V1 S4 C38 0.52(9) . . . . ? S2 V1 S4 C38 -176.45(11) . . . . ? N2 V1 N1 C75 -176(24) . . . . ? Cl1 V1 N1 C75 -151.3(2) . . . . ? S4 V1 N1 C75 -73.7(2) . . . . ? S1 V1 N1 C75 62.8(2) . . . . ? S3 V1 N1 C75 -8.7(2) . . . . ? S2 V1 N1 C75 129.5(2) . . . . ? N2 V1 N1 C79 3.1(15) . . . . ? Cl1 V1 N1 C79 27.8(2) . . . . ? S4 V1 N1 C79 105.3(2) . . . . ? S1 V1 N1 C79 -118.1(2) . . . . ? S3 V1 N1 C79 170.4(2) . . . . ? S2 V1 N1 C79 -51.4(2) . . . . ? N1 V1 N2 C84 -106.9(13) . . . . ? Cl1 V1 N2 C84 -131.6(2) . . . . ? S4 V1 N2 C84 151.3(2) . . . . ? S1 V1 N2 C84 13.8(2) . . . . ? S3 V1 N2 C84 85.6(2) . . . . ? S2 V1 N2 C84 -52.3(2) . . . . ? N1 V1 N2 C80 68.0(14) . . . . ? Cl1 V1 N2 C80 43.3(2) . . . . ? S4 V1 N2 C80 -33.8(2) . . . . ? S1 V1 N2 C80 -171.3(2) . . . . ? S3 V1 N2 C80 -99.4(2) . . . . ? S2 V1 N2 C80 122.7(2) . . . . ? V1 S2 C1 C2 175.6(2) . . . . ? V1 S2 C1 S1 -4.50(13) . . . . ? V1 S1 C1 C2 -175.6(2) . . . . ? V1 S1 C1 S2 4.52(13) . . . . ? S2 C1 C2 C7 102.4(3) . . . . ? S1 C1 C2 C7 -77.5(3) . . . . ? S2 C1 C2 C3 -77.1(3) . . . . ? S1 C1 C2 C3 103.0(3) . . . . ? C7 C2 C3 C4 -3.6(4) . . . . ? C1 C2 C3 C4 175.9(2) . . . . ? C7 C2 C3 C8 168.9(2) . . . . ? C1 C2 C3 C8 -11.6(4) . . . . ? C2 C3 C4 C5 1.0(4) . . . . ? C8 C3 C4 C5 -172.2(2) . . . . ? C3 C4 C5 C6 1.7(4) . . . . ? C4 C5 C6 C7 -1.8(4) . . . . ? C5 C6 C7 C2 -0.8(4) . . . . ? C5 C6 C7 C23 177.2(3) . . . . ? C3 C2 C7 C6 3.5(4) . . . . ? C1 C2 C7 C6 -176.0(2) . . . . ? C3 C2 C7 C23 -174.3(2) . . . . ? C1 C2 C7 C23 6.2(4) . . . . ? C4 C3 C8 C13 -86.1(3) . . . . ? C2 C3 C8 C13 101.2(3) . . . . ? C4 C3 C8 C9 83.1(3) . . . . ? C2 C3 C8 C9 -89.6(3) . . . . ? C13 C8 C9 C10 1.2(4) . . . . ? C3 C8 C9 C10 -168.2(3) . . . . ? C13 C8 C9 C14 178.5(3) . . . . ? C3 C8 C9 C14 9.1(4) . . . . ? C8 C9 C10 C11 0.1(4) . . . . ? C14 C9 C10 C11 -177.3(3) . . . . ? C9 C10 C11 C12 -2.0(4) . . . . ? C9 C10 C11 C17 179.6(3) . . . . ? C10 C11 C12 C13 2.6(4) . . . . ? C17 C11 C12 C13 -178.9(3) . . . . ? C11 C12 C13 C8 -1.4(4) . . . . ? C11 C12 C13 C20 176.6(3) . . . . ? C9 C8 C13 C12 -0.6(4) . . . . ? C3 C8 C13 C12 168.4(3) . . . . ? C9 C8 C13 C20 -178.6(3) . . . . ? C3 C8 C13 C20 -9.5(4) . . . . ? C10 C9 C14 C16 72.7(4) . . . . ? C8 C9 C14 C16 -104.6(3) . . . . ? C10 C9 C14 C15 -51.7(4) . . . . ? C8 C9 C14 C15 131.0(3) . . . . ? C10 C11 C17 C18 -0.2(4) . . . . ? C12 C11 C17 C18 -178.6(3) . . . . ? C10 C11 C17 C19 -125.8(3) . . . . ? C12 C11 C17 C19 55.8(4) . . . . ? C12 C13 C20 C21 47.2(4) . . . . ? C8 C13 C20 C21 -134.8(3) . . . . ? C12 C13 C20 C22 -77.3(3) . . . . ? C8 C13 C20 C22 100.6(3) . . . . ? C6 C7 C23 C24 81.5(3) . . . . ? C2 C7 C23 C24 -100.6(3) . . . . ? C6 C7 C23 C28 -93.1(3) . . . . ? C2 C7 C23 C28 84.8(3) . . . . ? C28 C23 C24 C25 -0.3(4) . . . . ? C7 C23 C24 C25 -174.8(3) . . . . ? C28 C23 C24 C29 177.4(3) . . . . ? C7 C23 C24 C29 2.9(4) . . . . ? C23 C24 C25 C26 -0.9(5) . . . . ? C29 C24 C25 C26 -178.7(3) . . . . ? C24 C25 C26 C27 1.0(5) . . . . ? C24 C25 C26 C32 -179.4(3) . . . . ? C25 C26 C27 C28 0.3(5) . . . . ? C32 C26 C27 C28 -179.4(3) . . . . ? C26 C27 C28 C23 -1.5(4) . . . . ? C26 C27 C28 C35 175.2(3) . . . . ? C24 C23 C28 C27 1.4(4) . . . . ? C7 C23 C28 C27 176.0(3) . . . . ? C24 C23 C28 C35 -175.2(3) . . . . ? C7 C23 C28 C35 -0.7(4) . . . . ? C25 C24 C29 C30 -48.0(4) . . . . ? C23 C24 C29 C30 134.4(3) . . . . ? C25 C24 C29 C31 76.2(4) . . . . ? C23 C24 C29 C31 -101.4(3) . . . . ? C25 C26 C32 C33 122.7(4) . . . . ? C27 C26 C32 C33 -57.6(5) . . . . ? C25 C26 C32 C34 -104.0(4) . . . . ? C27 C26 C32 C34 75.7(4) . . . . ? C27 C28 C35 C36 36.3(4) . . . . ? C23 C28 C35 C36 -147.1(3) . . . . ? C27 C28 C35 C37 -88.5(3) . . . . ? C23 C28 C35 C37 88.0(3) . . . . ? V1 S4 C38 C39 178.5(2) . . . . ? V1 S4 C38 S3 -0.79(14) . . . . ? V1 S3 C38 C39 -178.5(2) . . . . ? V1 S3 C38 S4 0.79(14) . . . . ? S4 C38 C39 C40 -78.6(3) . . . . ? S3 C38 C39 C40 100.6(3) . . . . ? S4 C38 C39 C44 103.4(3) . . . . ? S3 C38 C39 C44 -77.4(3) . . . . ? C44 C39 C40 C41 5.8(4) . . . . ? C38 C39 C40 C41 -172.2(3) . . . . ? C44 C39 C40 C45 -173.0(3) . . . . ? C38 C39 C40 C45 9.0(4) . . . . ? C39 C40 C41 C42 -1.2(5) . . . . ? C45 C40 C41 C42 177.8(3) . . . . ? C40 C41 C42 C43 -3.3(5) . . . . ? C41 C42 C43 C44 3.2(5) . . . . ? C42 C43 C44 C39 1.4(5) . . . . ? C42 C43 C44 C60 -172.2(3) . . . . ? C40 C39 C44 C43 -5.9(4) . . . . ? C38 C39 C44 C43 172.0(3) . . . . ? C40 C39 C44 C60 167.3(3) . . . . ? C38 C39 C44 C60 -14.7(4) . . . . ? C41 C40 C45 C50 81.9(4) . . . . ? C39 C40 C45 C50 -99.2(3) . . . . ? C41 C40 C45 C46 -92.0(3) . . . . ? C39 C40 C45 C46 86.9(4) . . . . ? C50 C45 C46 C47 -1.5(4) . . . . ? C40 C45 C46 C47 172.5(3) . . . . ? C50 C45 C46 C51 -178.3(3) . . . . ? C40 C45 C46 C51 -4.4(4) . . . . ? C45 C46 C47 C48 -0.4(5) . . . . ? C51 C46 C47 C48 176.5(3) . . . . ? C46 C47 C48 C49 1.6(5) . . . . ? C46 C47 C48 C54 -178.2(3) . . . . ? C47 C48 C49 C50 -1.0(5) . . . . ? C54 C48 C49 C50 178.8(3) . . . . ? C48 C49 C50 C45 -0.9(5) . . . . ? C48 C49 C50 C57 -178.5(3) . . . . ? C46 C45 C50 C49 2.1(4) . . . . ? C40 C45 C50 C49 -171.7(3) . . . . ? C46 C45 C50 C57 179.7(3) . . . . ? C40 C45 C50 C57 5.9(4) . . . . ? C47 C46 C51 C53 41.7(4) . . . . ? C45 C46 C51 C53 -141.5(3) . . . . ? C47 C46 C51 C52 -82.0(4) . . . . ? C45 C46 C51 C52 94.8(4) . . . . ? C49 C48 C54 C56 126.8(4) . . . . ? C47 C48 C54 C56 -53.5(5) . . . . ? C49 C48 C54 C56' 24.5(8) . . . . ? C47 C48 C54 C56' -155.7(6) . . . . ? C49 C48 C54 C55' -123.2(6) . . . . ? C47 C48 C54 C55' 56.6(7) . . . . ? C49 C48 C54 C55 -103.4(5) . . . . ? C47 C48 C54 C55 76.3(5) . . . . ? C49 C50 C57 C58 70.3(4) . . . . ? C45 C50 C57 C58 -107.3(3) . . . . ? C49 C50 C57 C59 -53.7(4) . . . . ? C45 C50 C57 C59 128.7(3) . . . . ? C43 C44 C60 C61 -84.2(4) . . . . ? C39 C44 C60 C61 102.5(3) . . . . ? C43 C44 C60 C65 87.7(3) . . . . ? C39 C44 C60 C65 -85.7(3) . . . . ? C65 C60 C61 C62 -1.5(4) . . . . ? C44 C60 C61 C62 170.2(3) . . . . ? C65 C60 C61 C66 -179.1(3) . . . . ? C44 C60 C61 C66 -7.5(4) . . . . ? C60 C61 C62 C63 0.4(4) . . . . ? C66 C61 C62 C63 178.1(3) . . . . ? C61 C62 C63 C64 0.6(4) . . . . ? C61 C62 C63 C69 -175.8(3) . . . . ? C62 C63 C64 C65 -0.6(4) . . . . ? C69 C63 C64 C65 175.7(3) . . . . ? C63 C64 C65 C60 -0.4(4) . . . . ? C63 C64 C65 C72 -177.8(3) . . . . ? C61 C60 C65 C64 1.5(4) . . . . ? C44 C60 C65 C64 -170.6(2) . . . . ? C61 C60 C65 C72 178.8(3) . . . . ? C44 C60 C65 C72 6.7(4) . . . . ? C62 C61 C66 C68 48.7(4) . . . . ? C60 C61 C66 C68 -133.7(3) . . . . ? C62 C61 C66 C67 -74.9(4) . . . . ? C60 C61 C66 C67 102.7(3) . . . . ? C64 C63 C69 C70 -86.0(3) . . . . ? C62 C63 C69 C70 90.3(3) . . . . ? C64 C63 C69 C71 37.1(4) . . . . ? C62 C63 C69 C71 -146.6(3) . . . . ? C64 C65 C72 C74 -47.7(4) . . . . ? C60 C65 C72 C74 135.0(3) . . . . ? C64 C65 C72 C73 75.7(3) . . . . ? C60 C65 C72 C73 -101.6(3) . . . . ? C79 N1 C75 C76 -0.1(4) . . . . ? V1 N1 C75 C76 179.0(3) . . . . ? N1 C75 C76 C77 -1.7(5) . . . . ? C75 C76 C77 C78 1.9(5) . . . . ? C76 C77 C78 C79 -0.3(5) . . . . ? C75 N1 C79 C78 1.8(4) . . . . ? V1 N1 C79 C78 -177.3(2) . . . . ? C77 C78 C79 N1 -1.6(5) . . . . ? C84 N2 C80 C81 1.1(5) . . . . ? V1 N2 C80 C81 -174.0(3) . . . . ? N2 C80 C81 C82 0.6(5) . . . . ? C80 C81 C82 C83 -2.1(6) . . . . ? C81 C82 C83 C84 1.8(5) . . . . ? C80 N2 C84 C83 -1.5(4) . . . . ? V1 N2 C84 C83 173.6(2) . . . . ? C82 C83 C84 N2 0.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.539 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.065