Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0186 loop_ _publ_author_name 'Charles Riordan' 'Koyu Fujita' 'Arnold Rheingold' _publ_contact_author_name 'Prof Charles Riordan' _publ_contact_author_address ; Chemistry & Biochemistry University of Delaware Brown Laboratory Newark DE 19716 UNITED STATES OF AMERICA ; _publ_contact_author_email RIORDAN@UDEL.EDU _publ_section_title ; Thioether-ligated nickel(I) complexes for the activation of dioxygen ; data_cgr117 _database_code_CSD 199593 _audit_creation_method SHELXL-97 _chemical_name_systematic ; C38 H56 B S3 Tl with 2.5 CHCl3 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41.50 H58.50 B Cl7.50 S3 Tl' _chemical_formula_weight 1134.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tl Tl -2.8358 9.6688 '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' _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 13.3263(18) _cell_length_b 16.333(2) _cell_length_c 23.039(3) _cell_angle_alpha 74.611(2) _cell_angle_beta 89.092(2) _cell_angle_gamma 75.496(2) _cell_volume 4673.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2276 _exptl_absorpt_coefficient_mu 4.048 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3764 _exptl_absorpt_correction_T_max 0.3764 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45397 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16418 _reflns_number_gt 13585 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0847P)^2^+25.0565P] 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 16418 _refine_ls_number_parameters 949 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1509 _refine_ls_wR_factor_gt 0.1419 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.001 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 Tl1 Tl 0.41364(2) 0.779144(18) 0.318590(12) 0.03681(10) Uani 1 1 d . . . Tl2 Tl 0.40113(2) 0.325227(18) 0.185660(13) 0.04037(10) Uani 1 1 d . . . B1 B 0.3931(6) 0.5722(5) 0.2097(3) 0.0278(16) Uani 1 1 d . . . B2 B 0.3981(6) 0.0614(5) 0.2711(3) 0.0269(15) Uani 1 1 d . . . S1 S 0.33098(13) 0.61498(11) 0.31971(7) 0.0301(4) Uani 1 1 d . . . S2 S 0.54294(14) 0.64844(11) 0.25534(7) 0.0306(4) Uani 1 1 d . . . S3 S 0.25978(14) 0.51515(12) 0.13556(7) 0.0323(4) Uani 1 1 d . . . S4 S 0.23404(13) 0.22405(11) 0.22451(7) 0.0305(4) Uani 1 1 d . . . S5 S 0.41523(13) 0.15175(10) 0.14759(7) 0.0266(3) Uani 1 1 d . . . S6 S 0.56890(14) -0.08339(11) 0.33458(7) 0.0312(4) Uani 1 1 d . . . C1 C 0.2908(5) 0.6068(5) 0.2469(3) 0.0327(15) Uani 1 1 d . . . H1A H 0.2462 0.5654 0.2528 0.039 Uiso 1 1 calc R . . H1B H 0.2497 0.6650 0.2229 0.039 Uiso 1 1 calc R . . C2 C 0.2173(5) 0.6185(4) 0.3661(3) 0.0292(14) Uani 1 1 d . . . C3 C 0.1211(6) 0.6866(5) 0.3344(3) 0.0384(16) Uani 1 1 d . . . H3A H 0.1015 0.6719 0.2978 0.046 Uiso 1 1 calc R . . H3B H 0.1355 0.7451 0.3218 0.046 Uiso 1 1 calc R . . C4 C 0.0308(6) 0.6885(6) 0.3775(4) 0.048(2) Uani 1 1 d . . . H4A H -0.0327 0.7331 0.3563 0.058 Uiso 1 1 calc R . . C5 C 0.0616(7) 0.7133(6) 0.4325(4) 0.053(2) Uani 1 1 d . . . H5A H 0.0037 0.7165 0.4600 0.063 Uiso 1 1 calc R . . H5B H 0.0763 0.7718 0.4199 0.063 Uiso 1 1 calc R . . C6 C 0.1582(6) 0.6446(6) 0.4655(3) 0.0448(19) Uani 1 1 d . . . H6A H 0.1778 0.6603 0.5021 0.054 Uiso 1 1 calc R . . C7 C 0.2479(6) 0.6423(5) 0.4225(3) 0.0394(17) Uani 1 1 d . . . H7A H 0.2636 0.7005 0.4105 0.047 Uiso 1 1 calc R . . H7B H 0.3110 0.5983 0.4432 0.047 Uiso 1 1 calc R . . C8 C 0.1357(7) 0.5538(6) 0.4841(4) 0.051(2) Uani 1 1 d . . . H8A H 0.1981 0.5092 0.5052 0.061 Uiso 1 1 calc R . . H8B H 0.0785 0.5543 0.5120 0.061 Uiso 1 1 calc R . . C9 C 0.1057(6) 0.5305(5) 0.4286(4) 0.0459(19) Uani 1 1 d . . . H9A H 0.0914 0.4711 0.4410 0.055 Uiso 1 1 calc R . . C10 C 0.0092(6) 0.5977(6) 0.3959(4) 0.051(2) Uani 1 1 d . . . H10A H -0.0497 0.5983 0.4226 0.062 Uiso 1 1 calc R . . H10B H -0.0097 0.5819 0.3596 0.062 Uiso 1 1 calc R . . C11 C 0.1940(6) 0.5289(5) 0.3852(3) 0.0362(16) Uani 1 1 d . . . H11A H 0.2569 0.4839 0.4053 0.043 Uiso 1 1 calc R . . H11B H 0.1740 0.5132 0.3492 0.043 Uiso 1 1 calc R . . C12 C 0.4667(5) 0.6419(4) 0.1931(3) 0.0306(15) Uani 1 1 d . . . H12A H 0.4215 0.7011 0.1744 0.037 Uiso 1 1 calc R . . H12B H 0.5147 0.6256 0.1624 0.037 Uiso 1 1 calc R . . C13 C 0.6479(5) 0.6958(4) 0.2207(3) 0.0262(13) Uani 1 1 d . . . C14 C 0.7280(6) 0.6286(5) 0.1972(3) 0.0378(17) Uani 1 1 d . . . H14A H 0.6945 0.6118 0.1656 0.045 Uiso 1 1 calc R . . H14B H 0.7553 0.5751 0.2305 0.045 Uiso 1 1 calc R . . C15 C 0.8179(6) 0.6684(5) 0.1709(4) 0.047(2) Uani 1 1 d . . . H15A H 0.8699 0.6249 0.1551 0.057 Uiso 1 1 calc R . . C16 C 0.7747(7) 0.7499(6) 0.1208(4) 0.0465(19) Uani 1 1 d . . . H16A H 0.7405 0.7346 0.0888 0.056 Uiso 1 1 calc R . . H16B H 0.8321 0.7750 0.1030 0.056 Uiso 1 1 calc R . . C17 C 0.6972(6) 0.8175(5) 0.1437(3) 0.0376(17) Uani 1 1 d . . . H17A H 0.6700 0.8714 0.1098 0.045 Uiso 1 1 calc R . . C18 C 0.6064(5) 0.7783(5) 0.1700(3) 0.0350(16) Uani 1 1 d . . . H18A H 0.5552 0.8218 0.1854 0.042 Uiso 1 1 calc R . . H18B H 0.5709 0.7640 0.1379 0.042 Uiso 1 1 calc R . . C19 C 0.8693(6) 0.6925(6) 0.2213(4) 0.049(2) Uani 1 1 d . . . H19A H 0.8974 0.6390 0.2545 0.058 Uiso 1 1 calc R . . H19B H 0.9276 0.7178 0.2053 0.058 Uiso 1 1 calc R . . C20 C 0.7470(7) 0.8415(5) 0.1938(4) 0.0445(19) Uani 1 1 d . . . H20A H 0.6948 0.8845 0.2090 0.053 Uiso 1 1 calc R . . H20B H 0.8039 0.8687 0.1778 0.053 Uiso 1 1 calc R . . C21 C 0.7899(6) 0.7588(5) 0.2451(3) 0.0416(18) Uani 1 1 d . . . H21A H 0.8239 0.7745 0.2775 0.050 Uiso 1 1 calc R . . C22 C 0.7015(6) 0.7193(5) 0.2707(3) 0.0353(16) Uani 1 1 d . . . H22A H 0.6505 0.7619 0.2870 0.042 Uiso 1 1 calc R . . H22B H 0.7288 0.6658 0.3041 0.042 Uiso 1 1 calc R . . C23 C 0.3531(6) 0.5768(5) 0.1400(3) 0.0322(15) Uani 1 1 d . . . H23A H 0.4146 0.5552 0.1184 0.039 Uiso 1 1 calc R . . H23B H 0.3223 0.6391 0.1184 0.039 Uiso 1 1 calc R . . C24 C 0.2438(5) 0.5237(5) 0.0544(3) 0.0320(15) Uani 1 1 d . . . C25 C 0.1850(6) 0.6181(5) 0.0201(3) 0.0359(16) Uani 1 1 d . . . H25A H 0.1171 0.6346 0.0378 0.043 Uiso 1 1 calc R . . H25B H 0.2255 0.6598 0.0238 0.043 Uiso 1 1 calc R . . C26 C 0.1683(7) 0.6226(5) -0.0465(3) 0.0443(19) Uani 1 1 d . . . H26A H 0.1299 0.6837 -0.0687 0.053 Uiso 1 1 calc R . . C27 C 0.1034(7) 0.5591(5) -0.0506(4) 0.049(2) Uani 1 1 d . . . H27A H 0.0358 0.5755 -0.0326 0.059 Uiso 1 1 calc R . . H27B H 0.0897 0.5625 -0.0934 0.059 Uiso 1 1 calc R . . C28 C 0.3481(6) 0.4989(6) 0.0262(3) 0.0456(19) Uani 1 1 d . . . H28A H 0.3866 0.4386 0.0482 0.055 Uiso 1 1 calc R . . H28B H 0.3903 0.5396 0.0295 0.055 Uiso 1 1 calc R . . C29 C 0.2713(8) 0.5980(7) -0.0746(4) 0.058(2) Uani 1 1 d . . . H29A H 0.3134 0.6392 -0.0720 0.070 Uiso 1 1 calc R . . H29B H 0.2594 0.6019 -0.1176 0.070 Uiso 1 1 calc R . . C30 C 0.3295(7) 0.5038(7) -0.0407(4) 0.054(2) Uani 1 1 d . . . H30A H 0.3974 0.4865 -0.0590 0.065 Uiso 1 1 calc R . . C31 C 0.2624(8) 0.4414(6) -0.0448(4) 0.060(3) Uani 1 1 d . . . H31A H 0.2503 0.4438 -0.0875 0.072 Uiso 1 1 calc R . . H31B H 0.2993 0.3804 -0.0232 0.072 Uiso 1 1 calc R . . C32 C 0.1609(7) 0.4669(5) -0.0176(3) 0.047(2) Uani 1 1 d . . . H32A H 0.1182 0.4257 -0.0208 0.056 Uiso 1 1 calc R . . C33 C 0.1782(7) 0.4617(5) 0.0499(3) 0.0444(19) Uani 1 1 d . . . H33A H 0.1106 0.4785 0.0677 0.053 Uiso 1 1 calc R . . H33B H 0.2140 0.4008 0.0724 0.053 Uiso 1 1 calc R . . C34 C 0.4588(6) 0.4728(4) 0.2432(3) 0.0320(15) Uani 1 1 d . . . C35 C 0.5563(7) 0.4366(5) 0.2252(4) 0.051(2) Uani 1 1 d . . . H35A H 0.5862 0.4722 0.1939 0.061 Uiso 1 1 calc R . . C36 C 0.6112(7) 0.3507(6) 0.2511(5) 0.066(3) Uani 1 1 d . . . H36A H 0.6774 0.3286 0.2373 0.080 Uiso 1 1 calc R . . C37 C 0.5706(9) 0.2968(6) 0.2970(5) 0.070(3) Uani 1 1 d . . . H37A H 0.6085 0.2379 0.3149 0.084 Uiso 1 1 calc R . . C38 C 0.4751(10) 0.3295(6) 0.3162(4) 0.064(3) Uani 1 1 d . . . H38A H 0.4464 0.2932 0.3478 0.077 Uiso 1 1 calc R . . C39 C 0.4193(7) 0.4162(5) 0.2895(3) 0.0406(18) Uani 1 1 d . . . H39A H 0.3526 0.4374 0.3032 0.049 Uiso 1 1 calc R . . C40 C 0.3208(5) 0.1487(4) 0.2866(3) 0.0300(14) Uani 1 1 d . . . H40A H 0.3644 0.1814 0.3006 0.036 Uiso 1 1 calc R . . H40B H 0.2783 0.1284 0.3204 0.036 Uiso 1 1 calc R . . C41 C 0.1237(5) 0.2825(4) 0.2591(3) 0.0286(14) Uani 1 1 d . . . C42 C 0.0637(6) 0.3592(5) 0.2072(3) 0.0423(18) Uani 1 1 d . . . H42A H 0.1087 0.3987 0.1902 0.051 Uiso 1 1 calc R . . H42B H 0.0433 0.3363 0.1747 0.051 Uiso 1 1 calc R . . C43 C -0.0336(6) 0.4104(5) 0.2311(3) 0.045(2) Uani 1 1 d . . . H43A H -0.0728 0.4600 0.1973 0.055 Uiso 1 1 calc R . . C44 C 0.0010(7) 0.4473(5) 0.2793(4) 0.051(2) Uani 1 1 d . . . H44A H -0.0604 0.4820 0.2947 0.062 Uiso 1 1 calc R . . H44B H 0.0458 0.4867 0.2618 0.062 Uiso 1 1 calc R . . C45 C 0.0608(6) 0.3717(5) 0.3309(3) 0.0403(18) Uani 1 1 d . . . H45A H 0.0828 0.3957 0.3629 0.048 Uiso 1 1 calc R . . C46 C 0.1566(5) 0.3202(5) 0.3070(3) 0.0328(15) Uani 1 1 d . . . H46A H 0.2016 0.3595 0.2895 0.039 Uiso 1 1 calc R . . H46B H 0.1969 0.2721 0.3404 0.039 Uiso 1 1 calc R . . C47 C -0.0091(6) 0.3109(5) 0.3576(3) 0.0424(18) Uani 1 1 d . . . H47A H 0.0291 0.2619 0.3913 0.051 Uiso 1 1 calc R . . H47B H -0.0709 0.3440 0.3736 0.051 Uiso 1 1 calc R . . C48 C -0.0428(6) 0.2749(6) 0.3092(4) 0.0475(19) Uani 1 1 d . . . H48A H -0.0888 0.2355 0.3264 0.057 Uiso 1 1 calc R . . C49 C -0.1016(6) 0.3510(6) 0.2568(4) 0.052(2) Uani 1 1 d . . . H49A H -0.1234 0.3274 0.2251 0.063 Uiso 1 1 calc R . . H49B H -0.1647 0.3846 0.2715 0.063 Uiso 1 1 calc R . . C50 C 0.0541(6) 0.2226(5) 0.2852(4) 0.0405(17) Uani 1 1 d . . . H50A H 0.0925 0.1729 0.3183 0.049 Uiso 1 1 calc R . . H50B H 0.0328 0.1984 0.2536 0.049 Uiso 1 1 calc R . . C51 C 0.4797(5) 0.0862(4) 0.2198(3) 0.0280(14) Uani 1 1 d . . . H51A H 0.5263 0.0314 0.2145 0.034 Uiso 1 1 calc R . . H51B H 0.5231 0.1191 0.2338 0.034 Uiso 1 1 calc R . . C52 C 0.5129(5) 0.1445(4) 0.0917(3) 0.0264(13) Uani 1 1 d . . . C53 C 0.6123(6) 0.1640(5) 0.1087(3) 0.0368(16) Uani 1 1 d . . . H53A H 0.6446 0.1206 0.1465 0.044 Uiso 1 1 calc R . . H53B H 0.5963 0.2232 0.1155 0.044 Uiso 1 1 calc R . . C54 C 0.6874(7) 0.1598(6) 0.0582(4) 0.051(2) Uani 1 1 d . . . H54A H 0.7532 0.1716 0.0700 0.061 Uiso 1 1 calc R . . C55 C 0.6386(7) 0.2286(6) 0.0010(4) 0.051(2) Uani 1 1 d . . . H55A H 0.6875 0.2270 -0.0317 0.061 Uiso 1 1 calc R . . H55B H 0.6234 0.2878 0.0078 0.061 Uiso 1 1 calc R . . C56 C 0.5380(7) 0.2104(5) -0.0173(3) 0.0417(18) Uani 1 1 d . . . H56A H 0.5056 0.2557 -0.0550 0.050 Uiso 1 1 calc R . . C57 C 0.4626(6) 0.2130(4) 0.0335(3) 0.0342(16) Uani 1 1 d . . . H57A H 0.3979 0.2004 0.0220 0.041 Uiso 1 1 calc R . . H57B H 0.4445 0.2723 0.0401 0.041 Uiso 1 1 calc R . . C58 C 0.7114(6) 0.0684(6) 0.0475(4) 0.050(2) Uani 1 1 d . . . H58A H 0.7613 0.0652 0.0153 0.060 Uiso 1 1 calc R . . H58B H 0.7433 0.0234 0.0848 0.060 Uiso 1 1 calc R . . C59 C 0.5641(7) 0.1190(5) -0.0285(3) 0.0413(18) Uani 1 1 d . . . H59A H 0.5002 0.1066 -0.0413 0.050 Uiso 1 1 calc R . . H59B H 0.6133 0.1169 -0.0611 0.050 Uiso 1 1 calc R . . C60 C 0.6121(6) 0.0508(5) 0.0290(3) 0.0388(17) Uani 1 1 d . . . H60A H 0.6283 -0.0088 0.0218 0.047 Uiso 1 1 calc R . . C61 C 0.5366(5) 0.0536(4) 0.0796(3) 0.0306(14) Uani 1 1 d . . . H61A H 0.5676 0.0076 0.1167 0.037 Uiso 1 1 calc R . . H61B H 0.4715 0.0419 0.0678 0.037 Uiso 1 1 calc R . . C62 C 0.4647(5) 0.0111(4) 0.3366(3) 0.0319(15) Uani 1 1 d . . . H62A H 0.4163 -0.0080 0.3672 0.038 Uiso 1 1 calc R . . H62B H 0.4942 0.0537 0.3495 0.038 Uiso 1 1 calc R . . C63 C 0.6184(5) -0.1315(4) 0.4134(3) 0.0299(14) Uani 1 1 d . . . C64 C 0.6516(7) -0.0659(5) 0.4392(4) 0.049(2) Uani 1 1 d . . . H64A H 0.5912 -0.0160 0.4389 0.059 Uiso 1 1 calc R . . H64B H 0.7047 -0.0428 0.4143 0.059 Uiso 1 1 calc R . . C65 C 0.6966(8) -0.1113(6) 0.5045(4) 0.059(3) Uani 1 1 d . . . H65A H 0.7183 -0.0678 0.5216 0.071 Uiso 1 1 calc R . . C66 C 0.7918(7) -0.1870(7) 0.5036(4) 0.067(3) Uani 1 1 d . . . H66A H 0.8442 -0.1642 0.4778 0.081 Uiso 1 1 calc R . . H66B H 0.8236 -0.2151 0.5450 0.081 Uiso 1 1 calc R . . C67 C 0.5367(6) -0.1669(6) 0.4527(3) 0.0435(18) Uani 1 1 d . . . H67A H 0.5146 -0.2101 0.4361 0.052 Uiso 1 1 calc R . . H67B H 0.4750 -0.1181 0.4524 0.052 Uiso 1 1 calc R . . C68 C 0.6149(7) -0.1456(6) 0.5426(4) 0.054(2) Uani 1 1 d . . . H68A H 0.6433 -0.1736 0.5846 0.065 Uiso 1 1 calc R . . H68B H 0.5542 -0.0963 0.5428 0.065 Uiso 1 1 calc R . . C69 C 0.5818(7) -0.2112(6) 0.5179(3) 0.053(2) Uani 1 1 d . . . H69A H 0.5278 -0.2337 0.5433 0.063 Uiso 1 1 calc R . . C70 C 0.6762(8) -0.2873(5) 0.5185(3) 0.056(2) Uani 1 1 d . . . H70A H 0.7058 -0.3153 0.5603 0.067 Uiso 1 1 calc R . . H70B H 0.6549 -0.3321 0.5033 0.067 Uiso 1 1 calc R . . C71 C 0.7568(7) -0.2532(6) 0.4792(4) 0.055(2) Uani 1 1 d . . . H71A H 0.8179 -0.3034 0.4794 0.066 Uiso 1 1 calc R . . C72 C 0.7117(7) -0.2097(5) 0.4140(3) 0.046(2) Uani 1 1 d . . . H72A H 0.6892 -0.2529 0.3976 0.056 Uiso 1 1 calc R . . H72B H 0.7655 -0.1890 0.3883 0.056 Uiso 1 1 calc R . . C73 C 0.3311(5) -0.0014(4) 0.2544(3) 0.0276(14) Uani 1 1 d . . . C74 C 0.3585(6) -0.0471(4) 0.2102(3) 0.0336(15) Uani 1 1 d . . . H74A H 0.4173 -0.0396 0.1876 0.040 Uiso 1 1 calc R . . C75 C 0.3031(7) -0.1023(5) 0.1986(3) 0.047(2) Uani 1 1 d . . . H75A H 0.3239 -0.1320 0.1684 0.056 Uiso 1 1 calc R . . C76 C 0.2158(7) -0.1149(5) 0.2313(4) 0.048(2) Uani 1 1 d . . . H76A H 0.1774 -0.1530 0.2235 0.058 Uiso 1 1 calc R . . C77 C 0.1870(7) -0.0719(5) 0.2743(4) 0.050(2) Uani 1 1 d . . . H77A H 0.1280 -0.0798 0.2967 0.060 Uiso 1 1 calc R . . C78 C 0.2435(6) -0.0162(5) 0.2856(4) 0.0382(17) Uani 1 1 d . . . H78A H 0.2217 0.0131 0.3159 0.046 Uiso 1 1 calc R . . C79 C 0.8154(12) 1.0093(10) 0.2891(7) 0.104(4) Uiso 1 1 d . . . H79A H 0.7527 0.9867 0.2872 0.124 Uiso 1 1 calc R A 1 Cl1 Cl 0.9036(10) 0.9256(9) 0.3285(6) 0.150(5) Uiso 0.457(9) 1 d P B 1 Cl2 Cl 0.8564(8) 1.0319(8) 0.2153(5) 0.126(4) Uiso 0.457(9) 1 d P B 1 Cl3 Cl 0.7714(10) 1.1049(8) 0.3057(6) 0.149(5) Uiso 0.457(9) 1 d P B 1 Cl1A Cl 0.8937(8) 0.9643(7) 0.2438(5) 0.139(4) Uiso 0.543(9) 1 d P B 2 Cl2A Cl 0.9103(8) 0.9879(7) 0.3565(5) 0.146(4) Uiso 0.543(9) 1 d P B 2 Cl3A Cl 0.7986(11) 1.1287(9) 0.2515(7) 0.195(6) Uiso 0.543(9) 1 d P B 2 C80 C 0.8364(19) 0.0896(17) 0.4838(11) 0.180(9) Uiso 1 1 d . . . H80A H 0.8416 0.0307 0.4770 0.216 Uiso 1 1 calc R C 3 Cl4 Cl 0.7243(8) 0.1757(7) 0.4446(5) 0.212(4) Uiso 0.829(8) 1 d P D 3 Cl5 Cl 0.9438(5) 0.1209(4) 0.4753(3) 0.132(2) Uiso 0.829(8) 1 d P D 3 Cl4A Cl 0.8163(9) 0.0622(8) 0.5631(5) 0.040(4) Uiso 0.171(8) 1 d P D 4 Cl5A Cl 0.8816(14) 0.1714(12) 0.4588(8) 0.075(5) Uiso 0.171(8) 1 d P D 4 Cl6 Cl 0.7736(7) 0.1047(6) 0.5593(4) 0.200(3) Uiso 1 1 d . D . C81 C 1.0746(10) 0.8728(10) 0.0814(6) 0.095(4) Uani 1 1 d . . . H81A H 1.1200 0.9145 0.0721 0.113 Uiso 1 1 calc R E 1 Cl7 Cl 0.9824(7) 0.9197(6) 0.1306(6) 0.091(3) Uiso 0.448(15) 1 d P F 1 Cl8 Cl 1.1533(6) 0.7840(5) 0.1195(3) 0.069(2) Uiso 0.448(15) 1 d P F 1 Cl7A Cl 0.9643(5) 0.9246(4) 0.1039(4) 0.084(2) Uiso 0.552(15) 1 d P F 2 Cl8A Cl 1.1144(6) 0.7591(5) 0.1265(3) 0.084(2) Uiso 0.552(15) 1 d P F 2 Cl9 Cl 1.0424(3) 0.8663(3) 0.00811(19) 0.1142(12) Uiso 1 1 d . F . C82 C 0.4145(6) -0.4837(5) 0.6093(3) 0.0429(18) Uani 1 1 d . . . H82A H 0.4621 -0.5040 0.6462 0.051 Uiso 1 1 calc R . . Cl10 Cl 0.4584(3) -0.4069(2) 0.55594(11) 0.0793(8) Uani 1 1 d . . . Cl11 Cl 0.28831(19) -0.4404(2) 0.62871(11) 0.0722(7) Uani 1 1 d . . . Cl12 Cl 0.4147(2) -0.57551(16) 0.58165(10) 0.0633(6) Uani 1 1 d . . . C83 C 0.8340(6) -0.1383(5) -0.1042(3) 0.0385(17) Uani 1 1 d . . . H83A H 0.7825 -0.1294 -0.1378 0.046 Uiso 1 1 calc R . . Cl13 Cl 0.94790(19) -0.11600(18) -0.13550(11) 0.0646(6) Uani 1 1 d . . . Cl14 Cl 0.8587(2) -0.24768(14) -0.06060(11) 0.0621(6) Uani 1 1 d . . . Cl15 Cl 0.77979(18) -0.06787(15) -0.05982(10) 0.0572(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tl1 0.04442(18) 0.03331(16) 0.03369(16) -0.00896(12) -0.00029(12) -0.01165(12) Tl2 0.0543(2) 0.03006(16) 0.03912(17) -0.01361(12) -0.00384(13) -0.01010(13) B1 0.040(4) 0.027(4) 0.022(3) -0.010(3) 0.001(3) -0.014(3) B2 0.033(4) 0.021(3) 0.021(3) -0.005(3) -0.003(3) 0.002(3) S1 0.0344(9) 0.0353(9) 0.0253(8) -0.0126(7) 0.0031(7) -0.0128(7) S2 0.0395(9) 0.0327(9) 0.0237(8) -0.0089(7) -0.0001(7) -0.0152(7) S3 0.0422(10) 0.0364(9) 0.0242(8) -0.0095(7) -0.0001(7) -0.0189(8) S4 0.0340(9) 0.0273(8) 0.0257(8) -0.0096(6) -0.0028(7) 0.0032(7) S5 0.0327(8) 0.0229(8) 0.0223(8) -0.0049(6) -0.0006(6) -0.0046(6) S6 0.0402(9) 0.0265(8) 0.0195(8) -0.0057(6) -0.0010(7) 0.0046(7) C1 0.038(4) 0.037(4) 0.026(3) -0.011(3) -0.002(3) -0.012(3) C2 0.034(4) 0.030(3) 0.026(3) -0.010(3) 0.004(3) -0.011(3) C3 0.035(4) 0.038(4) 0.038(4) -0.008(3) -0.002(3) -0.004(3) C4 0.041(4) 0.054(5) 0.046(5) -0.015(4) 0.000(4) -0.001(4) C5 0.045(5) 0.053(5) 0.069(6) -0.033(4) 0.021(4) -0.011(4) C6 0.048(5) 0.066(5) 0.031(4) -0.026(4) 0.007(3) -0.019(4) C7 0.042(4) 0.051(5) 0.033(4) -0.018(3) 0.005(3) -0.019(4) C8 0.049(5) 0.062(5) 0.037(4) -0.008(4) 0.013(4) -0.014(4) C9 0.052(5) 0.044(4) 0.049(5) -0.015(4) 0.015(4) -0.024(4) C10 0.041(5) 0.072(6) 0.051(5) -0.027(4) 0.013(4) -0.025(4) C11 0.042(4) 0.033(4) 0.035(4) -0.010(3) 0.007(3) -0.012(3) C12 0.041(4) 0.032(4) 0.025(3) -0.009(3) -0.001(3) -0.017(3) C13 0.029(3) 0.026(3) 0.025(3) -0.008(3) -0.001(3) -0.008(3) C14 0.048(4) 0.026(4) 0.038(4) -0.009(3) 0.007(3) -0.007(3) C15 0.039(4) 0.034(4) 0.061(5) -0.008(4) 0.014(4) -0.001(3) C16 0.054(5) 0.057(5) 0.036(4) -0.014(4) 0.016(4) -0.026(4) C17 0.043(4) 0.029(4) 0.035(4) 0.004(3) -0.005(3) -0.011(3) C18 0.034(4) 0.029(4) 0.040(4) -0.005(3) -0.004(3) -0.008(3) C19 0.032(4) 0.051(5) 0.056(5) -0.003(4) -0.003(4) -0.010(4) C20 0.049(5) 0.035(4) 0.054(5) -0.012(4) 0.005(4) -0.019(4) C21 0.038(4) 0.052(5) 0.040(4) -0.012(4) -0.005(3) -0.019(4) C22 0.047(4) 0.036(4) 0.025(3) -0.008(3) -0.004(3) -0.015(3) C23 0.044(4) 0.034(4) 0.025(3) -0.009(3) 0.000(3) -0.019(3) C24 0.038(4) 0.034(4) 0.025(3) -0.009(3) -0.007(3) -0.010(3) C25 0.043(4) 0.030(4) 0.035(4) -0.009(3) -0.004(3) -0.009(3) C26 0.060(5) 0.040(4) 0.030(4) -0.005(3) -0.011(3) -0.010(4) C27 0.054(5) 0.052(5) 0.038(4) -0.012(4) -0.017(4) -0.010(4) C28 0.043(4) 0.061(5) 0.034(4) -0.022(4) -0.005(3) -0.005(4) C29 0.069(6) 0.081(7) 0.032(4) -0.012(4) -0.001(4) -0.034(5) C30 0.048(5) 0.083(7) 0.035(4) -0.031(4) 0.000(4) -0.007(4) C31 0.083(7) 0.051(5) 0.040(5) -0.024(4) -0.021(4) 0.006(5) C32 0.065(5) 0.043(4) 0.037(4) -0.011(3) -0.016(4) -0.020(4) C33 0.068(5) 0.034(4) 0.037(4) -0.006(3) -0.012(4) -0.023(4) C34 0.041(4) 0.032(4) 0.030(3) -0.014(3) -0.003(3) -0.014(3) C35 0.045(5) 0.041(5) 0.070(6) -0.017(4) 0.001(4) -0.016(4) C36 0.041(5) 0.048(5) 0.111(9) -0.030(6) -0.011(5) -0.004(4) C37 0.090(8) 0.035(5) 0.077(7) -0.010(5) -0.042(6) -0.002(5) C38 0.123(10) 0.038(5) 0.032(4) -0.006(4) -0.008(5) -0.023(5) C39 0.067(5) 0.036(4) 0.022(3) -0.009(3) 0.003(3) -0.016(4) C40 0.034(4) 0.025(3) 0.026(3) -0.005(3) -0.003(3) -0.001(3) C41 0.030(3) 0.022(3) 0.029(3) -0.008(3) -0.004(3) 0.005(3) C42 0.044(4) 0.040(4) 0.030(4) -0.006(3) -0.008(3) 0.011(3) C43 0.040(4) 0.047(5) 0.035(4) -0.011(3) -0.007(3) 0.014(4) C44 0.054(5) 0.040(4) 0.056(5) -0.019(4) 0.004(4) 0.002(4) C45 0.039(4) 0.047(4) 0.038(4) -0.027(3) -0.001(3) 0.000(3) C46 0.031(4) 0.033(4) 0.037(4) -0.015(3) -0.001(3) -0.007(3) C47 0.031(4) 0.053(5) 0.040(4) -0.016(4) 0.002(3) -0.001(3) C48 0.039(4) 0.053(5) 0.055(5) -0.020(4) 0.007(4) -0.012(4) C49 0.035(4) 0.075(6) 0.045(5) -0.026(4) -0.008(4) 0.004(4) C50 0.037(4) 0.042(4) 0.047(4) -0.020(4) 0.002(3) -0.010(3) C51 0.038(4) 0.022(3) 0.023(3) -0.005(3) -0.002(3) -0.006(3) C52 0.033(4) 0.023(3) 0.020(3) -0.002(2) 0.000(3) -0.005(3) C53 0.043(4) 0.046(4) 0.023(3) -0.007(3) 0.000(3) -0.018(3) C54 0.050(5) 0.076(6) 0.044(5) -0.021(4) 0.014(4) -0.040(5) C55 0.075(6) 0.051(5) 0.039(4) -0.014(4) 0.020(4) -0.038(5) C56 0.071(5) 0.032(4) 0.018(3) 0.001(3) -0.003(3) -0.015(4) C57 0.053(4) 0.022(3) 0.024(3) -0.002(3) -0.004(3) -0.006(3) C58 0.045(5) 0.062(5) 0.039(4) -0.012(4) 0.011(4) -0.009(4) C59 0.057(5) 0.043(4) 0.026(4) -0.011(3) 0.009(3) -0.017(4) C60 0.053(5) 0.032(4) 0.029(4) -0.008(3) 0.007(3) -0.007(3) C61 0.038(4) 0.019(3) 0.031(4) -0.002(3) 0.005(3) -0.006(3) C62 0.037(4) 0.023(3) 0.027(3) -0.004(3) -0.002(3) 0.005(3) C63 0.036(4) 0.029(3) 0.019(3) -0.004(3) -0.003(3) -0.001(3) C64 0.064(5) 0.039(4) 0.041(4) -0.008(4) -0.009(4) -0.012(4) C65 0.083(7) 0.047(5) 0.047(5) -0.012(4) -0.031(5) -0.014(5) C66 0.050(5) 0.085(7) 0.048(5) 0.003(5) -0.020(4) -0.005(5) C67 0.046(4) 0.050(5) 0.028(4) -0.001(3) -0.003(3) -0.011(4) C68 0.069(6) 0.049(5) 0.029(4) -0.010(4) -0.011(4) 0.011(4) C69 0.054(5) 0.064(6) 0.027(4) 0.002(4) -0.005(4) -0.005(4) C70 0.091(7) 0.037(4) 0.026(4) 0.001(3) -0.011(4) 0.000(4) C71 0.052(5) 0.052(5) 0.040(5) -0.005(4) -0.010(4) 0.019(4) C72 0.052(5) 0.040(4) 0.029(4) -0.006(3) -0.002(3) 0.016(4) C73 0.035(4) 0.019(3) 0.023(3) -0.002(2) -0.001(3) 0.000(3) C74 0.049(4) 0.020(3) 0.030(4) -0.002(3) -0.001(3) -0.010(3) C75 0.077(6) 0.034(4) 0.031(4) -0.006(3) 0.000(4) -0.020(4) C76 0.057(5) 0.035(4) 0.051(5) -0.001(4) -0.007(4) -0.019(4) C77 0.044(5) 0.039(4) 0.062(5) -0.005(4) 0.009(4) -0.011(4) C78 0.042(4) 0.026(4) 0.045(4) -0.007(3) 0.010(3) -0.007(3) C81 0.071(8) 0.110(10) 0.095(9) -0.019(8) -0.003(7) -0.019(7) C82 0.050(5) 0.046(4) 0.031(4) -0.012(3) -0.003(3) -0.007(4) Cl10 0.105(2) 0.094(2) 0.0443(13) -0.0009(13) 0.0016(13) -0.0533(17) Cl11 0.0527(13) 0.0963(19) 0.0544(13) -0.0270(13) 0.0032(11) 0.0118(13) Cl12 0.0770(16) 0.0646(14) 0.0502(12) -0.0289(11) -0.0119(11) -0.0062(12) C83 0.040(4) 0.038(4) 0.040(4) -0.015(3) -0.003(3) -0.009(3) Cl13 0.0621(14) 0.0859(17) 0.0565(13) -0.0224(12) 0.0127(11) -0.0355(13) Cl14 0.0790(16) 0.0346(11) 0.0664(14) -0.0055(10) -0.0050(12) -0.0110(10) Cl15 0.0592(13) 0.0536(12) 0.0593(13) -0.0299(10) -0.0032(10) 0.0008(10) _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 Tl1 S2 3.0625(17) . ? Tl1 S1 3.1377(17) . ? Tl1 S6(a) 3.4997(19) . ? Tl2 S4 3.0797(19) . ? Tl2 S3 3.1216(19) . ? Tl2 S5 3.1433(16) . ? B1 C34 1.626(10) . ? B1 C12 1.649(9) . ? B1 C1 1.657(10) . ? B1 C23 1.677(9) . ? B2 C51 1.634(10) . ? B2 C73 1.637(10) . ? B2 C40 1.658(9) . ? B2 C62 1.661(9) . ? S1 C1 1.818(7) . ? S1 C2 1.839(7) . ? S2 C12 1.812(6) . ? S2 C13 1.836(7) . ? S3 C23 1.804(7) . ? S3 C24 1.849(7) . ? S4 C40 1.817(6) . ? S4 C41 1.836(6) . ? S5 C51 1.814(6) . ? S5 C52 1.822(6) . ? S6 C62 1.810(6) . ? S6 C63 1.836(6) . ? C2 C3 1.516(10) . ? C2 C11 1.521(9) . ? C2 C7 1.538(9) . ? C3 C4 1.547(11) . ? C4 C5 1.522(12) . ? C4 C10 1.529(12) . ? C5 C6 1.532(12) . ? C6 C8 1.534(12) . ? C6 C7 1.540(10) . ? C8 C9 1.513(12) . ? C9 C10 1.521(12) . ? C9 C11 1.531(10) . ? C13 C18 1.515(9) . ? C13 C14 1.531(9) . ? C13 C22 1.544(9) . ? C14 C15 1.544(11) . ? C15 C16 1.502(11) . ? C15 C19 1.542(12) . ? C16 C17 1.512(11) . ? C17 C20 1.523(11) . ? C17 C18 1.550(10) . ? C19 C21 1.522(12) . ? C20 C21 1.528(11) . ? C21 C22 1.520(10) . ? C24 C33 1.519(10) . ? C24 C28 1.531(11) . ? C24 C25 1.544(9) . ? C25 C26 1.535(10) . ? C26 C29 1.517(13) . ? C26 C27 1.529(11) . ? C27 C32 1.505(11) . ? C28 C30 1.543(10) . ? C29 C30 1.537(14) . ? C30 C31 1.535(14) . ? C31 C32 1.492(13) . ? C32 C33 1.552(10) . ? C34 C35 1.392(11) . ? C34 C39 1.405(10) . ? C35 C36 1.385(13) . ? C36 C37 1.383(15) . ? C37 C38 1.366(15) . ? C38 C39 1.401(12) . ? C41 C50 1.517(10) . ? C41 C46 1.518(9) . ? C41 C42 1.540(9) . ? C42 C43 1.539(10) . ? C43 C49 1.494(13) . ? C43 C44 1.523(12) . ? C44 C45 1.528(11) . ? C45 C46 1.526(10) . ? C45 C47 1.534(11) . ? C47 C48 1.513(11) . ? C48 C49 1.537(12) . ? C48 C50 1.542(11) . ? C52 C53 1.517(9) . ? C52 C57 1.535(9) . ? C52 C61 1.539(9) . ? C53 C54 1.526(10) . ? C54 C55 1.517(12) . ? C54 C58 1.531(12) . ? C55 C56 1.533(12) . ? C56 C57 1.532(10) . ? C56 C59 1.535(10) . ? C58 C60 1.514(12) . ? C59 C60 1.514(10) . ? C60 C61 1.530(10) . ? C63 C64 1.509(10) . ? C63 C67 1.533(10) . ? C63 C72 1.541(9) . ? C64 C65 1.544(11) . ? C65 C68 1.511(14) . ? C65 C66 1.538(14) . ? C66 C71 1.514(14) . ? C67 C69 1.541(10) . ? C68 C69 1.494(13) . ? C69 C70 1.529(12) . ? C70 C71 1.513(13) . ? C71 C72 1.540(10) . ? C73 C78 1.400(10) . ? C73 C74 1.406(9) . ? C74 C75 1.379(11) . ? C75 C76 1.405(12) . ? C76 C77 1.357(12) . ? C77 C78 1.392(11) . ? C79 Cl1 1.626(19) . ? C79 Cl1A 1.646(17) . ? C79 Cl3 1.666(19) . ? C79 Cl2 1.752(18) . ? C79 Cl3A 1.87(2) . ? C79 Cl2A 1.919(18) . ? C80 Cl5A 1.57(3) . ? C80 Cl5 1.63(2) . ? C80 Cl4A 1.80(3) . ? C80 Cl4 1.83(3) . ? C80 Cl6 1.97(2) . ? Cl4A Cl6 0.765(13) . ? C81 Cl8 1.602(15) . ? C81 Cl7A 1.652(15) . ? C81 Cl9 1.786(14) . ? C81 Cl8A 1.820(16) . ? C81 Cl7 1.824(17) . ? C82 Cl10 1.717(8) . ? C82 Cl11 1.755(8) . ? C82 Cl12 1.777(8) . ? C83 Cl13 1.749(8) . ? C83 Cl14 1.753(8) . ? C83 Cl15 1.754(7) . ? 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 S2 Tl1 S1 63.63(4) . . ? S4 Tl2 S3 99.93(5) . . ? S4 Tl2 S5 60.78(4) . . ? S3 Tl2 S5 131.33(4) . . ? C34 B1 C12 112.6(6) . . ? C34 B1 C1 112.5(6) . . ? C12 B1 C1 112.5(5) . . ? C34 B1 C23 109.7(5) . . ? C12 B1 C23 99.8(5) . . ? C1 B1 C23 109.0(6) . . ? C51 B2 C73 112.2(5) . . ? C51 B2 C40 113.2(5) . . ? C73 B2 C40 111.1(5) . . ? C51 B2 C62 108.4(5) . . ? C73 B2 C62 110.0(5) . . ? C40 B2 C62 101.4(5) . . ? C1 S1 C2 107.1(3) . . ? C1 S1 Tl1 116.2(2) . . ? C2 S1 Tl1 107.8(2) . . ? C12 S2 C13 105.4(3) . . ? C12 S2 Tl1 110.1(2) . . ? C13 S2 Tl1 106.6(2) . . ? C23 S3 C24 104.9(3) . . ? C23 S3 Tl2 99.2(2) . . ? C24 S3 Tl2 102.4(2) . . ? C40 S4 C41 106.0(3) . . ? C40 S4 Tl2 89.9(2) . . ? C41 S4 Tl2 114.2(2) . . ? C51 S5 C52 106.5(3) . . ? C51 S5 Tl2 90.7(2) . . ? C52 S5 Tl2 107.8(2) . . ? C62 S6 C63 104.3(3) . . ? B1 C1 S1 110.7(5) . . ? C3 C2 C11 109.2(6) . . ? C3 C2 C7 109.5(6) . . ? C11 C2 C7 109.1(6) . . ? C3 C2 S1 112.9(5) . . ? C11 C2 S1 110.5(5) . . ? C7 C2 S1 105.5(5) . . ? C2 C3 C4 109.6(6) . . ? C5 C4 C10 110.6(7) . . ? C5 C4 C3 108.8(7) . . ? C10 C4 C3 108.9(7) . . ? C4 C5 C6 109.7(7) . . ? C5 C6 C8 109.6(7) . . ? C5 C6 C7 108.9(7) . . ? C8 C6 C7 109.1(7) . . ? C2 C7 C6 109.6(6) . . ? C9 C8 C6 109.6(6) . . ? C8 C9 C10 110.5(7) . . ? C8 C9 C11 110.1(7) . . ? C10 C9 C11 108.4(7) . . ? C9 C10 C4 109.2(7) . . ? C2 C11 C9 110.1(6) . . ? B1 C12 S2 116.3(4) . . ? C18 C13 C14 110.0(6) . . ? C18 C13 C22 109.2(5) . . ? C14 C13 C22 108.6(6) . . ? C18 C13 S2 111.5(5) . . ? C14 C13 S2 110.7(5) . . ? C22 C13 S2 106.8(4) . . ? C13 C14 C15 109.8(6) . . ? C16 C15 C19 109.5(7) . . ? C16 C15 C14 108.9(7) . . ? C19 C15 C14 108.5(7) . . ? C15 C16 C17 111.0(6) . . ? C16 C17 C20 110.8(6) . . ? C16 C17 C18 108.9(6) . . ? C20 C17 C18 108.0(6) . . ? C13 C18 C17 109.6(6) . . ? C21 C19 C15 109.9(6) . . ? C17 C20 C21 109.6(6) . . ? C22 C21 C19 109.7(6) . . ? C22 C21 C20 109.4(6) . . ? C19 C21 C20 109.5(7) . . ? C21 C22 C13 109.6(6) . . ? B1 C23 S3 115.9(5) . . ? C33 C24 C28 110.3(6) . . ? C33 C24 C25 108.7(6) . . ? C28 C24 C25 109.2(6) . . ? C33 C24 S3 106.3(5) . . ? C28 C24 S3 112.2(5) . . ? C25 C24 S3 110.1(5) . . ? C26 C25 C24 109.2(6) . . ? C29 C26 C27 109.8(7) . . ? C29 C26 C25 110.8(7) . . ? C27 C26 C25 108.5(6) . . ? C32 C27 C26 109.6(6) . . ? C24 C28 C30 109.8(6) . . ? C26 C29 C30 109.1(7) . . ? C31 C30 C29 108.9(7) . . ? C31 C30 C28 108.9(8) . . ? C29 C30 C28 109.3(7) . . ? C32 C31 C30 110.3(7) . . ? C31 C32 C27 110.1(7) . . ? C31 C32 C33 110.3(7) . . ? C27 C32 C33 109.2(7) . . ? C24 C33 C32 108.7(6) . . ? C35 C34 C39 115.6(7) . . ? C35 C34 B1 121.6(7) . . ? C39 C34 B1 122.7(7) . . ? C36 C35 C34 122.5(9) . . ? C37 C36 C35 120.5(9) . . ? C38 C37 C36 119.0(9) . . ? C37 C38 C39 120.3(9) . . ? C38 C39 C34 122.0(8) . . ? B2 C40 S4 115.5(4) . . ? C50 C41 C46 110.3(6) . . ? C50 C41 C42 109.5(6) . . ? C46 C41 C42 108.3(6) . . ? C50 C41 S4 110.3(5) . . ? C46 C41 S4 113.0(5) . . ? C42 C41 S4 105.3(5) . . ? C43 C42 C41 109.4(6) . . ? C49 C43 C44 110.5(7) . . ? C49 C43 C42 110.0(7) . . ? C44 C43 C42 108.3(7) . . ? C43 C44 C45 109.3(6) . . ? C46 C45 C44 109.3(6) . . ? C46 C45 C47 109.7(6) . . ? C44 C45 C47 109.4(7) . . ? C41 C46 C45 109.7(6) . . ? C48 C47 C45 109.5(6) . . ? C47 C48 C49 109.7(7) . . ? C47 C48 C50 109.2(6) . . ? C49 C48 C50 108.8(7) . . ? C43 C49 C48 110.1(7) . . ? C41 C50 C48 109.6(6) . . ? B2 C51 S5 112.7(5) . . ? C53 C52 C57 109.3(5) . . ? C53 C52 C61 110.4(6) . . ? C57 C52 C61 107.7(5) . . ? C53 C52 S5 113.6(5) . . ? C57 C52 S5 105.6(5) . . ? C61 C52 S5 109.9(4) . . ? C52 C53 C54 109.7(6) . . ? C55 C54 C53 109.3(7) . . ? C55 C54 C58 109.6(7) . . ? C53 C54 C58 109.7(7) . . ? C54 C55 C56 109.5(6) . . ? C57 C56 C55 109.6(6) . . ? C57 C56 C59 109.7(6) . . ? C55 C56 C59 108.7(7) . . ? C56 C57 C52 109.8(6) . . ? C60 C58 C54 109.5(7) . . ? C60 C59 C56 109.1(6) . . ? C59 C60 C58 109.8(7) . . ? C59 C60 C61 110.3(6) . . ? C58 C60 C61 109.4(6) . . ? C60 C61 C52 109.5(5) . . ? B2 C62 S6 114.0(4) . . ? C64 C63 C67 109.1(6) . . ? C64 C63 C72 110.2(7) . . ? C67 C63 C72 107.9(6) . . ? C64 C63 S6 111.9(5) . . ? C67 C63 S6 111.0(5) . . ? C72 C63 S6 106.7(4) . . ? C63 C64 C65 109.3(6) . . ? C68 C65 C66 110.5(8) . . ? C68 C65 C64 109.7(7) . . ? C66 C65 C64 108.9(8) . . ? C71 C66 C65 108.4(7) . . ? C63 C67 C69 110.1(6) . . ? C69 C68 C65 110.1(7) . . ? C68 C69 C70 108.9(8) . . ? C68 C69 C67 109.3(7) . . ? C70 C69 C67 109.7(7) . . ? C71 C70 C69 109.4(7) . . ? C70 C71 C66 109.8(8) . . ? C70 C71 C72 110.4(7) . . ? C66 C71 C72 109.5(7) . . ? C71 C72 C63 109.2(6) . . ? C78 C73 C74 115.2(6) . . ? C78 C73 B2 121.3(6) . . ? C74 C73 B2 123.4(6) . . ? C75 C74 C73 122.4(7) . . ? C74 C75 C76 120.2(8) . . ? C77 C76 C75 119.1(8) . . ? C76 C77 C78 120.2(8) . . ? C77 C78 C73 123.0(7) . . ? Cl1 C79 Cl1A 70.2(8) . . ? Cl1 C79 Cl3 125.7(12) . . ? Cl1A C79 Cl3 141.0(12) . . ? Cl1 C79 Cl2 106.3(10) . . ? Cl1A C79 Cl2 38.2(5) . . ? Cl3 C79 Cl2 107.6(10) . . ? Cl1 C79 Cl3A 139.2(12) . . ? Cl1A C79 Cl3A 101.1(10) . . ? Cl3 C79 Cl3A 41.9(6) . . ? Cl2 C79 Cl3A 65.6(8) . . ? Cl1 C79 Cl2A 44.3(6) . . ? Cl1A C79 Cl2A 100.4(9) . . ? Cl3 C79 Cl2A 81.9(9) . . ? Cl2 C79 Cl2A 120.8(10) . . ? Cl3A C79 Cl2A 103.1(9) . . ? Cl5A C80 Cl5 36.6(9) . . ? Cl5A C80 Cl4A 116.0(17) . . ? Cl5 C80 Cl4A 107.0(14) . . ? Cl5A C80 Cl4 76.3(13) . . ? Cl5 C80 Cl4 112.5(15) . . ? Cl4A C80 Cl4 108.8(14) . . ? Cl5A C80 Cl6 105.4(15) . . ? Cl5 C80 Cl6 111.4(14) . . ? Cl4A C80 Cl6 22.9(5) . . ? Cl4 C80 Cl6 86.8(11) . . ? Cl6 Cl4A C80 91.2(14) . . ? Cl4A Cl6 C80 66.0(13) . . ? Cl8 C81 Cl7A 126.4(9) . . ? Cl8 C81 Cl9 111.7(9) . . ? Cl7A C81 Cl9 104.7(8) . . ? Cl8 C81 Cl8A 23.4(3) . . ? Cl7A C81 Cl8A 110.6(8) . . ? Cl9 C81 Cl8A 104.5(8) . . ? Cl8 C81 Cl7 110.3(9) . . ? Cl7A C81 Cl7 20.5(4) . . ? Cl9 C81 Cl7 125.1(8) . . ? Cl8A C81 Cl7 100.1(8) . . ? Cl10 C82 Cl11 111.7(5) . . ? Cl10 C82 Cl12 110.0(4) . . ? Cl11 C82 Cl12 108.7(5) . . ? Cl13 C83 Cl14 110.3(4) . . ? Cl13 C83 Cl15 111.7(4) . . ? Cl14 C83 Cl15 109.6(4) . . ? #loop_ #_geom_hbond_atom_site_label_D #_geom_hbond_atom_site_label_H #_geom_hbond_atom_site_label_A #_geom_hbond_distance_DH #_geom_hbond_distance_HA #_geom_hbond_distance_DA #_geom_hbond_angle_DHA #_geom_hbond_site_symmetry_A _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.949 _refine_diff_density_min -2.295 _refine_diff_density_rms 0.145 #===END data_cgr121 _database_code_CSD 199594 _audit_creation_method SHELXL-97 _chemical_name_systematic ; C42 H65 B Ni O P S3, C4H8O, 0.5C5H12 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48.50 H79 B Ni O P S3' _chemical_formula_weight 874.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' _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 15.0616(18) _cell_length_b 19.580(2) _cell_length_c 15.6526(19) _cell_angle_alpha 90.00 _cell_angle_beta 93.736(2) _cell_angle_gamma 90.00 _cell_volume 4606.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 0.627 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8342 _exptl_absorpt_correction_T_max 0.8342 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28794 _diffrn_reflns_av_R_equivalents 0.0194 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.32 _reflns_number_total 10739 _reflns_number_gt 9572 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0595P)^2^+1.8704P] 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 10739 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0996 _refine_ls_wR_factor_gt 0.0963 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.007 _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 Ni1 Ni 0.329223(13) 0.236140(10) 1.019723(13) 0.01608(6) Uani 1 1 d . . . S1 S 0.22067(2) 0.274080(19) 0.92256(2) 0.01629(9) Uani 1 1 d . . . S2 S 0.27570(2) 0.127088(18) 1.02132(2) 0.01593(8) Uani 1 1 d . . . S3 S 0.42917(2) 0.219058(19) 0.91850(2) 0.01607(8) Uani 1 1 d . . . P1 P 0.36724(3) 0.29615(2) 1.13473(3) 0.01637(9) Uani 1 1 d . . . B1 B 0.27408(11) 0.15101(9) 0.83697(11) 0.0162(3) Uani 1 1 d . . . C1 C 0.18942(10) 0.20168(8) 0.85384(10) 0.0189(3) Uani 1 1 d . . . H1A H 0.1428 0.1749 0.8805 0.023 Uiso 1 1 calc R . . H1B H 0.1637 0.2189 0.7981 0.023 Uiso 1 1 calc R . . C2 C 0.11618(10) 0.30103(8) 0.96654(10) 0.0162(3) Uani 1 1 d . . . C3 C 0.13585(11) 0.36807(8) 1.01505(10) 0.0182(3) Uani 1 1 d . . . H3A H 0.1810 0.3600 1.0628 0.022 Uiso 1 1 calc R . . H3B H 0.1600 0.4021 0.9760 0.022 Uiso 1 1 calc R . . C4 C 0.08048(11) 0.24850(8) 1.02836(11) 0.0190(3) Uani 1 1 d . . . H4A H 0.1254 0.2401 1.0762 0.023 Uiso 1 1 calc R . . H4B H 0.0685 0.2048 0.9981 0.023 Uiso 1 1 calc R . . C5 C 0.04649(10) 0.31457(8) 0.89270(10) 0.0195(3) Uani 1 1 d . . . H5A H 0.0337 0.2717 0.8606 0.023 Uiso 1 1 calc R . . H5B H 0.0699 0.3484 0.8528 0.023 Uiso 1 1 calc R . . C6 C 0.05022(11) 0.39555(8) 1.05031(11) 0.0213(3) Uani 1 1 d . . . H6A H 0.0634 0.4392 1.0819 0.026 Uiso 1 1 calc R . . C7 C 0.01400(12) 0.34280(9) 1.11151(11) 0.0238(3) Uani 1 1 d . . . H7A H 0.0584 0.3346 1.1599 0.029 Uiso 1 1 calc R . . H7B H -0.0410 0.3604 1.1350 0.029 Uiso 1 1 calc R . . C8 C -0.00601(11) 0.27578(9) 1.06355(11) 0.0225(3) Uani 1 1 d . . . H8A H -0.0297 0.2415 1.1036 0.027 Uiso 1 1 calc R . . C9 C -0.07544(11) 0.28903(10) 0.98906(12) 0.0262(4) Uani 1 1 d . . . H9A H -0.0889 0.2459 0.9578 0.031 Uiso 1 1 calc R . . H9B H -0.1312 0.3061 1.0116 0.031 Uiso 1 1 calc R . . C10 C -0.03952(11) 0.34187(9) 0.92805(11) 0.0222(3) Uani 1 1 d . . . H10A H -0.0848 0.3503 0.8796 0.027 Uiso 1 1 calc R . . C11 C -0.01958(11) 0.40880(9) 0.97606(11) 0.0235(3) Uani 1 1 d . . . H11A H -0.0748 0.4269 0.9986 0.028 Uiso 1 1 calc R . . H11B H 0.0032 0.4431 0.9365 0.028 Uiso 1 1 calc R . . C12 C 0.29082(11) 0.09412(8) 0.91476(10) 0.0181(3) Uani 1 1 d . . . H12A H 0.3521 0.0762 0.9133 0.022 Uiso 1 1 calc R . . H12B H 0.2494 0.0554 0.9035 0.022 Uiso 1 1 calc R . . C13 C 0.33053(10) 0.06409(7) 1.09425(10) 0.0150(3) Uani 1 1 d . . . C14 C 0.31449(10) 0.08741(8) 1.18538(10) 0.0179(3) Uani 1 1 d . . . H14A H 0.2498 0.0913 1.1921 0.021 Uiso 1 1 calc R . . H14B H 0.3417 0.1329 1.1961 0.021 Uiso 1 1 calc R . . C15 C 0.43072(10) 0.05928(8) 1.08402(10) 0.0176(3) Uani 1 1 d . . . H15A H 0.4587 0.1045 1.0944 0.021 Uiso 1 1 calc R . . H15B H 0.4416 0.0449 1.0250 0.021 Uiso 1 1 calc R . . C16 C 0.28733(11) -0.00618(8) 1.07834(11) 0.0203(3) Uani 1 1 d . . . H16A H 0.2225 -0.0029 1.0844 0.024 Uiso 1 1 calc R . . H16B H 0.2968 -0.0215 1.0194 0.024 Uiso 1 1 calc R . . C17 C 0.35553(10) 0.03549(8) 1.25026(10) 0.0193(3) Uani 1 1 d . . . H17A H 0.3451 0.0509 1.3097 0.023 Uiso 1 1 calc R . . C18 C 0.45597(10) 0.03037(8) 1.23984(10) 0.0205(3) Uani 1 1 d . . . H18A H 0.4830 -0.0027 1.2817 0.025 Uiso 1 1 calc R . . H18B H 0.4842 0.0754 1.2510 0.025 Uiso 1 1 calc R . . C19 C 0.47178(10) 0.00702(8) 1.14848(10) 0.0202(3) Uani 1 1 d . . . H19A H 0.5372 0.0036 1.1417 0.024 Uiso 1 1 calc R . . C20 C 0.42885(12) -0.06287(8) 1.13269(11) 0.0238(3) Uani 1 1 d . . . H20A H 0.4558 -0.0964 1.1740 0.029 Uiso 1 1 calc R . . H20B H 0.4396 -0.0787 1.0742 0.029 Uiso 1 1 calc R . . C21 C 0.32846(11) -0.05801(8) 1.14293(11) 0.0226(3) Uani 1 1 d . . . H21A H 0.3005 -0.1038 1.1322 0.027 Uiso 1 1 calc R . . C22 C 0.31226(11) -0.03442(9) 1.23405(11) 0.0230(3) Uani 1 1 d . . . H22A H 0.2475 -0.0313 1.2410 0.028 Uiso 1 1 calc R . . H22B H 0.3380 -0.0679 1.2760 0.028 Uiso 1 1 calc R . . C23 C 0.36405(10) 0.19636(8) 0.82085(10) 0.0185(3) Uani 1 1 d . . . H23A H 0.3459 0.2388 0.7900 0.022 Uiso 1 1 calc R . . H23B H 0.4021 0.1700 0.7836 0.022 Uiso 1 1 calc R . . C24 C 0.50110(10) 0.28913(8) 0.88578(10) 0.0164(3) Uani 1 1 d . . . C25 C 0.56747(10) 0.30415(8) 0.96148(10) 0.0187(3) Uani 1 1 d . . . H25A H 0.6016 0.2623 0.9773 0.022 Uiso 1 1 calc R . . H25B H 0.5351 0.3186 1.0115 0.022 Uiso 1 1 calc R . . C26 C 0.44755(10) 0.35370(8) 0.86199(11) 0.0196(3) Uani 1 1 d . . . H26A H 0.4145 0.3687 0.9113 0.024 Uiso 1 1 calc R . . H26B H 0.4040 0.3440 0.8134 0.024 Uiso 1 1 calc R . . C27 C 0.55215(11) 0.26603(8) 0.80917(10) 0.0185(3) Uani 1 1 d . . . H27A H 0.5863 0.2241 0.8243 0.022 Uiso 1 1 calc R . . H27B H 0.5097 0.2555 0.7600 0.022 Uiso 1 1 calc R . . C28 C 0.63149(11) 0.36101(8) 0.93722(11) 0.0213(3) Uani 1 1 d . . . H28A H 0.6746 0.3710 0.9869 0.026 Uiso 1 1 calc R . . C29 C 0.57831(12) 0.42565(9) 0.91244(12) 0.0251(4) Uani 1 1 d . . . H29A H 0.5462 0.4416 0.9619 0.030 Uiso 1 1 calc R . . H29B H 0.6194 0.4623 0.8966 0.030 Uiso 1 1 calc R . . C30 C 0.51181(11) 0.41049(8) 0.83697(11) 0.0230(3) Uani 1 1 d . . . H30A H 0.4772 0.4528 0.8214 0.028 Uiso 1 1 calc R . . C31 C 0.56189(12) 0.38702(9) 0.76012(11) 0.0244(3) Uani 1 1 d . . . H31A H 0.6022 0.4237 0.7429 0.029 Uiso 1 1 calc R . . H31B H 0.5190 0.3770 0.7111 0.029 Uiso 1 1 calc R . . C32 C 0.61587(11) 0.32282(8) 0.78430(10) 0.0206(3) Uani 1 1 d . . . H32A H 0.6489 0.3076 0.7343 0.025 Uiso 1 1 calc R . . C33 C 0.68205(11) 0.33765(9) 0.86057(11) 0.0227(3) Uani 1 1 d . . . H33A H 0.7241 0.3737 0.8450 0.027 Uiso 1 1 calc R . . H33B H 0.7167 0.2959 0.8759 0.027 Uiso 1 1 calc R . . C34 C 0.25144(10) 0.10459(8) 0.75128(10) 0.0165(3) Uani 1 1 d . . . C35 C 0.31714(11) 0.06383(8) 0.71752(11) 0.0210(3) Uani 1 1 d . . . H35A H 0.3761 0.0661 0.7430 0.025 Uiso 1 1 calc R . . C36 C 0.29992(12) 0.02030(9) 0.64853(11) 0.0248(3) Uani 1 1 d . . . H36A H 0.3467 -0.0062 0.6277 0.030 Uiso 1 1 calc R . . C37 C 0.21475(12) 0.01535(9) 0.60982(11) 0.0248(3) Uani 1 1 d . . . H37A H 0.2025 -0.0142 0.5624 0.030 Uiso 1 1 calc R . . C38 C 0.14794(11) 0.05445(9) 0.64179(11) 0.0236(3) Uani 1 1 d . . . H38A H 0.0891 0.0515 0.6162 0.028 Uiso 1 1 calc R . . C39 C 0.16608(11) 0.09800(8) 0.71095(10) 0.0206(3) Uani 1 1 d . . . H39A H 0.1189 0.1242 0.7316 0.025 Uiso 1 1 calc R . . C40 C 0.29607(12) 0.29546(9) 1.22525(11) 0.0239(3) Uani 1 1 d . . . H40A H 0.3224 0.3246 1.2711 0.036 Uiso 1 1 calc R . . H40B H 0.2909 0.2486 1.2465 0.036 Uiso 1 1 calc R . . H40C H 0.2369 0.3128 1.2066 0.036 Uiso 1 1 calc R . . C41 C 0.47308(11) 0.27184(9) 1.19002(12) 0.0252(4) Uani 1 1 d . . . H41A H 0.4848 0.3011 1.2403 0.038 Uiso 1 1 calc R . . H41B H 0.5210 0.2773 1.1512 0.038 Uiso 1 1 calc R . . H41C H 0.4702 0.2241 1.2083 0.038 Uiso 1 1 calc R . . C42 C 0.38360(12) 0.38813(8) 1.12142(11) 0.0232(3) Uani 1 1 d . . . H42A H 0.4003 0.4088 1.1772 0.035 Uiso 1 1 calc R . . H42B H 0.3282 0.4089 1.0974 0.035 Uiso 1 1 calc R . . H42C H 0.4310 0.3960 1.0825 0.035 Uiso 1 1 calc R . . C43 C 0.79690(18) 0.09247(12) 0.16778(19) 0.0560(7) Uani 1 1 d . . . H43A H 0.8316 0.0706 0.2162 0.067 Uiso 1 1 calc R . . H43B H 0.7939 0.0609 0.1183 0.067 Uiso 1 1 calc R . . C44 C 0.7083(2) 0.11027(17) 0.1916(2) 0.0747(9) Uani 1 1 d . . . H44A H 0.7095 0.1252 0.2521 0.090 Uiso 1 1 calc R . . H44B H 0.6673 0.0709 0.1836 0.090 Uiso 1 1 calc R . . C45 C 0.67980(19) 0.16779(16) 0.1324(2) 0.0696(8) Uani 1 1 d . . . H45A H 0.6437 0.1507 0.0817 0.084 Uiso 1 1 calc R . . H45B H 0.6450 0.2023 0.1621 0.084 Uiso 1 1 calc R . . C46 C 0.7651(2) 0.19642(17) 0.1076(2) 0.0714(9) Uani 1 1 d . . . H46A H 0.7673 0.1960 0.0445 0.086 Uiso 1 1 calc R . . H46B H 0.7716 0.2442 0.1278 0.086 Uiso 1 1 calc R . . C47 C -0.0030(3) 0.0136(2) 1.0432(3) 0.126(2) Uani 1 1 d . . . H47A H -0.0563 0.0431 1.0443 0.151 Uiso 1 1 calc R . . H47B H 0.0500 0.0422 1.0581 0.151 Uiso 1 1 calc R . . C48 C -0.0087(5) -0.0438(3) 1.1115(4) 0.175(4) Uani 1 1 d . . . H48A H -0.0024 -0.0228 1.1692 0.210 Uiso 1 1 calc R . . H48B H -0.0685 -0.0650 1.1049 0.210 Uiso 1 1 calc R . . C49 C 0.0434(3) -0.0856(3) 1.1078(4) 0.0519(14) Uani 0.50 1 d P . . H49A H 0.0359 -0.1192 1.1531 0.078 Uiso 0.50 1 calc PR . . H49B H 0.1030 -0.0654 1.1153 0.078 Uiso 0.50 1 calc PR . . H49C H 0.0364 -0.1080 1.0518 0.078 Uiso 0.50 1 calc PR . . O1 O 0.83535(13) 0.15501(11) 0.14635(15) 0.0683(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01761(11) 0.01576(11) 0.01471(11) -0.00037(7) -0.00010(8) -0.00005(7) S1 0.01757(18) 0.01554(17) 0.01574(18) -0.00063(14) 0.00087(14) 0.00213(13) S2 0.01773(17) 0.01481(18) 0.01529(18) 0.00098(13) 0.00142(14) 0.00138(13) S3 0.01607(17) 0.01547(17) 0.01674(18) -0.00060(14) 0.00148(14) -0.00097(13) P1 0.01816(19) 0.01585(19) 0.01501(19) -0.00023(14) 0.00022(15) -0.00105(14) B1 0.0173(8) 0.0163(8) 0.0148(8) -0.0011(6) -0.0003(6) 0.0011(6) C1 0.0200(7) 0.0191(7) 0.0172(7) -0.0041(6) -0.0025(6) 0.0024(6) C2 0.0174(7) 0.0156(7) 0.0154(7) -0.0002(6) 0.0009(6) 0.0030(5) C3 0.0223(7) 0.0157(7) 0.0164(7) 0.0003(6) 0.0005(6) 0.0013(6) C4 0.0218(8) 0.0166(7) 0.0186(8) 0.0016(6) 0.0016(6) 0.0009(6) C5 0.0211(7) 0.0208(8) 0.0163(7) -0.0001(6) -0.0012(6) 0.0036(6) C6 0.0266(8) 0.0182(7) 0.0192(8) -0.0021(6) 0.0034(6) 0.0037(6) C7 0.0270(8) 0.0278(9) 0.0172(8) 0.0016(7) 0.0059(6) 0.0046(7) C8 0.0230(8) 0.0231(8) 0.0221(8) 0.0041(6) 0.0058(7) 0.0008(6) C9 0.0183(8) 0.0294(9) 0.0310(9) 0.0004(7) 0.0015(7) 0.0003(6) C10 0.0187(7) 0.0268(8) 0.0210(8) 0.0005(7) -0.0005(6) 0.0051(6) C11 0.0246(8) 0.0231(8) 0.0229(8) 0.0021(7) 0.0037(7) 0.0083(6) C12 0.0222(7) 0.0168(7) 0.0151(7) -0.0012(6) -0.0002(6) -0.0001(6) C13 0.0160(7) 0.0135(7) 0.0157(7) 0.0021(5) 0.0016(6) 0.0007(5) C14 0.0194(7) 0.0182(7) 0.0165(7) 0.0008(6) 0.0040(6) 0.0027(6) C15 0.0166(7) 0.0202(7) 0.0162(7) 0.0006(6) 0.0024(6) 0.0003(6) C16 0.0225(8) 0.0174(7) 0.0208(8) 0.0012(6) -0.0011(6) -0.0031(6) C17 0.0227(7) 0.0209(8) 0.0148(7) 0.0015(6) 0.0035(6) 0.0032(6) C18 0.0213(7) 0.0220(8) 0.0178(8) 0.0012(6) -0.0012(6) 0.0027(6) C19 0.0178(7) 0.0241(8) 0.0190(8) 0.0012(6) 0.0028(6) 0.0053(6) C20 0.0320(9) 0.0185(8) 0.0210(8) 0.0010(6) 0.0019(7) 0.0078(6) C21 0.0292(8) 0.0151(7) 0.0231(8) 0.0026(6) -0.0002(7) -0.0023(6) C22 0.0243(8) 0.0224(8) 0.0227(8) 0.0078(7) 0.0036(7) -0.0011(6) C23 0.0202(7) 0.0198(7) 0.0153(7) -0.0021(6) 0.0004(6) -0.0017(6) C24 0.0166(7) 0.0147(7) 0.0181(7) -0.0005(6) 0.0031(6) -0.0004(5) C25 0.0204(7) 0.0188(7) 0.0170(7) -0.0006(6) 0.0019(6) -0.0013(6) C26 0.0201(7) 0.0175(7) 0.0216(8) 0.0009(6) 0.0037(6) 0.0018(6) C27 0.0200(7) 0.0177(7) 0.0179(8) -0.0019(6) 0.0032(6) 0.0004(6) C28 0.0215(8) 0.0216(8) 0.0209(8) -0.0025(6) 0.0011(6) -0.0053(6) C29 0.0304(9) 0.0182(8) 0.0273(9) -0.0035(7) 0.0067(7) -0.0044(6) C30 0.0260(8) 0.0160(7) 0.0272(9) 0.0033(6) 0.0045(7) 0.0017(6) C31 0.0269(8) 0.0234(8) 0.0234(8) 0.0049(7) 0.0049(7) -0.0021(7) C32 0.0222(7) 0.0212(8) 0.0191(8) -0.0009(6) 0.0075(6) -0.0015(6) C33 0.0189(7) 0.0247(8) 0.0249(8) 0.0006(7) 0.0047(6) -0.0038(6) C34 0.0200(7) 0.0147(7) 0.0150(7) 0.0016(6) 0.0014(6) -0.0009(5) C35 0.0195(7) 0.0227(8) 0.0207(8) -0.0016(6) 0.0008(6) -0.0008(6) C36 0.0271(8) 0.0237(8) 0.0240(8) -0.0070(7) 0.0056(7) 0.0008(7) C37 0.0338(9) 0.0232(8) 0.0172(8) -0.0051(6) -0.0005(7) -0.0037(7) C38 0.0244(8) 0.0255(8) 0.0202(8) 0.0006(7) -0.0049(6) -0.0030(6) C39 0.0210(7) 0.0208(8) 0.0199(8) -0.0003(6) 0.0005(6) 0.0012(6) C40 0.0273(8) 0.0237(8) 0.0214(8) -0.0019(7) 0.0067(7) -0.0037(6) C41 0.0229(8) 0.0295(9) 0.0224(8) 0.0020(7) -0.0047(7) -0.0012(7) C42 0.0281(8) 0.0175(8) 0.0241(8) -0.0007(6) 0.0024(7) -0.0041(6) C43 0.0620(16) 0.0368(12) 0.0656(17) -0.0101(12) -0.0230(13) 0.0000(11) C44 0.078(2) 0.071(2) 0.078(2) 0.0306(17) 0.0214(17) -0.0071(16) C45 0.0481(15) 0.0691(19) 0.092(2) 0.0221(17) 0.0106(15) 0.0108(13) C46 0.0734(19) 0.0677(19) 0.071(2) 0.0319(16) -0.0076(16) -0.0228(15) C47 0.109(3) 0.122(4) 0.158(4) -0.085(3) 0.085(3) -0.066(3) C48 0.248(8) 0.151(5) 0.140(5) -0.082(4) 0.123(5) -0.137(5) C49 0.041(3) 0.056(3) 0.057(3) 0.023(3) -0.012(2) -0.013(2) O1 0.0477(10) 0.0736(14) 0.0835(15) 0.0097(12) 0.0041(10) -0.0101(9) _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 Ni1 P1 2.1942(5) . ? Ni1 S3 2.2801(5) . ? Ni1 S2 2.2831(5) . ? Ni1 S1 2.2834(5) . ? S1 C1 1.8227(16) . ? S1 C2 1.8357(15) . ? S2 C12 1.8166(16) . ? S2 C13 1.8396(15) . ? S3 C23 1.8168(16) . ? S3 C24 1.8414(16) . ? P1 C41 1.8267(17) . ? P1 C42 1.8315(17) . ? P1 C40 1.8316(17) . ? B1 C34 1.638(2) . ? B1 C1 1.650(2) . ? B1 C23 1.653(2) . ? B1 C12 1.657(2) . ? C2 C4 1.533(2) . ? C2 C5 1.533(2) . ? C2 C3 1.536(2) . ? C3 C6 1.533(2) . ? C4 C8 1.542(2) . ? C5 C10 1.537(2) . ? C6 C7 1.533(2) . ? C6 C11 1.537(2) . ? C7 C8 1.532(2) . ? C8 C9 1.537(2) . ? C9 C10 1.531(2) . ? C10 C11 1.531(2) . ? C13 C15 1.531(2) . ? C13 C14 1.532(2) . ? C13 C16 1.535(2) . ? C14 C17 1.538(2) . ? C15 C19 1.538(2) . ? C16 C21 1.534(2) . ? C17 C22 1.530(2) . ? C17 C18 1.535(2) . ? C18 C19 1.535(2) . ? C19 C20 1.527(2) . ? C20 C21 1.534(2) . ? C21 C22 1.534(2) . ? C24 C25 1.528(2) . ? C24 C26 1.533(2) . ? C24 C27 1.534(2) . ? C25 C28 1.537(2) . ? C26 C30 1.542(2) . ? C27 C32 1.535(2) . ? C28 C33 1.532(2) . ? C28 C29 1.534(2) . ? C29 C30 1.527(2) . ? C30 C31 1.531(2) . ? C31 C32 1.531(2) . ? C32 C33 1.532(2) . ? C34 C39 1.401(2) . ? C34 C35 1.401(2) . ? C35 C36 1.387(2) . ? C36 C37 1.386(2) . ? C37 C38 1.384(2) . ? C38 C39 1.391(2) . ? C43 O1 1.404(3) . ? C43 C44 1.452(4) . ? C44 C45 1.503(4) . ? C45 C46 1.476(4) . ? C46 O1 1.436(4) . ? C47 C47 1.461(8) 3_557 ? C47 C48 1.558(8) . ? C48 C49 1.138(8) . ? 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 P1 Ni1 S3 119.986(18) . . ? P1 Ni1 S2 124.423(17) . . ? S3 Ni1 S2 96.890(16) . . ? P1 Ni1 S1 120.629(17) . . ? S3 Ni1 S1 93.522(18) . . ? S2 Ni1 S1 94.217(16) . . ? C1 S1 C2 104.49(7) . . ? C1 S1 Ni1 106.63(5) . . ? C2 S1 Ni1 115.97(5) . . ? C12 S2 C13 104.68(7) . . ? C12 S2 Ni1 104.88(5) . . ? C13 S2 Ni1 119.30(5) . . ? C23 S3 C24 104.09(7) . . ? C23 S3 Ni1 106.02(5) . . ? C24 S3 Ni1 120.73(5) . . ? C41 P1 C42 100.98(8) . . ? C41 P1 C40 99.69(8) . . ? C42 P1 C40 100.66(8) . . ? C41 P1 Ni1 114.97(6) . . ? C42 P1 Ni1 117.59(6) . . ? C40 P1 Ni1 119.74(6) . . ? C34 B1 C1 110.05(12) . . ? C34 B1 C23 107.59(12) . . ? C1 B1 C23 110.56(13) . . ? C34 B1 C12 104.02(12) . . ? C1 B1 C12 111.63(13) . . ? C23 B1 C12 112.72(12) . . ? B1 C1 S1 112.92(10) . . ? C4 C2 C5 109.92(13) . . ? C4 C2 C3 109.00(13) . . ? C5 C2 C3 108.99(12) . . ? C4 C2 S1 112.85(10) . . ? C5 C2 S1 109.19(11) . . ? C3 C2 S1 106.78(10) . . ? C6 C3 C2 109.77(13) . . ? C2 C4 C8 109.40(13) . . ? C2 C5 C10 109.91(13) . . ? C3 C6 C7 109.30(13) . . ? C3 C6 C11 109.69(13) . . ? C7 C6 C11 109.42(14) . . ? C8 C7 C6 109.73(13) . . ? C7 C8 C9 109.25(14) . . ? C7 C8 C4 109.14(14) . . ? C9 C8 C4 109.65(14) . . ? C10 C9 C8 109.68(14) . . ? C9 C10 C11 109.78(14) . . ? C9 C10 C5 109.27(14) . . ? C11 C10 C5 109.35(14) . . ? C10 C11 C6 109.23(13) . . ? B1 C12 S2 114.43(10) . . ? C15 C13 C14 109.40(12) . . ? C15 C13 C16 109.77(13) . . ? C14 C13 C16 109.10(13) . . ? C15 C13 S2 112.46(10) . . ? C14 C13 S2 106.63(10) . . ? C16 C13 S2 109.38(10) . . ? C13 C14 C17 109.68(12) . . ? C13 C15 C19 109.22(12) . . ? C21 C16 C13 109.71(13) . . ? C22 C17 C18 109.63(13) . . ? C22 C17 C14 109.47(13) . . ? C18 C17 C14 109.23(13) . . ? C17 C18 C19 109.40(13) . . ? C20 C19 C15 110.02(13) . . ? C20 C19 C18 109.15(14) . . ? C15 C19 C18 109.44(13) . . ? C19 C20 C21 109.72(13) . . ? C16 C21 C22 109.37(14) . . ? C16 C21 C20 109.31(13) . . ? C22 C21 C20 109.48(14) . . ? C17 C22 C21 109.38(13) . . ? B1 C23 S3 113.95(11) . . ? C25 C24 C26 109.69(13) . . ? C25 C24 C27 109.08(12) . . ? C26 C24 C27 109.62(13) . . ? C25 C24 S3 107.14(11) . . ? C26 C24 S3 111.86(10) . . ? C27 C24 S3 109.37(10) . . ? C24 C25 C28 109.70(13) . . ? C24 C26 C30 109.13(13) . . ? C32 C27 C24 109.76(13) . . ? C33 C28 C29 109.04(14) . . ? C33 C28 C25 109.22(13) . . ? C29 C28 C25 109.54(13) . . ? C30 C29 C28 109.91(13) . . ? C31 C30 C29 109.52(14) . . ? C31 C30 C26 109.43(14) . . ? C29 C30 C26 109.55(14) . . ? C30 C31 C32 109.45(14) . . ? C33 C32 C31 110.18(14) . . ? C33 C32 C27 108.99(13) . . ? C31 C32 C27 109.06(13) . . ? C32 C33 C28 109.59(13) . . ? C39 C34 C35 115.31(14) . . ? C39 C34 B1 123.80(14) . . ? C35 C34 B1 120.70(13) . . ? C36 C35 C34 122.88(15) . . ? C35 C36 C37 120.27(16) . . ? C38 C37 C36 118.52(15) . . ? C37 C38 C39 120.66(15) . . ? C38 C39 C34 122.35(15) . . ? O1 C43 C44 104.6(2) . . ? C43 C44 C45 104.6(2) . . ? C46 C45 C44 103.2(2) . . ? O1 C46 C45 107.7(2) . . ? C47 C47 C48 112.5(5) 3_557 . ? C49 C48 C47 114.4(5) . . ? C43 O1 C46 106.8(2) . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.642 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.068 #===END data_cgr124 _database_code_CSD 199595 _audit_creation_method SHELXL-97 _chemical_name_systematic ; C50 H73 B Ni S, C2H6O (ACETONE)? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H79 B Ni O S4' _chemical_formula_weight 929.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' _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 13.198(4) _cell_length_b 13.392(4) _cell_length_c 15.607(5) _cell_angle_alpha 88.952(7) _cell_angle_beta 66.668(6) _cell_angle_gamma 80.078(6) _cell_volume 2491.3(13) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 0.594 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8905 _exptl_absorpt_correction_T_max 0.9162 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15874 _diffrn_reflns_av_R_equivalents 0.0779 _diffrn_reflns_av_sigmaI/netI 0.2425 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9626 _reflns_number_gt 3545 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0900P)^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 9626 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1882 _refine_ls_R_factor_gt 0.0901 _refine_ls_wR_factor_ref 0.2531 _refine_ls_wR_factor_gt 0.2109 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 Ni1 Ni 0.88204(8) 0.83803(7) 0.26270(7) 0.0410(3) Uani 1 1 d . . . S1 S 0.72986(17) 0.77410(14) 0.31642(14) 0.0434(5) Uani 1 1 d . . . S2 S 0.93754(16) 0.79187(14) 0.37835(13) 0.0407(5) Uani 1 1 d . . . S3 S 0.57534(18) 0.71795(15) 0.63578(15) 0.0520(6) Uani 1 1 d . . . S4 S 1.02301(18) 0.88625(15) 0.15436(15) 0.0504(6) Uani 1 1 d . . . B1 B 0.7062(7) 0.8462(6) 0.5007(6) 0.041(2) Uani 1 1 d . . . C1 C 0.6418(6) 0.8208(6) 0.4367(5) 0.045(2) Uani 1 1 d . . . H1A H 0.5906 0.8826 0.4352 0.054 Uiso 1 1 calc R . . H1B H 0.5958 0.7700 0.4673 0.054 Uiso 1 1 calc R . . C2 C 0.6363(6) 0.7956(5) 0.2538(5) 0.0378(19) Uani 1 1 d . . . C3 C 0.6949(6) 0.7435(5) 0.1582(5) 0.043(2) Uani 1 1 d . . . H3A H 0.7623 0.7721 0.1232 0.052 Uiso 1 1 calc R . . H3B H 0.7187 0.6712 0.1642 0.052 Uiso 1 1 calc R . . C4 C 0.6220(7) 0.7544(6) 0.1046(6) 0.052(2) Uani 1 1 d . . . H4A H 0.6646 0.7212 0.0413 0.062 Uiso 1 1 calc R . . C5 C 0.5833(7) 0.8680(6) 0.0974(5) 0.057(2) Uani 1 1 d . . . H5A H 0.6485 0.9000 0.0637 0.068 Uiso 1 1 calc R . . H5B H 0.5350 0.8767 0.0626 0.068 Uiso 1 1 calc R . . C6 C 0.5334(7) 0.7457(6) 0.3073(6) 0.052(2) Uani 1 1 d . . . H6A H 0.5580 0.6734 0.3128 0.063 Uiso 1 1 calc R . . H6B H 0.4928 0.7778 0.3705 0.063 Uiso 1 1 calc R . . C7 C 0.5973(7) 0.9078(5) 0.2451(6) 0.051(2) Uani 1 1 d . . . H7A H 0.5577 0.9422 0.3074 0.062 Uiso 1 1 calc R . . H7B H 0.6622 0.9398 0.2105 0.062 Uiso 1 1 calc R . . C8 C 0.5196(7) 0.9177(6) 0.1940(6) 0.054(2) Uani 1 1 d . . . H8A H 0.4941 0.9907 0.1887 0.065 Uiso 1 1 calc R . . C9 C 0.4171(7) 0.8691(7) 0.2473(6) 0.060(3) Uani 1 1 d . . . H9A H 0.3758 0.9024 0.3099 0.072 Uiso 1 1 calc R . . H9B H 0.3668 0.8774 0.2143 0.072 Uiso 1 1 calc R . . C10 C 0.4555(7) 0.7580(6) 0.2547(6) 0.052(2) Uani 1 1 d . . . H10A H 0.3897 0.7257 0.2889 0.062 Uiso 1 1 calc R . . C11 C 0.5212(7) 0.7058(7) 0.1559(6) 0.061(3) Uani 1 1 d . . . H11A H 0.5454 0.6333 0.1607 0.073 Uiso 1 1 calc R . . H11B H 0.4727 0.7128 0.1213 0.073 Uiso 1 1 calc R . . C12 C 0.8208(6) 0.7598(5) 0.4782(5) 0.048(2) Uani 1 1 d . . . H12A H 0.8067 0.6933 0.4654 0.057 Uiso 1 1 calc R . . H12B H 0.8399 0.7553 0.5329 0.057 Uiso 1 1 calc R . . C13 C 1.0411(6) 0.6737(5) 0.3379(5) 0.0392(19) Uani 1 1 d . . . C14 C 1.0076(6) 0.6002(5) 0.2849(5) 0.047(2) Uani 1 1 d . . . H14A H 0.9358 0.5818 0.3257 0.056 Uiso 1 1 calc R . . H14B H 0.9984 0.6327 0.2310 0.056 Uiso 1 1 calc R . . C15 C 1.1537(6) 0.7016(5) 0.2740(5) 0.044(2) Uani 1 1 d . . . H15A H 1.1464 0.7361 0.2203 0.052 Uiso 1 1 calc R . . H15B H 1.1761 0.7481 0.3082 0.052 Uiso 1 1 calc R . . C16 C 1.0556(6) 0.6232(5) 0.4215(6) 0.050(2) Uani 1 1 d . . . H16A H 0.9844 0.6056 0.4645 0.059 Uiso 1 1 calc R . . H16B H 1.0783 0.6701 0.4552 0.059 Uiso 1 1 calc R . . C17 C 1.1462(7) 0.5264(6) 0.3866(6) 0.053(2) Uani 1 1 d . . . H17A H 1.1544 0.4921 0.4408 0.064 Uiso 1 1 calc R . . C18 C 1.1110(7) 0.4543(6) 0.3324(7) 0.061(3) Uani 1 1 d . . . H18A H 1.1681 0.3926 0.3104 0.073 Uiso 1 1 calc R . . H18B H 1.0400 0.4348 0.3736 0.073 Uiso 1 1 calc R . . C19 C 1.0976(7) 0.5053(6) 0.2518(6) 0.054(2) Uani 1 1 d . . . H19A H 1.0751 0.4581 0.2173 0.065 Uiso 1 1 calc R . . C20 C 1.2096(7) 0.5357(6) 0.1849(6) 0.060(3) Uani 1 1 d . . . H20A H 1.2679 0.4751 0.1605 0.072 Uiso 1 1 calc R . . H20B H 1.1999 0.5703 0.1321 0.072 Uiso 1 1 calc R . . C21 C 1.2430(7) 0.6058(6) 0.2400(6) 0.052(2) Uani 1 1 d . . . H21A H 1.3150 0.6250 0.1985 0.062 Uiso 1 1 calc R . . C22 C 1.2576(7) 0.5544(6) 0.3229(6) 0.057(2) Uani 1 1 d . . . H22A H 1.2807 0.6005 0.3569 0.068 Uiso 1 1 calc R . . H22B H 1.3156 0.4933 0.3014 0.068 Uiso 1 1 calc R . . C23 C 0.6191(6) 0.8393(5) 0.6093(5) 0.046(2) Uani 1 1 d . . . H23A H 0.5524 0.8919 0.6229 0.055 Uiso 1 1 calc R . . H23B H 0.6550 0.8539 0.6508 0.055 Uiso 1 1 calc R . . C24 C 0.4838(6) 0.7267(5) 0.7607(5) 0.0386(19) Uani 1 1 d . . . C25 C 0.4390(7) 0.6284(6) 0.7830(6) 0.053(2) Uani 1 1 d . . . H25A H 0.3970 0.6196 0.7449 0.064 Uiso 1 1 calc R . . H25B H 0.5021 0.5714 0.7668 0.064 Uiso 1 1 calc R . . C26 C 0.3843(6) 0.8126(6) 0.7876(5) 0.051(2) Uani 1 1 d . . . H26A H 0.4108 0.8775 0.7746 0.061 Uiso 1 1 calc R . . H26B H 0.3416 0.8055 0.7497 0.061 Uiso 1 1 calc R . . C27 C 0.5506(6) 0.7408(6) 0.8185(5) 0.048(2) Uani 1 1 d . . . H27A H 0.5761 0.8062 0.8068 0.057 Uiso 1 1 calc R . . H27B H 0.6167 0.6867 0.8011 0.057 Uiso 1 1 calc R . . C28 C 0.4746(8) 0.7372(7) 0.9223(6) 0.061(2) Uani 1 1 d . . . H28A H 0.5178 0.7439 0.9605 0.073 Uiso 1 1 calc R . . C29 C 0.3758(8) 0.8255(7) 0.9487(6) 0.076(3) Uani 1 1 d . . . H29A H 0.4032 0.8900 0.9367 0.091 Uiso 1 1 calc R . . H29B H 0.3278 0.8257 1.0153 0.091 Uiso 1 1 calc R . . C30 C 0.3088(7) 0.8130(6) 0.8896(6) 0.060(3) Uani 1 1 d . . . H30A H 0.2443 0.8698 0.9056 0.071 Uiso 1 1 calc R . . C31 C 0.2675(7) 0.7147(7) 0.9094(7) 0.067(3) Uani 1 1 d . . . H31A H 0.2229 0.7070 0.8733 0.080 Uiso 1 1 calc R . . H31B H 0.2191 0.7146 0.9759 0.080 Uiso 1 1 calc R . . C32 C 0.3643(7) 0.6272(6) 0.8841(6) 0.057(2) Uani 1 1 d . . . H32A H 0.3361 0.5623 0.8967 0.068 Uiso 1 1 calc R . . C33 C 0.4308(8) 0.6397(7) 0.9416(7) 0.075(3) Uani 1 1 d . . . H33A H 0.3828 0.6393 1.0081 0.090 Uiso 1 1 calc R . . H33B H 0.4936 0.5827 0.9264 0.090 Uiso 1 1 calc R . . C34 C 0.7319(6) 0.9606(6) 0.4923(5) 0.043(2) Uani 1 1 d . . . C35 C 0.6757(7) 1.0413(6) 0.4620(5) 0.052(2) Uani 1 1 d . . . H35A H 0.6240 1.0276 0.4382 0.063 Uiso 1 1 calc R . . C36 C 0.6908(8) 1.1396(6) 0.4645(6) 0.061(3) Uani 1 1 d . . . H36A H 0.6487 1.1907 0.4439 0.073 Uiso 1 1 calc R . . C37 C 0.7672(8) 1.1648(6) 0.4971(6) 0.062(3) Uani 1 1 d . . . H37A H 0.7779 1.2322 0.4989 0.074 Uiso 1 1 calc R . . C38 C 0.8277(7) 1.0868(7) 0.5269(6) 0.060(3) Uani 1 1 d . . . H38A H 0.8809 1.1014 0.5486 0.072 Uiso 1 1 calc R . . C39 C 0.8104(7) 0.9874(6) 0.5252(6) 0.053(2) Uani 1 1 d . . . H39A H 0.8520 0.9364 0.5464 0.063 Uiso 1 1 calc R . . C40 C 0.8944(7) 0.8984(7) 0.1446(6) 0.062(3) Uani 1 1 d . . . H40A H 0.8913 0.8541 0.0968 0.075 Uiso 1 1 calc R . . H40B H 0.8532 0.9677 0.1490 0.075 Uiso 1 1 calc R . . C41 C 1.0439(6) 1.0124(6) 0.1819(6) 0.047(2) Uani 1 1 d . . . C42 C 0.9395(6) 1.0779(5) 0.2523(6) 0.047(2) Uani 1 1 d . . . H42A H 0.9115 1.0434 0.3108 0.056 Uiso 1 1 calc R . . H42B H 0.8806 1.0902 0.2280 0.056 Uiso 1 1 calc R . . C43 C 1.1319(7) 0.9898(6) 0.2265(6) 0.054(2) Uani 1 1 d . . . H43A H 1.1009 0.9555 0.2848 0.065 Uiso 1 1 calc R . . H43B H 1.1996 0.9453 0.1836 0.065 Uiso 1 1 calc R . . C44 C 1.0915(7) 1.0638(6) 0.0909(6) 0.050(2) Uani 1 1 d . . . H44A H 1.0367 1.0754 0.0623 0.060 Uiso 1 1 calc R . . H44B H 1.1595 1.0202 0.0474 0.060 Uiso 1 1 calc R . . C45 C 1.1191(7) 1.1648(6) 0.1103(6) 0.054(2) Uani 1 1 d . . . H45A H 1.1494 1.1991 0.0511 0.065 Uiso 1 1 calc R . . C46 C 1.0155(7) 1.2307(6) 0.1771(7) 0.061(3) Uani 1 1 d . . . H46A H 0.9588 1.2428 0.1505 0.073 Uiso 1 1 calc R . . H46B H 1.0327 1.2964 0.1882 0.073 Uiso 1 1 calc R . . C47 C 0.9696(7) 1.1787(6) 0.2699(6) 0.056(2) Uani 1 1 d . . . H47A H 0.9014 1.2232 0.3142 0.067 Uiso 1 1 calc R . . C48 C 1.0550(7) 1.1576(6) 0.3122(6) 0.057(2) Uani 1 1 d . . . H48A H 1.0238 1.1240 0.3708 0.069 Uiso 1 1 calc R . . H48B H 1.0725 1.2219 0.3265 0.069 Uiso 1 1 calc R . . C49 C 1.1609(7) 1.0910(6) 0.2463(6) 0.056(2) Uani 1 1 d . . . H49A H 1.2168 1.0786 0.2746 0.067 Uiso 1 1 calc R . . C50 C 1.2092(7) 1.1429(6) 0.1528(7) 0.062(3) Uani 1 1 d . . . H50A H 1.2765 1.0986 0.1090 0.075 Uiso 1 1 calc R . . H50B H 1.2304 1.2067 0.1636 0.075 Uiso 1 1 calc R . . C51 C 0.6448(12) 1.4822(13) 0.4492(12) 0.196(9) Uani 1 1 d . . . H51A H 0.6371 1.4591 0.5103 0.294 Uiso 1 1 calc R . . H51B H 0.5942 1.4541 0.4293 0.294 Uiso 1 1 calc R . . H51C H 0.6266 1.5558 0.4524 0.294 Uiso 1 1 calc R . . C52 C 0.7608(12) 1.4486(9) 0.3817(11) 0.100(4) Uani 1 1 d . . . C53 C 0.7866(11) 1.4743(9) 0.2792(9) 0.113(4) Uani 1 1 d . . . H53A H 0.8634 1.4440 0.2402 0.169 Uiso 1 1 calc R . . H53B H 0.7768 1.5474 0.2747 0.169 Uiso 1 1 calc R . . H53C H 0.7358 1.4478 0.2583 0.169 Uiso 1 1 calc R . . O1 O 0.8354(8) 1.4044(6) 0.4047(7) 0.131(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0358(7) 0.0530(6) 0.0360(7) 0.0062(5) -0.0140(5) -0.0136(5) S1 0.0413(13) 0.0568(12) 0.0316(12) 0.0050(9) -0.0135(10) -0.0111(10) S2 0.0328(12) 0.0511(11) 0.0386(13) 0.0029(9) -0.0138(10) -0.0097(9) S3 0.0528(15) 0.0574(12) 0.0391(13) -0.0022(10) -0.0087(11) -0.0155(11) S4 0.0441(14) 0.0583(12) 0.0467(14) 0.0037(10) -0.0123(11) -0.0179(11) B1 0.033(5) 0.051(5) 0.040(6) 0.007(4) -0.015(5) -0.011(4) C1 0.040(5) 0.064(5) 0.037(5) 0.006(4) -0.021(4) -0.011(4) C2 0.036(5) 0.066(5) 0.017(4) 0.003(3) -0.011(4) -0.022(4) C3 0.039(5) 0.056(5) 0.029(5) 0.006(4) -0.007(4) -0.010(4) C4 0.047(5) 0.085(6) 0.030(5) -0.002(4) -0.018(4) -0.022(5) C5 0.049(6) 0.084(6) 0.037(6) 0.008(4) -0.015(5) -0.019(5) C6 0.049(6) 0.072(5) 0.042(5) 0.002(4) -0.020(5) -0.021(5) C7 0.044(5) 0.054(5) 0.061(6) -0.004(4) -0.026(5) -0.006(4) C8 0.053(6) 0.069(6) 0.040(6) 0.013(4) -0.017(5) -0.018(5) C9 0.042(6) 0.087(7) 0.064(7) 0.006(5) -0.030(5) -0.020(5) C10 0.038(5) 0.076(6) 0.051(6) 0.016(4) -0.019(5) -0.031(5) C11 0.062(6) 0.096(7) 0.037(6) 0.010(5) -0.021(5) -0.043(5) C12 0.035(5) 0.059(5) 0.045(5) 0.001(4) -0.012(4) -0.009(4) C13 0.032(5) 0.047(4) 0.046(5) 0.006(4) -0.020(4) -0.016(4) C14 0.034(5) 0.056(5) 0.046(5) 0.000(4) -0.009(4) -0.012(4) C15 0.037(5) 0.050(4) 0.050(5) 0.013(4) -0.020(4) -0.018(4) C16 0.031(5) 0.057(5) 0.063(6) 0.012(4) -0.020(5) -0.010(4) C17 0.045(6) 0.054(5) 0.063(6) 0.013(4) -0.021(5) -0.015(4) C18 0.043(6) 0.047(5) 0.083(8) 0.011(5) -0.014(5) -0.017(4) C19 0.061(6) 0.047(5) 0.057(6) -0.003(4) -0.030(5) -0.002(4) C20 0.041(5) 0.055(5) 0.067(7) -0.008(5) -0.003(5) -0.008(4) C21 0.029(5) 0.057(5) 0.061(6) 0.012(4) -0.009(5) -0.008(4) C22 0.037(5) 0.061(5) 0.068(7) 0.012(5) -0.016(5) -0.011(4) C23 0.029(5) 0.065(5) 0.037(5) -0.001(4) -0.003(4) -0.014(4) C24 0.036(5) 0.050(4) 0.035(5) 0.009(4) -0.018(4) -0.011(4) C25 0.055(6) 0.053(5) 0.047(6) 0.005(4) -0.015(5) -0.010(4) C26 0.045(5) 0.061(5) 0.040(5) 0.009(4) -0.015(4) -0.004(4) C27 0.044(5) 0.070(5) 0.033(5) 0.009(4) -0.015(4) -0.023(4) C28 0.071(7) 0.083(6) 0.041(6) 0.019(5) -0.028(5) -0.031(6) C29 0.093(8) 0.082(6) 0.042(6) -0.007(5) -0.007(6) -0.034(6) C30 0.045(6) 0.064(6) 0.049(6) -0.007(5) -0.004(5) 0.006(5) C31 0.041(6) 0.094(7) 0.058(7) 0.012(5) -0.009(5) -0.023(5) C32 0.046(6) 0.058(5) 0.056(6) 0.009(4) -0.003(5) -0.025(5) C33 0.065(7) 0.083(7) 0.059(7) 0.024(5) -0.005(6) -0.015(6) C34 0.033(5) 0.058(5) 0.040(5) 0.002(4) -0.014(4) -0.009(4) C35 0.052(6) 0.060(5) 0.042(5) 0.010(4) -0.017(5) -0.012(5) C36 0.054(6) 0.059(6) 0.054(6) 0.012(4) -0.010(5) -0.001(5) C37 0.067(7) 0.045(5) 0.057(6) 0.003(4) -0.007(5) -0.011(5) C38 0.056(6) 0.080(6) 0.041(6) -0.006(5) -0.010(5) -0.028(5) C39 0.047(5) 0.057(5) 0.055(6) -0.005(4) -0.021(5) -0.008(4) C40 0.069(7) 0.079(6) 0.063(6) 0.033(5) -0.041(5) -0.042(5) C41 0.031(5) 0.061(5) 0.052(6) 0.009(4) -0.018(4) -0.015(4) C42 0.037(5) 0.057(5) 0.044(5) 0.005(4) -0.013(4) -0.010(4) C43 0.042(5) 0.064(5) 0.059(6) 0.003(4) -0.022(5) -0.010(4) C44 0.045(5) 0.060(5) 0.045(6) 0.018(4) -0.017(4) -0.017(4) C45 0.068(7) 0.063(5) 0.041(6) 0.026(4) -0.024(5) -0.035(5) C46 0.061(6) 0.056(5) 0.067(7) 0.011(5) -0.025(5) -0.021(5) C47 0.042(6) 0.061(5) 0.054(6) -0.006(4) -0.008(5) -0.010(4) C48 0.068(7) 0.070(5) 0.038(5) 0.004(4) -0.019(5) -0.028(5) C49 0.052(6) 0.082(6) 0.050(6) 0.015(5) -0.028(5) -0.033(5) C50 0.054(6) 0.069(6) 0.067(7) 0.002(5) -0.019(5) -0.030(5) C51 0.097(12) 0.254(19) 0.198(19) -0.073(16) -0.042(13) 0.036(13) C52 0.099(11) 0.080(8) 0.143(14) 0.001(8) -0.069(11) -0.022(8) C53 0.133(12) 0.120(9) 0.110(11) 0.008(8) -0.065(10) -0.046(8) O1 0.125(8) 0.119(7) 0.153(9) 0.013(6) -0.068(7) -0.006(6) _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 Ni1 C40 1.957(9) . ? Ni1 S4 2.149(2) . ? Ni1 S1 2.169(2) . ? Ni1 S2 2.242(2) . ? S1 C1 1.825(7) . ? S1 C2 1.839(7) . ? S2 C12 1.813(8) . ? S2 C13 1.838(7) . ? S3 C23 1.804(8) . ? S3 C24 1.835(8) . ? S4 C40 1.743(8) . ? S4 C41 1.843(7) . ? B1 C34 1.618(11) . ? B1 C1 1.620(11) . ? B1 C23 1.640(11) . ? B1 C12 1.656(11) . ? C2 C3 1.501(9) . ? C2 C7 1.524(10) . ? C2 C6 1.544(10) . ? C3 C4 1.493(10) . ? C4 C11 1.507(11) . ? C4 C5 1.537(11) . ? C5 C8 1.504(10) . ? C6 C10 1.537(10) . ? C7 C8 1.517(10) . ? C8 C9 1.530(11) . ? C9 C10 1.506(11) . ? C10 C11 1.546(10) . ? C13 C14 1.523(9) . ? C13 C16 1.523(11) . ? C13 C15 1.533(10) . ? C14 C19 1.520(9) . ? C15 C21 1.525(9) . ? C16 C17 1.543(9) . ? C17 C22 1.520(11) . ? C17 C18 1.536(10) . ? C18 C19 1.478(12) . ? C19 C20 1.552(11) . ? C20 C21 1.513(10) . ? C21 C22 1.517(12) . ? C24 C26 1.512(9) . ? C24 C25 1.514(10) . ? C24 C27 1.523(9) . ? C25 C32 1.495(11) . ? C26 C30 1.507(11) . ? C27 C28 1.536(11) . ? C28 C33 1.495(11) . ? C28 C29 1.526(12) . ? C29 C30 1.538(12) . ? C30 C31 1.491(11) . ? C31 C32 1.504(11) . ? C32 C33 1.511(12) . ? C34 C35 1.387(10) . ? C34 C39 1.422(10) . ? C35 C36 1.368(10) . ? C36 C37 1.386(11) . ? C37 C38 1.391(12) . ? C38 C39 1.391(10) . ? C41 C44 1.513(11) . ? C41 C42 1.514(9) . ? C41 C43 1.561(10) . ? C42 C47 1.530(10) . ? C43 C49 1.539(10) . ? C44 C45 1.525(10) . ? C45 C46 1.491(11) . ? C45 C50 1.562(11) . ? C46 C47 1.537(12) . ? C47 C48 1.503(11) . ? C48 C49 1.507(10) . ? C49 C50 1.548(11) . ? C51 C52 1.469(17) . ? C52 O1 1.232(13) . ? C52 C53 1.544(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 C40 Ni1 S4 50.0(2) . . ? C40 Ni1 S1 108.0(2) . . ? S4 Ni1 S1 154.47(9) . . ? C40 Ni1 S2 155.5(2) . . ? S4 Ni1 S2 105.96(9) . . ? S1 Ni1 S2 96.54(9) . . ? C1 S1 C2 105.2(3) . . ? C1 S1 Ni1 111.2(2) . . ? C2 S1 Ni1 118.2(3) . . ? C12 S2 C13 105.7(4) . . ? C12 S2 Ni1 109.8(3) . . ? C13 S2 Ni1 107.5(3) . . ? C23 S3 C24 106.4(3) . . ? C40 S4 C41 109.1(4) . . ? C40 S4 Ni1 59.3(3) . . ? C41 S4 Ni1 112.8(3) . . ? C34 B1 C1 113.4(7) . . ? C34 B1 C23 106.0(6) . . ? C1 B1 C23 105.9(6) . . ? C34 B1 C12 112.3(7) . . ? C1 B1 C12 110.0(6) . . ? C23 B1 C12 109.0(7) . . ? B1 C1 S1 116.5(5) . . ? C3 C2 C7 109.4(6) . . ? C3 C2 C6 107.3(5) . . ? C7 C2 C6 109.4(6) . . ? C3 C2 S1 109.6(5) . . ? C7 C2 S1 113.0(5) . . ? C6 C2 S1 108.0(5) . . ? C4 C3 C2 112.5(6) . . ? C3 C4 C11 109.2(7) . . ? C3 C4 C5 108.6(6) . . ? C11 C4 C5 109.4(7) . . ? C8 C5 C4 109.3(7) . . ? C10 C6 C2 109.6(7) . . ? C8 C7 C2 109.1(6) . . ? C5 C8 C7 109.0(7) . . ? C5 C8 C9 110.5(6) . . ? C7 C8 C9 110.8(7) . . ? C10 C9 C8 109.0(7) . . ? C9 C10 C6 109.5(6) . . ? C9 C10 C11 109.8(7) . . ? C6 C10 C11 108.7(7) . . ? C4 C11 C10 109.4(6) . . ? B1 C12 S2 110.8(6) . . ? C14 C13 C16 109.8(6) . . ? C14 C13 C15 109.5(6) . . ? C16 C13 C15 107.8(6) . . ? C14 C13 S2 112.3(5) . . ? C16 C13 S2 109.3(5) . . ? C15 C13 S2 107.9(5) . . ? C19 C14 C13 109.7(6) . . ? C21 C15 C13 109.8(6) . . ? C13 C16 C17 109.0(7) . . ? C22 C17 C18 109.5(7) . . ? C22 C17 C16 109.8(7) . . ? C18 C17 C16 109.5(6) . . ? C19 C18 C17 109.7(7) . . ? C18 C19 C14 110.4(7) . . ? C18 C19 C20 110.5(8) . . ? C14 C19 C20 108.9(7) . . ? C21 C20 C19 107.8(7) . . ? C20 C21 C22 111.3(7) . . ? C20 C21 C15 109.5(6) . . ? C22 C21 C15 109.7(7) . . ? C21 C22 C17 108.3(7) . . ? B1 C23 S3 114.4(5) . . ? C26 C24 C25 107.6(6) . . ? C26 C24 C27 108.6(6) . . ? C25 C24 C27 109.9(7) . . ? C26 C24 S3 113.4(5) . . ? C25 C24 S3 107.4(5) . . ? C27 C24 S3 109.9(5) . . ? C32 C25 C24 111.7(6) . . ? C30 C26 C24 111.2(7) . . ? C24 C27 C28 108.4(7) . . ? C33 C28 C29 109.0(8) . . ? C33 C28 C27 111.2(7) . . ? C29 C28 C27 108.9(7) . . ? C28 C29 C30 108.5(6) . . ? C31 C30 C26 109.5(7) . . ? C31 C30 C29 109.0(8) . . ? C26 C30 C29 109.1(7) . . ? C30 C31 C32 110.6(7) . . ? C25 C32 C31 109.5(8) . . ? C25 C32 C33 108.5(7) . . ? C31 C32 C33 108.6(7) . . ? C28 C33 C32 110.5(8) . . ? C35 C34 C39 114.4(7) . . ? C35 C34 B1 125.2(7) . . ? C39 C34 B1 120.2(7) . . ? C36 C35 C34 124.2(8) . . ? C35 C36 C37 120.9(9) . . ? C36 C37 C38 117.7(8) . . ? C37 C38 C39 120.8(8) . . ? C38 C39 C34 122.1(8) . . ? S4 C40 Ni1 70.8(3) . . ? C44 C41 C42 111.8(6) . . ? C44 C41 C43 110.4(6) . . ? C42 C41 C43 107.8(6) . . ? C44 C41 S4 107.9(5) . . ? C42 C41 S4 114.1(5) . . ? C43 C41 S4 104.6(5) . . ? C41 C42 C47 108.5(6) . . ? C49 C43 C41 108.6(6) . . ? C41 C44 C45 109.2(6) . . ? C46 C45 C44 109.7(7) . . ? C46 C45 C50 110.3(7) . . ? C44 C45 C50 108.3(7) . . ? C45 C46 C47 109.7(7) . . ? C48 C47 C42 108.6(7) . . ? C48 C47 C46 111.2(7) . . ? C42 C47 C46 109.3(7) . . ? C47 C48 C49 110.9(6) . . ? C48 C49 C43 108.6(7) . . ? C48 C49 C50 109.7(7) . . ? C43 C49 C50 108.5(6) . . ? C49 C50 C45 109.5(7) . . ? O1 C52 C51 122.7(16) . . ? O1 C52 C53 120.8(13) . . ? C51 C52 C53 116.4(13) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.495 _refine_diff_density_min -1.203 _refine_diff_density_rms 0.127 #===END data_cgr125 _database_code_CSD 199596 _audit_creation_method SHELXL-97 _chemical_name_systematic ; C40 H56 B Ni O S3, CH3CN ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H59 B N Ni O S3' _chemical_formula_weight 759.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ni Ni 0.3393 1.1124 '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' _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 13.917(4) _cell_length_b 11.629(3) _cell_length_c 23.722(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.156(6) _cell_angle_gamma 90.00 _cell_volume 3829(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1628 _exptl_absorpt_coefficient_mu 0.705 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8164 _exptl_absorpt_correction_T_max 0.8719 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27934 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0888 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 28.62 _reflns_number_total 9290 _reflns_number_gt 6181 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0681P)^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 9290 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0989 _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.1545 _refine_ls_wR_factor_gt 0.1377 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.046 _refine_ls_shift/su_mean 0.001 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 Ni1 Ni 0.06543(3) 0.18832(3) 0.211791(17) 0.03785(14) Uani 1 1 d . . . S1 S -0.06750(6) 0.07936(6) 0.22024(3) 0.03539(19) Uani 1 1 d . . . S2 S 0.00028(6) 0.35230(6) 0.24463(3) 0.03454(19) Uani 1 1 d . . . S3 S 0.03551(6) 0.23412(6) 0.11919(3) 0.03554(19) Uani 1 1 d . . . O1 O 0.2413(3) 0.0792(3) 0.25074(17) 0.1088(13) Uani 1 1 d . . . B1 B -0.1512(3) 0.2766(3) 0.16348(15) 0.0339(8) Uani 1 1 d . . . C1 C -0.1559(2) 0.1353(2) 0.16801(14) 0.0389(7) Uani 1 1 d . . . H1A H -0.1449 0.1019 0.1311 0.047 Uiso 1 1 calc R . . H1B H -0.2203 0.1123 0.1778 0.047 Uiso 1 1 calc R . . C2 C -0.0538(2) -0.0740(2) 0.20442(13) 0.0342(7) Uani 1 1 d . . . C3 C 0.0009(3) -0.1251(3) 0.25645(15) 0.0505(9) Uani 1 1 d . . . H3A H -0.0347 -0.1117 0.2900 0.061 Uiso 1 1 calc R . . H3B H 0.0644 -0.0887 0.2625 0.061 Uiso 1 1 calc R . . C4 C 0.0016(3) -0.0940(2) 0.15274(14) 0.0461(8) Uani 1 1 d . . . H4A H 0.0653 -0.0579 0.1580 0.055 Uiso 1 1 calc R . . H4B H -0.0330 -0.0597 0.1194 0.055 Uiso 1 1 calc R . . C5 C -0.1527(3) -0.1289(2) 0.19620(16) 0.0486(9) Uani 1 1 d . . . H5A H -0.1885 -0.0955 0.1631 0.058 Uiso 1 1 calc R . . H5B H -0.1889 -0.1146 0.2294 0.058 Uiso 1 1 calc R . . C6 C 0.0127(3) -0.2554(3) 0.24676(16) 0.0614(11) Uani 1 1 d . . . H6A H 0.0487 -0.2897 0.2801 0.074 Uiso 1 1 calc R . . C7 C -0.0863(3) -0.3110(3) 0.23880(17) 0.0629(12) Uani 1 1 d . . . H7A H -0.0795 -0.3941 0.2336 0.076 Uiso 1 1 calc R . . H7B H -0.1219 -0.2980 0.2724 0.076 Uiso 1 1 calc R . . C8 C -0.1406(3) -0.2592(3) 0.18771(16) 0.0540(10) Uani 1 1 d . . . H8A H -0.2049 -0.2956 0.1822 0.065 Uiso 1 1 calc R . . C9 C -0.0857(3) -0.2790(3) 0.13587(16) 0.0598(11) Uani 1 1 d . . . H9A H -0.0789 -0.3618 0.1294 0.072 Uiso 1 1 calc R . . H9B H -0.1213 -0.2457 0.1027 0.072 Uiso 1 1 calc R . . C10 C 0.0127(3) -0.2243(3) 0.14400(17) 0.0578(11) Uani 1 1 d . . . H10A H 0.0486 -0.2383 0.1101 0.069 Uiso 1 1 calc R . . C11 C 0.0679(3) -0.2747(3) 0.19522(19) 0.0680(12) Uani 1 1 d . . . H11A H 0.1314 -0.2382 0.2006 0.082 Uiso 1 1 calc R . . H11B H 0.0774 -0.3573 0.1896 0.082 Uiso 1 1 calc R . . C12 C -0.1270(2) 0.3326(2) 0.22735(13) 0.0359(7) Uani 1 1 d . . . H12A H -0.1530 0.2819 0.2555 0.043 Uiso 1 1 calc R . . H12B H -0.1595 0.4071 0.2293 0.043 Uiso 1 1 calc R . . C13 C 0.0200(2) 0.3620(2) 0.32166(13) 0.0350(7) Uani 1 1 d . . . C14 C 0.1220(2) 0.4061(3) 0.33280(14) 0.0461(8) Uani 1 1 d . . . H14A H 0.1285 0.4808 0.3143 0.055 Uiso 1 1 calc R . . H14B H 0.1672 0.3523 0.3171 0.055 Uiso 1 1 calc R . . C15 C 0.0099(3) 0.2460(2) 0.35034(13) 0.0431(8) Uani 1 1 d . . . H15A H -0.0559 0.2172 0.3429 0.052 Uiso 1 1 calc R . . H15B H 0.0542 0.1905 0.3351 0.052 Uiso 1 1 calc R . . C16 C -0.0498(3) 0.4474(3) 0.34540(14) 0.0446(8) Uani 1 1 d . . . H16A H -0.0445 0.5221 0.3268 0.054 Uiso 1 1 calc R . . H16B H -0.1161 0.4198 0.3382 0.054 Uiso 1 1 calc R . . C17 C 0.1455(3) 0.4186(3) 0.39642(16) 0.0541(9) Uani 1 1 d . . . H17A H 0.2123 0.4468 0.4038 0.065 Uiso 1 1 calc R . . C18 C 0.0757(3) 0.5032(3) 0.41987(16) 0.0604(11) Uani 1 1 d . . . H18A H 0.0905 0.5122 0.4607 0.072 Uiso 1 1 calc R . . H18B H 0.0825 0.5785 0.4020 0.072 Uiso 1 1 calc R . . C19 C -0.0263(3) 0.4605(3) 0.40870(15) 0.0535(10) Uani 1 1 d . . . H19A H -0.0714 0.5162 0.4241 0.064 Uiso 1 1 calc R . . C20 C -0.0374(3) 0.3439(3) 0.43673(16) 0.0611(11) Uani 1 1 d . . . H20A H -0.0243 0.3512 0.4777 0.073 Uiso 1 1 calc R . . H20B H -0.1035 0.3161 0.4292 0.073 Uiso 1 1 calc R . . C21 C 0.0328(3) 0.2589(3) 0.41345(15) 0.0534(10) Uani 1 1 d . . . H21A H 0.0264 0.1834 0.4321 0.064 Uiso 1 1 calc R . . C22 C 0.1347(3) 0.3027(3) 0.42455(15) 0.0606(11) Uani 1 1 d . . . H22A H 0.1799 0.2477 0.4097 0.073 Uiso 1 1 calc R . . H22B H 0.1501 0.3100 0.4654 0.073 Uiso 1 1 calc R . . C23 C -0.0737(2) 0.3189(2) 0.11818(14) 0.0373(7) Uani 1 1 d . . . H23A H -0.0561 0.3991 0.1264 0.045 Uiso 1 1 calc R . . H23B H -0.1055 0.3164 0.0800 0.045 Uiso 1 1 calc R . . C24 C 0.1272(2) 0.3275(2) 0.09163(13) 0.0353(7) Uani 1 1 d . . . C25 C 0.2219(3) 0.2621(3) 0.09673(17) 0.0565(10) Uani 1 1 d . . . H25A H 0.2150 0.1897 0.0757 0.068 Uiso 1 1 calc R . . H25B H 0.2393 0.2440 0.1365 0.068 Uiso 1 1 calc R . . C26 C 0.1393(2) 0.4402(3) 0.12461(15) 0.0462(8) Uani 1 1 d . . . H26A H 0.1568 0.4237 0.1645 0.055 Uiso 1 1 calc R . . H26B H 0.0783 0.4827 0.1220 0.055 Uiso 1 1 calc R . . C27 C 0.1006(3) 0.3544(3) 0.03031(15) 0.0528(9) Uani 1 1 d . . . H27A H 0.0393 0.3963 0.0268 0.063 Uiso 1 1 calc R . . H27B H 0.0924 0.2827 0.0089 0.063 Uiso 1 1 calc R . . C28 C 0.3013(3) 0.3354(3) 0.0730(2) 0.0658(12) Uani 1 1 d . . . H28A H 0.3631 0.2929 0.0763 0.079 Uiso 1 1 calc R . . C29 C 0.2728(3) 0.3610(4) 0.01144(19) 0.0771(14) Uani 1 1 d . . . H29A H 0.3236 0.4059 -0.0047 0.093 Uiso 1 1 calc R . . H29B H 0.2652 0.2887 -0.0097 0.093 Uiso 1 1 calc R . . C30 C 0.1794(3) 0.4274(3) 0.00597(16) 0.0616(11) Uani 1 1 d . . . H30A H 0.1616 0.4444 -0.0343 0.074 Uiso 1 1 calc R . . C31 C 0.1908(3) 0.5389(3) 0.03906(17) 0.0584(10) Uani 1 1 d . . . H31A H 0.2408 0.5863 0.0236 0.070 Uiso 1 1 calc R . . H31B H 0.1302 0.5820 0.0357 0.070 Uiso 1 1 calc R . . C32 C 0.2182(2) 0.5129(3) 0.10018(15) 0.0474(9) Uani 1 1 d . . . H32A H 0.2255 0.5860 0.1215 0.057 Uiso 1 1 calc R . . C33 C 0.3115(3) 0.4477(3) 0.10587(18) 0.0613(11) Uani 1 1 d . . . H33A H 0.3291 0.4314 0.1458 0.074 Uiso 1 1 calc R . . H33B H 0.3629 0.4943 0.0913 0.074 Uiso 1 1 calc R . . C34 C -0.2537(2) 0.3261(2) 0.13704(13) 0.0348(7) Uani 1 1 d . . . C35 C -0.2741(2) 0.4428(2) 0.13654(14) 0.0415(8) Uani 1 1 d . . . H35A H -0.2296 0.4930 0.1553 0.050 Uiso 1 1 calc R . . C36 C -0.3566(3) 0.4887(3) 0.10980(15) 0.0498(9) Uani 1 1 d . . . H36A H -0.3676 0.5684 0.1110 0.060 Uiso 1 1 calc R . . C37 C -0.4222(3) 0.4188(3) 0.08173(16) 0.0539(9) Uani 1 1 d . . . H37A H -0.4780 0.4499 0.0629 0.065 Uiso 1 1 calc R . . C38 C -0.4060(3) 0.3022(3) 0.08112(17) 0.0562(10) Uani 1 1 d . . . H38A H -0.4513 0.2529 0.0624 0.067 Uiso 1 1 calc R . . C39 C -0.3235(2) 0.2584(3) 0.10799(15) 0.0467(8) Uani 1 1 d . . . H39A H -0.3135 0.1785 0.1067 0.056 Uiso 1 1 calc R . . C40 C 0.1789(3) 0.1233(3) 0.23687(15) 0.0461(8) Uani 1 1 d . . . C41 C 0.3811(5) 0.3922(6) 0.4915(3) 0.139(3) Uani 1 1 d . . . H41A H 0.3584 0.3181 0.5038 0.208 Uiso 1 1 calc R . . H41B H 0.4487 0.4010 0.5037 0.208 Uiso 1 1 calc R . . H41C H 0.3731 0.3966 0.4506 0.208 Uiso 1 1 calc R . . C42 C 0.3272(4) 0.4810(5) 0.5152(2) 0.0871(16) Uani 1 1 d . . . N1 N 0.2838(4) 0.5486(4) 0.5334(2) 0.124(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0356(3) 0.0349(2) 0.0429(3) 0.00065(17) 0.00185(18) 0.00292(17) S1 0.0415(5) 0.0251(3) 0.0399(5) -0.0001(3) 0.0053(4) 0.0022(3) S2 0.0362(5) 0.0331(4) 0.0346(4) -0.0001(3) 0.0041(3) -0.0026(3) S3 0.0333(4) 0.0325(3) 0.0415(5) -0.0021(3) 0.0067(3) -0.0003(3) O1 0.068(3) 0.132(3) 0.124(3) -0.008(2) -0.011(2) 0.028(2) B1 0.034(2) 0.0268(14) 0.041(2) -0.0023(14) 0.0060(16) -0.0015(14) C1 0.0380(19) 0.0279(13) 0.050(2) 0.0016(13) -0.0012(15) 0.0010(13) C2 0.0435(19) 0.0240(12) 0.0353(17) -0.0017(12) 0.0049(14) 0.0022(12) C3 0.071(3) 0.0375(16) 0.042(2) 0.0015(14) -0.0057(18) 0.0097(16) C4 0.059(2) 0.0342(15) 0.047(2) -0.0033(14) 0.0134(17) -0.0002(15) C5 0.050(2) 0.0328(15) 0.063(2) -0.0024(15) 0.0084(18) -0.0033(15) C6 0.097(3) 0.0343(17) 0.051(2) 0.0038(16) -0.012(2) 0.0162(19) C7 0.100(4) 0.0290(16) 0.061(3) 0.0063(16) 0.016(2) -0.0007(19) C8 0.064(3) 0.0305(15) 0.067(3) -0.0025(16) 0.005(2) -0.0099(16) C9 0.092(3) 0.0336(16) 0.053(2) -0.0093(16) -0.004(2) -0.0018(19) C10 0.081(3) 0.0393(17) 0.057(2) -0.0079(16) 0.029(2) 0.0105(19) C11 0.072(3) 0.0368(18) 0.096(3) -0.011(2) 0.006(3) 0.0180(18) C12 0.0338(18) 0.0302(13) 0.0445(19) -0.0007(13) 0.0080(14) 0.0032(12) C13 0.0399(19) 0.0318(14) 0.0337(17) 0.0009(12) 0.0049(14) -0.0007(13) C14 0.047(2) 0.0502(18) 0.041(2) -0.0025(15) -0.0002(16) -0.0044(16) C15 0.061(2) 0.0302(14) 0.0389(19) 0.0041(13) 0.0110(16) 0.0032(14) C16 0.053(2) 0.0397(16) 0.041(2) 0.0023(14) 0.0032(16) 0.0106(15) C17 0.050(2) 0.062(2) 0.049(2) -0.0114(18) -0.0067(17) -0.0007(18) C18 0.083(3) 0.051(2) 0.045(2) -0.0126(17) -0.011(2) 0.005(2) C19 0.074(3) 0.0454(18) 0.041(2) -0.0045(16) 0.0064(19) 0.0224(18) C20 0.082(3) 0.065(2) 0.038(2) 0.0051(17) 0.017(2) 0.011(2) C21 0.081(3) 0.0377(16) 0.042(2) 0.0049(15) 0.0090(19) 0.0122(18) C22 0.080(3) 0.064(2) 0.037(2) -0.0086(17) -0.0075(19) 0.029(2) C23 0.0321(18) 0.0364(15) 0.0436(19) 0.0030(13) 0.0032(14) 0.0020(13) C24 0.0329(18) 0.0355(14) 0.0385(18) 0.0007(13) 0.0094(14) -0.0014(13) C25 0.044(2) 0.0494(19) 0.079(3) 0.0158(19) 0.018(2) 0.0066(17) C26 0.041(2) 0.0446(17) 0.054(2) -0.0144(16) 0.0113(16) -0.0083(15) C27 0.063(3) 0.0503(18) 0.045(2) -0.0020(16) 0.0015(18) -0.0163(18) C28 0.039(2) 0.056(2) 0.107(4) 0.020(2) 0.035(2) 0.0087(17) C29 0.099(4) 0.060(2) 0.080(3) -0.014(2) 0.060(3) -0.020(2) C30 0.080(3) 0.067(2) 0.038(2) 0.0044(18) 0.008(2) -0.027(2) C31 0.056(3) 0.0468(19) 0.073(3) 0.0144(18) 0.008(2) -0.0121(17) C32 0.043(2) 0.0457(17) 0.055(2) -0.0060(16) 0.0101(17) -0.0147(16) C33 0.041(2) 0.076(3) 0.067(3) 0.014(2) 0.0051(19) -0.019(2) C34 0.0345(18) 0.0323(14) 0.0383(18) 0.0030(12) 0.0076(14) 0.0016(12) C35 0.041(2) 0.0362(15) 0.048(2) -0.0032(14) 0.0024(15) 0.0050(14) C36 0.051(2) 0.0486(18) 0.051(2) 0.0044(16) 0.0077(18) 0.0179(17) C37 0.037(2) 0.072(2) 0.051(2) 0.0079(19) -0.0007(17) 0.0173(19) C38 0.041(2) 0.061(2) 0.065(3) -0.0046(19) -0.0088(18) -0.0003(18) C39 0.039(2) 0.0390(16) 0.061(2) -0.0041(15) -0.0037(17) 0.0025(15) C40 0.048(2) 0.0500(19) 0.041(2) -0.0060(16) 0.0085(17) 0.0046(17) C41 0.142(6) 0.181(6) 0.091(5) -0.007(4) -0.013(4) 0.091(5) C42 0.106(5) 0.096(4) 0.057(3) 0.003(3) -0.011(3) 0.019(3) N1 0.166(6) 0.103(4) 0.097(4) -0.007(3) -0.021(4) 0.027(4) _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 Ni1 C40 1.812(4) . ? Ni1 S1 2.2632(10) . ? Ni1 S3 2.2695(11) . ? Ni1 S2 2.2734(9) . ? S1 C1 1.803(3) . ? S1 C2 1.836(3) . ? S2 C12 1.804(3) . ? S2 C13 1.832(3) . ? S3 C23 1.810(3) . ? S3 C24 1.832(3) . ? O1 C40 1.041(4) . ? B1 C34 1.621(5) . ? B1 C1 1.648(4) . ? B1 C23 1.652(4) . ? B1 C12 1.661(5) . ? C2 C4 1.513(4) . ? C2 C5 1.517(4) . ? C2 C3 1.523(4) . ? C3 C6 1.542(4) . ? C4 C10 1.538(4) . ? C5 C8 1.539(4) . ? C6 C11 1.508(5) . ? C6 C7 1.521(6) . ? C7 C8 1.507(5) . ? C8 C9 1.512(5) . ? C9 C10 1.509(5) . ? C10 C11 1.508(6) . ? C13 C14 1.514(4) . ? C13 C15 1.522(4) . ? C13 C16 1.526(4) . ? C14 C17 1.528(5) . ? C15 C21 1.515(5) . ? C16 C19 1.521(5) . ? C17 C22 1.516(5) . ? C17 C18 1.517(5) . ? C18 C19 1.508(5) . ? C19 C20 1.523(5) . ? C20 C21 1.521(5) . ? C21 C22 1.512(5) . ? C24 C27 1.507(5) . ? C24 C25 1.519(4) . ? C24 C26 1.529(4) . ? C25 C28 1.534(5) . ? C26 C32 1.533(4) . ? C27 C30 1.532(5) . ? C28 C29 1.515(6) . ? C28 C33 1.522(5) . ? C29 C30 1.509(6) . ? C30 C31 1.518(5) . ? C31 C32 1.503(5) . ? C32 C33 1.503(5) . ? C34 C35 1.387(4) . ? C34 C39 1.393(4) . ? C35 C36 1.378(5) . ? C36 C37 1.359(5) . ? C37 C38 1.374(5) . ? C38 C39 1.371(5) . ? C41 C42 1.417(7) . ? C42 N1 1.098(6) . ? 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 C40 Ni1 S1 115.87(12) . . ? C40 Ni1 S3 120.67(11) . . ? S1 Ni1 S3 97.08(3) . . ? C40 Ni1 S2 126.66(11) . . ? S1 Ni1 S2 95.19(4) . . ? S3 Ni1 S2 94.88(3) . . ? C1 S1 C2 106.64(14) . . ? C1 S1 Ni1 104.96(11) . . ? C2 S1 Ni1 115.34(11) . . ? C12 S2 C13 107.97(15) . . ? C12 S2 Ni1 103.00(9) . . ? C13 S2 Ni1 111.04(10) . . ? C23 S3 C24 106.15(14) . . ? C23 S3 Ni1 103.62(11) . . ? C24 S3 Ni1 113.64(11) . . ? C34 B1 C1 110.0(2) . . ? C34 B1 C23 103.9(2) . . ? C1 B1 C23 111.7(2) . . ? C34 B1 C12 109.2(2) . . ? C1 B1 C12 109.7(3) . . ? C23 B1 C12 112.2(2) . . ? B1 C1 S1 112.1(2) . . ? C4 C2 C5 110.0(3) . . ? C4 C2 C3 110.0(3) . . ? C5 C2 C3 109.6(3) . . ? C4 C2 S1 112.4(2) . . ? C5 C2 S1 109.2(2) . . ? C3 C2 S1 105.5(2) . . ? C2 C3 C6 108.3(3) . . ? C2 C4 C10 108.8(3) . . ? C2 C5 C8 109.0(3) . . ? C11 C6 C7 110.3(3) . . ? C11 C6 C3 109.4(3) . . ? C7 C6 C3 109.3(3) . . ? C8 C7 C6 109.1(3) . . ? C7 C8 C9 109.8(3) . . ? C7 C8 C5 109.9(3) . . ? C9 C8 C5 108.8(3) . . ? C10 C9 C8 109.8(3) . . ? C9 C10 C11 110.1(3) . . ? C9 C10 C4 109.5(3) . . ? C11 C10 C4 108.9(3) . . ? C10 C11 C6 109.6(3) . . ? B1 C12 S2 112.9(2) . . ? C14 C13 C15 109.7(3) . . ? C14 C13 C16 109.3(3) . . ? C15 C13 C16 109.3(3) . . ? C14 C13 S2 105.4(2) . . ? C15 C13 S2 112.3(2) . . ? C16 C13 S2 110.8(2) . . ? C13 C14 C17 109.6(3) . . ? C21 C15 C13 109.5(3) . . ? C19 C16 C13 109.4(3) . . ? C22 C17 C18 109.2(3) . . ? C22 C17 C14 109.2(3) . . ? C18 C17 C14 109.1(3) . . ? C19 C18 C17 110.0(3) . . ? C18 C19 C16 109.8(3) . . ? C18 C19 C20 109.9(3) . . ? C16 C19 C20 108.7(3) . . ? C21 C20 C19 109.4(3) . . ? C22 C21 C15 109.4(3) . . ? C22 C21 C20 109.7(3) . . ? C15 C21 C20 109.2(3) . . ? C21 C22 C17 110.1(3) . . ? B1 C23 S3 114.6(2) . . ? C27 C24 C25 109.4(3) . . ? C27 C24 C26 109.0(3) . . ? C25 C24 C26 109.0(3) . . ? C27 C24 S3 109.8(2) . . ? C25 C24 S3 107.3(2) . . ? C26 C24 S3 112.3(2) . . ? C24 C25 C28 109.7(3) . . ? C24 C26 C32 109.6(3) . . ? C24 C27 C30 110.3(3) . . ? C29 C28 C33 109.5(3) . . ? C29 C28 C25 108.5(4) . . ? C33 C28 C25 109.4(3) . . ? C30 C29 C28 110.3(3) . . ? C29 C30 C31 109.6(3) . . ? C29 C30 C27 108.6(3) . . ? C31 C30 C27 109.2(3) . . ? C32 C31 C30 109.7(3) . . ? C33 C32 C31 110.2(3) . . ? C33 C32 C26 109.0(3) . . ? C31 C32 C26 109.7(3) . . ? C32 C33 C28 109.8(3) . . ? C35 C34 C39 114.5(3) . . ? C35 C34 B1 121.6(3) . . ? C39 C34 B1 123.5(3) . . ? C36 C35 C34 123.1(3) . . ? C37 C36 C35 120.1(3) . . ? C36 C37 C38 119.4(3) . . ? C39 C38 C37 119.6(3) . . ? C38 C39 C34 123.4(3) . . ? O1 C40 Ni1 175.1(4) . . ? N1 C42 C41 178.6(8) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 28.62 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.599 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.074