data_char155b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H76 B2 Ni2 S7.93' _chemical_formula_weight 974.30 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' _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 9.601(4) _cell_length_b 11.682(4) _cell_length_c 12.337(5) _cell_angle_alpha 64.454(4) _cell_angle_beta 77.614(5) _cell_angle_gamma 84.035(5) _cell_volume 1219.3(8) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 928 _cell_measurement_theta_min 3.20 _cell_measurement_theta_max 27.86 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 521 _exptl_absorpt_coefficient_mu 1.140 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7762 _exptl_absorpt_correction_T_max 0.9347 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 120(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 'Bruker AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 1 _diffrn_reflns_number 11896 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 28.18 _reflns_number_total 5388 _reflns_number_gt 4664 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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^)+(0.0499P)^2^+1.8174P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5388 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1115 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.04003(4) 0.10025(3) 0.32202(3) 0.01875(11) Uani 1 1 d . . . B B 0.1656(3) 0.2386(3) 0.0138(3) 0.0200(6) Uani 1 1 d . . . S1 S 0.25338(7) 0.04122(6) 0.23153(6) 0.01901(14) Uani 1 1 d . . . S2 S 0.08378(7) 0.31533(6) 0.21340(6) 0.01975(15) Uani 1 1 d . . . S3 S -0.08497(7) 0.09655(6) 0.18299(6) 0.01978(15) Uani 1 1 d . . . S4 S -0.07319(8) -0.05797(7) 0.48938(6) 0.02178(19) Uani 0.929(2) 1 d P . 1 S5 S 0.0000 0.0000 0.5000 0.02178(19) Uani 0.071(2) 2 d SP . 2 C1 C 0.1922(3) 0.2481(3) -0.2084(3) 0.0237(6) Uani 1 1 d . . . H1A H 0.1365 0.1735 -0.1706 0.028 Uiso 1 1 calc R . . C2 C 0.2387(3) 0.2994(3) -0.3340(3) 0.0270(6) Uani 1 1 d . . . H2A H 0.2146 0.2598 -0.3804 0.032 Uiso 1 1 calc R . . C3 C 0.3203(3) 0.4083(3) -0.3926(3) 0.0278(6) Uani 1 1 d . . . H3A H 0.3509 0.4446 -0.4790 0.033 Uiso 1 1 calc R . . C4 C 0.3565(3) 0.4631(3) -0.3228(3) 0.0260(6) Uani 1 1 d . . . H4A H 0.4134 0.5370 -0.3612 0.031 Uiso 1 1 calc R . . C5 C 0.3096(3) 0.4102(3) -0.1965(3) 0.0241(6) Uani 1 1 d . . . H5A H 0.3366 0.4489 -0.1504 0.029 Uiso 1 1 calc R . . C6 C 0.2241(3) 0.3022(3) -0.1347(2) 0.0199(5) Uani 1 1 d . . . C7 C 0.2487(3) 0.0998(3) 0.0697(2) 0.0211(5) Uani 1 1 d . . . H7A H 0.3478 0.1079 0.0232 0.025 Uiso 1 1 calc R . . H7B H 0.2004 0.0367 0.0573 0.025 Uiso 1 1 calc R . . C8 C 0.2792(3) -0.1336(3) 0.2853(2) 0.0209(5) Uani 1 1 d . . . C9 C 0.4145(3) -0.1570(3) 0.2056(3) 0.0259(6) Uani 1 1 d . . . H9A H 0.4356 -0.2482 0.2365 0.039 Uiso 1 1 calc R . . H9B H 0.4945 -0.1130 0.2080 0.039 Uiso 1 1 calc R . . H9C H 0.4001 -0.1247 0.1211 0.039 Uiso 1 1 calc R . . C10 C 0.1493(3) -0.1943(3) 0.2785(3) 0.0250(6) Uani 1 1 d . . . H10A H 0.1620 -0.2867 0.3132 0.038 Uiso 1 1 calc R . . H10B H 0.1396 -0.1630 0.1929 0.038 Uiso 1 1 calc R . . H10C H 0.0633 -0.1720 0.3250 0.038 Uiso 1 1 calc R . . C11 C 0.3003(3) -0.1834(3) 0.4183(3) 0.0271(6) Uani 1 1 d . . . H11A H 0.3117 -0.2759 0.4526 0.041 Uiso 1 1 calc R . . H11B H 0.2169 -0.1604 0.4668 0.041 Uiso 1 1 calc R . . H11C H 0.3857 -0.1455 0.4201 0.041 Uiso 1 1 calc R . . C12 C 0.2023(3) 0.3337(3) 0.0711(2) 0.0227(6) Uani 1 1 d . . . H12A H 0.1964 0.4227 0.0102 0.027 Uiso 1 1 calc R . . H12B H 0.3015 0.3170 0.0853 0.027 Uiso 1 1 calc R . . C13 C 0.1766(3) 0.3908(3) 0.2830(2) 0.0231(6) Uani 1 1 d . . . C14 C 0.3034(3) 0.3100(3) 0.3317(3) 0.0292(6) Uani 1 1 d . . . H14A H 0.3547 0.3544 0.3626 0.044 Uiso 1 1 calc R . . H14B H 0.3677 0.2950 0.2657 0.044 Uiso 1 1 calc R . . H14C H 0.2695 0.2285 0.3982 0.044 Uiso 1 1 calc R . . C15 C 0.2257(4) 0.5217(3) 0.1858(3) 0.0339(7) Uani 1 1 d . . . H15A H 0.2719 0.5642 0.2217 0.051 Uiso 1 1 calc R . . H15B H 0.1432 0.5723 0.1549 0.051 Uiso 1 1 calc R . . H15C H 0.2937 0.5126 0.1182 0.051 Uiso 1 1 calc R . . C16 C 0.0627(3) 0.4054(3) 0.3846(3) 0.0280(6) Uani 1 1 d . . . H16A H 0.1060 0.4413 0.4281 0.042 Uiso 1 1 calc R . . H16B H 0.0231 0.3222 0.4422 0.042 Uiso 1 1 calc R . . H16C H -0.0136 0.4623 0.3485 0.042 Uiso 1 1 calc R . . C17 C -0.0086(3) 0.2225(3) 0.0370(2) 0.0221(5) Uani 1 1 d . . . H17A H -0.0308 0.2058 -0.0296 0.026 Uiso 1 1 calc R . . H17B H -0.0557 0.3038 0.0316 0.026 Uiso 1 1 calc R . . C18 C -0.2761(3) 0.1448(3) 0.2101(3) 0.0233(6) Uani 1 1 d . . . C19 C -0.3371(3) 0.1611(3) 0.0996(3) 0.0299(7) Uani 1 1 d . . . H19A H -0.4404 0.1757 0.1153 0.045 Uiso 1 1 calc R . . H19B H -0.3176 0.0842 0.0853 0.045 Uiso 1 1 calc R . . H19C H -0.2925 0.2338 0.0272 0.045 Uiso 1 1 calc R . . C20 C -0.3516(3) 0.0367(3) 0.3240(3) 0.0306(6) Uani 1 1 d . . . H20A H -0.4535 0.0573 0.3390 0.046 Uiso 1 1 calc R . . H20B H -0.3107 0.0247 0.3945 0.046 Uiso 1 1 calc R . . H20C H -0.3392 -0.0415 0.3117 0.046 Uiso 1 1 calc R . . C21 C -0.2889(3) 0.2667(3) 0.2286(3) 0.0325(7) Uani 1 1 d . . . H21A H -0.3890 0.2943 0.2369 0.049 Uiso 1 1 calc R . . H21B H -0.2319 0.3330 0.1579 0.049 Uiso 1 1 calc R . . H21C H -0.2540 0.2511 0.3029 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.01805(18) 0.02285(19) 0.01562(17) -0.00797(14) -0.00311(13) -0.00219(13) B 0.0197(14) 0.0245(15) 0.0152(13) -0.0077(11) -0.0020(11) -0.0036(12) S1 0.0176(3) 0.0229(3) 0.0169(3) -0.0082(2) -0.0039(2) -0.0013(2) S2 0.0206(3) 0.0232(3) 0.0170(3) -0.0092(3) -0.0044(2) -0.0017(2) S3 0.0180(3) 0.0246(3) 0.0182(3) -0.0099(3) -0.0039(2) -0.0017(2) S4 0.0232(4) 0.0262(4) 0.0158(3) -0.0074(3) -0.0034(3) -0.0064(3) S5 0.0232(4) 0.0262(4) 0.0158(3) -0.0074(3) -0.0034(3) -0.0064(3) C1 0.0244(14) 0.0255(14) 0.0214(13) -0.0097(11) -0.0041(11) -0.0032(11) C2 0.0283(15) 0.0358(16) 0.0220(14) -0.0167(12) -0.0049(11) -0.0001(12) C3 0.0294(15) 0.0353(16) 0.0155(12) -0.0094(12) -0.0023(11) 0.0028(12) C4 0.0256(14) 0.0252(14) 0.0222(13) -0.0071(11) 0.0010(11) -0.0033(11) C5 0.0259(14) 0.0260(14) 0.0227(13) -0.0124(11) -0.0047(11) -0.0004(11) C6 0.0185(12) 0.0250(13) 0.0170(12) -0.0090(10) -0.0052(10) 0.0016(10) C7 0.0191(13) 0.0294(14) 0.0158(12) -0.0106(11) -0.0035(10) -0.0001(11) C8 0.0235(13) 0.0197(13) 0.0186(12) -0.0077(10) -0.0041(10) 0.0027(10) C9 0.0242(14) 0.0297(15) 0.0227(13) -0.0113(12) -0.0044(11) 0.0042(12) C10 0.0268(14) 0.0241(14) 0.0241(14) -0.0106(11) -0.0022(11) -0.0029(11) C11 0.0325(16) 0.0252(14) 0.0209(13) -0.0064(11) -0.0089(11) 0.0043(12) C12 0.0253(14) 0.0257(14) 0.0178(12) -0.0103(11) -0.0008(10) -0.0043(11) C13 0.0262(14) 0.0278(14) 0.0195(13) -0.0133(11) -0.0047(11) -0.0020(11) C14 0.0225(14) 0.0384(17) 0.0327(16) -0.0186(14) -0.0086(12) -0.0023(12) C15 0.048(2) 0.0301(16) 0.0262(15) -0.0123(13) -0.0067(14) -0.0097(14) C16 0.0310(16) 0.0350(16) 0.0226(14) -0.0174(12) -0.0040(12) 0.0020(13) C17 0.0220(13) 0.0279(14) 0.0164(12) -0.0084(11) -0.0049(10) -0.0021(11) C18 0.0175(13) 0.0291(14) 0.0246(13) -0.0120(12) -0.0044(10) -0.0014(11) C19 0.0205(14) 0.0415(18) 0.0256(14) -0.0103(13) -0.0055(11) -0.0060(13) C20 0.0243(15) 0.0380(17) 0.0274(15) -0.0117(13) -0.0027(12) -0.0058(13) C21 0.0206(14) 0.0370(17) 0.0451(18) -0.0243(15) -0.0025(13) 0.0017(12) _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 Ni S5 1.9633(7) . ? Ni S4 2.2415(9) . ? Ni S4 2.2481(11) 2_556 ? Ni S1 2.3036(10) . ? Ni S3 2.3112(9) . ? Ni S2 2.3149(11) . ? B C6 1.642(4) . ? B C12 1.650(4) . ? B C17 1.652(4) . ? B C7 1.656(4) . ? S1 C7 1.820(3) . ? S1 C8 1.862(3) . ? S2 C12 1.815(3) . ? S2 C13 1.858(3) . ? S3 C17 1.822(3) . ? S3 C18 1.866(3) . ? S4 S4 2.1768(15) 2_556 ? S4 Ni 2.2481(11) 2_556 ? S5 Ni 1.9633(7) 2_556 ? C1 C2 1.385(4) . ? C1 C6 1.406(4) . ? C2 C3 1.387(4) . ? C3 C4 1.387(4) . ? C4 C5 1.392(4) . ? C5 C6 1.401(4) . ? C8 C9 1.530(4) . ? C8 C10 1.531(4) . ? C8 C11 1.537(4) . ? C13 C14 1.524(4) . ? C13 C15 1.525(4) . ? C13 C16 1.534(4) . ? C18 C20 1.522(4) . ? C18 C21 1.525(4) . ? C18 C19 1.529(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S5 Ni S4 29.049(19) . . ? S5 Ni S4 28.96(2) . 2_556 ? S4 Ni S4 58.01(4) . 2_556 ? S5 Ni S1 111.88(3) . . ? S4 Ni S1 114.36(4) . . ? S4 Ni S1 103.86(3) 2_556 . ? S5 Ni S3 126.60(3) . . ? S4 Ni S3 98.04(4) . . ? S4 Ni S3 154.40(3) 2_556 . ? S1 Ni S3 94.01(4) . . ? S5 Ni S2 128.57(2) . . ? S4 Ni S2 148.58(3) . . ? S4 Ni S2 103.77(3) 2_556 . ? S1 Ni S2 94.00(3) . . ? S3 Ni S2 92.92(3) . . ? C6 B C12 109.0(2) . . ? C6 B C17 107.4(2) . . ? C12 B C17 110.4(2) . . ? C6 B C7 106.7(2) . . ? C12 B C7 111.3(2) . . ? C17 B C7 111.9(2) . . ? C7 S1 C8 104.79(12) . . ? C7 S1 Ni 106.81(9) . . ? C8 S1 Ni 113.93(9) . . ? C12 S2 C13 105.39(13) . . ? C12 S2 Ni 106.10(9) . . ? C13 S2 Ni 116.98(10) . . ? C17 S3 C18 103.96(13) . . ? C17 S3 Ni 105.13(9) . . ? C18 S3 Ni 113.33(9) . . ? S4 S4 Ni 61.15(4) 2_556 . ? S4 S4 Ni 60.85(3) 2_556 2_556 ? Ni S4 Ni 121.99(4) . 2_556 ? Ni S5 Ni 180.0 . 2_556 ? C2 C1 C6 122.5(3) . . ? C1 C2 C3 120.5(3) . . ? C4 C3 C2 118.7(3) . . ? C3 C4 C5 120.2(3) . . ? C4 C5 C6 122.6(3) . . ? C5 C6 C1 115.4(2) . . ? C5 C6 B 123.7(2) . . ? C1 C6 B 120.8(2) . . ? B C7 S1 113.57(18) . . ? C9 C8 C10 111.3(2) . . ? C9 C8 C11 110.1(2) . . ? C10 C8 C11 110.9(2) . . ? C9 C8 S1 107.68(19) . . ? C10 C8 S1 110.93(19) . . ? C11 C8 S1 105.68(18) . . ? B C12 S2 113.58(18) . . ? C14 C13 C15 110.4(3) . . ? C14 C13 C16 112.4(2) . . ? C15 C13 C16 109.4(3) . . ? C14 C13 S2 110.9(2) . . ? C15 C13 S2 108.30(19) . . ? C16 C13 S2 105.19(19) . . ? B C17 S3 114.93(18) . . ? C20 C18 C21 110.5(3) . . ? C20 C18 C19 109.5(2) . . ? C21 C18 C19 111.9(3) . . ? C20 C18 S3 107.2(2) . . ? C21 C18 S3 110.31(19) . . ? C19 C18 S3 107.2(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S5 Ni S1 C7 161.29(9) . . . . ? S4 Ni S1 C7 129.76(10) . . . . ? S4 Ni S1 C7 -169.41(10) 2_556 . . . ? S3 Ni S1 C7 29.06(10) . . . . ? S2 Ni S1 C7 -64.16(10) . . . . ? S5 Ni S1 C8 46.09(10) . . . . ? S4 Ni S1 C8 14.55(10) . . . . ? S4 Ni S1 C8 75.39(10) 2_556 . . . ? S3 Ni S1 C8 -86.15(10) . . . . ? S2 Ni S1 C8 -179.36(10) . . . . ? S5 Ni S2 C12 149.46(10) . . . . ? S4 Ni S2 C12 -177.63(10) . . . . ? S4 Ni S2 C12 132.55(10) 2_556 . . . ? S1 Ni S2 C12 27.22(10) . . . . ? S3 Ni S2 C12 -67.01(10) . . . . ? S5 Ni S2 C13 32.27(11) . . . . ? S4 Ni S2 C13 65.18(12) . . . . ? S4 Ni S2 C13 15.36(11) 2_556 . . . ? S1 Ni S2 C13 -89.97(11) . . . . ? S3 Ni S2 C13 175.80(11) . . . . ? S5 Ni S3 C17 173.65(10) . . . . ? S4 Ni S3 C17 179.50(10) . . . . ? S4 Ni S3 C17 160.18(11) 2_556 . . . ? S1 Ni S3 C17 -65.19(10) . . . . ? S2 Ni S3 C17 29.02(10) . . . . ? S5 Ni S3 C18 60.77(11) . . . . ? S4 Ni S3 C18 66.62(11) . . . . ? S4 Ni S3 C18 47.30(13) 2_556 . . . ? S1 Ni S3 C18 -178.07(10) . . . . ? S2 Ni S3 C18 -83.85(10) . . . . ? S5 Ni S4 S4 0.0 . . . 2_556 ? S1 Ni S4 S4 91.57(5) . . . 2_556 ? S3 Ni S4 S4 -170.30(4) . . . 2_556 ? S2 Ni S4 S4 -61.04(7) . . . 2_556 ? S5 Ni S4 Ni 0.0 . . . 2_556 ? S4 Ni S4 Ni 0.0 2_556 . . 2_556 ? S1 Ni S4 Ni 91.57(5) . . . 2_556 ? S3 Ni S4 Ni -170.30(4) . . . 2_556 ? S2 Ni S4 Ni -61.04(7) . . . 2_556 ? S4 Ni S5 Ni -71(7) . . . 2_556 ? S4 Ni S5 Ni 109(7) 2_556 . . 2_556 ? S1 Ni S5 Ni -172(7) . . . 2_556 ? S3 Ni S5 Ni -59(7) . . . 2_556 ? S2 Ni S5 Ni 74(7) . . . 2_556 ? C6 C1 C2 C3 0.0(5) . . . . ? C1 C2 C3 C4 1.2(5) . . . . ? C2 C3 C4 C5 -0.9(5) . . . . ? C3 C4 C5 C6 -0.7(5) . . . . ? C4 C5 C6 C1 1.9(4) . . . . ? C4 C5 C6 B -179.3(3) . . . . ? C2 C1 C6 C5 -1.5(4) . . . . ? C2 C1 C6 B 179.6(3) . . . . ? C12 B C6 C5 8.7(4) . . . . ? C17 B C6 C5 128.3(3) . . . . ? C7 B C6 C5 -111.6(3) . . . . ? C12 B C6 C1 -172.5(2) . . . . ? C17 B C6 C1 -52.9(3) . . . . ? C7 B C6 C1 67.2(3) . . . . ? C6 B C7 S1 157.99(18) . . . . ? C12 B C7 S1 39.2(3) . . . . ? C17 B C7 S1 -84.8(2) . . . . ? C8 S1 C7 B 157.17(19) . . . . ? Ni S1 C7 B 36.0(2) . . . . ? C7 S1 C8 C9 56.2(2) . . . . ? Ni S1 C8 C9 172.55(15) . . . . ? C7 S1 C8 C10 -65.9(2) . . . . ? Ni S1 C8 C10 50.5(2) . . . . ? C7 S1 C8 C11 173.84(19) . . . . ? Ni S1 C8 C11 -69.8(2) . . . . ? C6 B C12 S2 154.85(19) . . . . ? C17 B C12 S2 37.1(3) . . . . ? C7 B C12 S2 -87.7(2) . . . . ? C13 S2 C12 B 162.9(2) . . . . ? Ni S2 C12 B 38.2(2) . . . . ? C12 S2 C13 C14 -72.1(2) . . . . ? Ni S2 C13 C14 45.4(2) . . . . ? C12 S2 C13 C15 49.2(2) . . . . ? Ni S2 C13 C15 166.78(18) . . . . ? C12 S2 C13 C16 166.11(19) . . . . ? Ni S2 C13 C16 -76.3(2) . . . . ? C6 B C17 S3 154.02(19) . . . . ? C12 B C17 S3 -87.3(2) . . . . ? C7 B C17 S3 37.2(3) . . . . ? C18 S3 C17 B 156.8(2) . . . . ? Ni S3 C17 B 37.5(2) . . . . ? C17 S3 C18 C20 173.82(19) . . . . ? Ni S3 C18 C20 -72.6(2) . . . . ? C17 S3 C18 C21 -65.8(2) . . . . ? Ni S3 C18 C21 47.8(2) . . . . ? C17 S3 C18 C19 56.3(2) . . . . ? Ni S3 C18 C19 169.93(17) . . . . ? _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.803 _refine_diff_density_min -0.735 _refine_diff_density_rms 0.095 #===END data_char173 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H76 B2 Ni2 S7' _chemical_formula_weight 944.49 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' _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 9.4632(11) _cell_length_b 11.6124(14) _cell_length_c 12.4011(14) _cell_angle_alpha 63.307(5) _cell_angle_beta 80.785(6) _cell_angle_gamma 84.638(6) _cell_volume 1201.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 865 _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 23.52 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 506 _exptl_absorpt_coefficient_mu 1.116 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8085 _exptl_absorpt_correction_T_max 0.9684 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 120(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 'Bruker AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 1 _diffrn_reflns_number 13684 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.26 _reflns_number_total 5431 _reflns_number_gt 4630 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 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^)+(0.0415P)^2^+0.6288P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5431 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0900 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.05645(3) 0.09826(3) 0.31333(2) 0.01492(9) Uani 1 1 d . . . B1 B 0.1740(3) 0.2444(2) 0.0102(2) 0.0154(5) Uani 1 1 d . . . S1 S -0.07270(6) 0.09970(5) 0.17184(5) 0.01570(12) Uani 1 1 d . . . S2 S 0.09254(6) 0.31583(5) 0.20597(5) 0.01581(12) Uani 1 1 d . . . S3 S 0.26684(6) 0.04028(5) 0.22939(5) 0.01481(12) Uani 1 1 d . . . S4 S 0.0000 0.0000 0.5000 0.01680(16) Uani 1 2 d S . . C1 C 0.1913(2) 0.2588(2) -0.2104(2) 0.0180(5) Uani 1 1 d . . . H1A H 0.1332 0.1849 -0.1740 0.022 Uiso 1 1 calc R . . C2 C 0.2359(3) 0.3118(2) -0.3354(2) 0.0211(5) Uani 1 1 d . . . H2A H 0.2079 0.2742 -0.3825 0.025 Uiso 1 1 calc R . . C3 C 0.3213(3) 0.4201(2) -0.3915(2) 0.0227(5) Uani 1 1 d . . . H3A H 0.3508 0.4576 -0.4769 0.027 Uiso 1 1 calc R . . C4 C 0.3620(3) 0.4716(2) -0.3209(2) 0.0212(5) Uani 1 1 d . . . H4A H 0.4209 0.5450 -0.3577 0.025 Uiso 1 1 calc R . . C5 C 0.3176(2) 0.4172(2) -0.1959(2) 0.0186(5) Uani 1 1 d . . . H5A H 0.3486 0.4540 -0.1493 0.022 Uiso 1 1 calc R . . C6 C 0.2292(2) 0.3104(2) -0.1362(2) 0.0158(4) Uani 1 1 d . . . C7 C -0.0029(2) 0.2307(2) 0.02841(19) 0.0176(5) Uani 1 1 d . . . H7A H -0.0287 0.2171 -0.0392 0.021 Uiso 1 1 calc R . . H7B H -0.0495 0.3126 0.0233 0.021 Uiso 1 1 calc R . . C8 C -0.2638(2) 0.1425(2) 0.2022(2) 0.0192(5) Uani 1 1 d . . . C9 C -0.3238(3) 0.0302(2) 0.3205(2) 0.0232(5) Uani 1 1 d . . . H9A H -0.4257 0.0468 0.3403 0.035 Uiso 1 1 calc R . . H9B H -0.2722 0.0211 0.3865 0.035 Uiso 1 1 calc R . . H9C H -0.3119 -0.0494 0.3106 0.035 Uiso 1 1 calc R . . C10 C -0.3373(3) 0.1544(3) 0.0966(2) 0.0255(5) Uani 1 1 d . . . H10A H -0.4403 0.1698 0.1131 0.038 Uiso 1 1 calc R . . H10B H -0.3215 0.0744 0.0875 0.038 Uiso 1 1 calc R . . H10C H -0.2973 0.2266 0.0213 0.038 Uiso 1 1 calc R . . C11 C -0.2795(3) 0.2671(2) 0.2158(2) 0.0262(6) Uani 1 1 d . . . H11A H -0.3813 0.2877 0.2311 0.039 Uiso 1 1 calc R . . H11B H -0.2356 0.3373 0.1408 0.039 Uiso 1 1 calc R . . H11C H -0.2316 0.2566 0.2842 0.039 Uiso 1 1 calc R . . C12 C 0.2154(2) 0.3351(2) 0.0716(2) 0.0183(5) Uani 1 1 d . . . H12A H 0.2142 0.4267 0.0108 0.022 Uiso 1 1 calc R . . H12B H 0.3137 0.3120 0.0936 0.022 Uiso 1 1 calc R . . C13 C 0.1820(3) 0.3759(2) 0.2925(2) 0.0187(5) Uani 1 1 d . . . C14 C 0.0611(3) 0.3928(3) 0.3818(2) 0.0259(5) Uani 1 1 d . . . H14A H 0.0994 0.4263 0.4307 0.039 Uiso 1 1 calc R . . H14B H 0.0174 0.3093 0.4355 0.039 Uiso 1 1 calc R . . H14C H -0.0114 0.4536 0.3366 0.039 Uiso 1 1 calc R . . C15 C 0.2470(3) 0.5066(2) 0.2044(2) 0.0283(6) Uani 1 1 d . . . H15A H 0.2890 0.5420 0.2501 0.042 Uiso 1 1 calc R . . H15B H 0.1719 0.5660 0.1618 0.042 Uiso 1 1 calc R . . H15C H 0.3215 0.4954 0.1449 0.042 Uiso 1 1 calc R . . C16 C 0.2969(3) 0.2799(2) 0.3580(2) 0.0221(5) Uani 1 1 d . . . H16A H 0.3452 0.3151 0.4005 0.033 Uiso 1 1 calc R . . H16B H 0.3671 0.2642 0.2984 0.033 Uiso 1 1 calc R . . H16C H 0.2524 0.1986 0.4171 0.033 Uiso 1 1 calc R . . C17 C 0.2548(2) 0.1002(2) 0.06869(19) 0.0168(4) Uani 1 1 d . . . H17A H 0.3525 0.1056 0.0241 0.020 Uiso 1 1 calc R . . H17B H 0.2013 0.0383 0.0569 0.020 Uiso 1 1 calc R . . C18 C 0.2875(2) -0.1376(2) 0.2906(2) 0.0178(5) Uani 1 1 d . . . C19 C 0.3203(3) -0.1852(2) 0.4208(2) 0.0229(5) Uani 1 1 d . . . H19A H 0.3317 -0.2794 0.4586 0.034 Uiso 1 1 calc R . . H19B H 0.2411 -0.1600 0.4679 0.034 Uiso 1 1 calc R . . H19C H 0.4089 -0.1469 0.4195 0.034 Uiso 1 1 calc R . . C20 C 0.4151(3) -0.1671(2) 0.2133(2) 0.0230(5) Uani 1 1 d . . . H20A H 0.4352 -0.2602 0.2491 0.034 Uiso 1 1 calc R . . H20B H 0.4993 -0.1224 0.2108 0.034 Uiso 1 1 calc R . . H20C H 0.3925 -0.1375 0.1303 0.034 Uiso 1 1 calc R . . C21 C 0.1506(3) -0.1969(2) 0.2892(2) 0.0234(5) Uani 1 1 d . . . H21A H 0.1630 -0.2910 0.3245 0.035 Uiso 1 1 calc R . . H21B H 0.1308 -0.1639 0.2051 0.035 Uiso 1 1 calc R . . H21C H 0.0704 -0.1740 0.3371 0.035 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01596(15) 0.01490(15) 0.01180(14) -0.00443(11) -0.00052(11) -0.00062(11) B1 0.0159(12) 0.0164(12) 0.0138(12) -0.0068(10) -0.0012(9) -0.0008(9) S1 0.0145(3) 0.0159(3) 0.0158(3) -0.0064(2) -0.0014(2) -0.0004(2) S2 0.0183(3) 0.0157(3) 0.0132(3) -0.0064(2) -0.0012(2) -0.0008(2) S3 0.0147(3) 0.0140(3) 0.0136(3) -0.0043(2) -0.0019(2) 0.0006(2) S4 0.0190(4) 0.0168(4) 0.0125(4) -0.0050(3) -0.0002(3) -0.0016(3) C1 0.0190(11) 0.0170(11) 0.0174(11) -0.0071(9) -0.0029(9) 0.0005(9) C2 0.0231(12) 0.0251(12) 0.0179(11) -0.0121(10) -0.0046(9) 0.0033(10) C3 0.0250(12) 0.0230(12) 0.0123(11) -0.0026(9) 0.0000(9) 0.0035(10) C4 0.0234(12) 0.0151(11) 0.0179(11) -0.0027(9) 0.0022(9) -0.0007(9) C5 0.0203(11) 0.0161(11) 0.0177(11) -0.0069(9) 0.0004(9) -0.0002(9) C6 0.0150(11) 0.0143(10) 0.0161(11) -0.0052(9) -0.0030(8) 0.0032(8) C7 0.0184(11) 0.0190(11) 0.0117(10) -0.0038(9) -0.0012(8) -0.0002(9) C8 0.0145(11) 0.0197(11) 0.0209(12) -0.0076(10) -0.0002(9) -0.0002(9) C9 0.0189(12) 0.0240(12) 0.0214(12) -0.0061(10) 0.0019(9) -0.0043(10) C10 0.0162(11) 0.0325(14) 0.0257(13) -0.0101(11) -0.0053(10) -0.0007(10) C11 0.0190(12) 0.0218(12) 0.0357(15) -0.0135(11) 0.0043(10) 0.0009(10) C12 0.0210(11) 0.0171(11) 0.0137(11) -0.0051(9) 0.0004(9) -0.0004(9) C13 0.0242(12) 0.0167(11) 0.0166(11) -0.0078(9) -0.0042(9) -0.0021(9) C14 0.0285(13) 0.0335(14) 0.0232(13) -0.0199(11) -0.0026(10) 0.0023(11) C15 0.0410(16) 0.0208(13) 0.0247(13) -0.0095(11) -0.0058(11) -0.0087(11) C16 0.0212(12) 0.0254(13) 0.0224(12) -0.0117(10) -0.0055(10) -0.0023(10) C17 0.0187(11) 0.0178(11) 0.0120(10) -0.0060(9) 0.0000(8) 0.0012(9) C18 0.0209(11) 0.0119(10) 0.0180(11) -0.0042(9) -0.0051(9) 0.0034(9) C19 0.0286(13) 0.0177(11) 0.0178(12) -0.0040(10) -0.0042(10) 0.0021(10) C20 0.0210(12) 0.0199(12) 0.0270(13) -0.0107(10) -0.0035(10) 0.0068(9) C21 0.0255(13) 0.0156(11) 0.0264(13) -0.0071(10) -0.0008(10) -0.0037(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 S4 2.0714(4) . ? Ni1 S3 2.2839(6) . ? Ni1 S1 2.2869(6) . ? Ni1 S2 2.2948(7) . ? B1 C6 1.637(3) . ? B1 C12 1.654(3) . ? B1 C17 1.662(3) . ? B1 C7 1.666(3) . ? S1 C7 1.815(2) . ? S1 C8 1.855(2) . ? S2 C12 1.809(2) . ? S2 C13 1.852(2) . ? S3 C17 1.811(2) . ? S3 C18 1.856(2) . ? S4 Ni1 2.0714(4) 2_556 ? C1 C2 1.393(3) . ? C1 C6 1.405(3) . ? C2 C3 1.393(3) . ? C3 C4 1.377(3) . ? C4 C5 1.393(3) . ? C5 C6 1.399(3) . ? C8 C11 1.522(3) . ? C8 C10 1.526(3) . ? C8 C9 1.525(3) . ? C13 C14 1.523(3) . ? C13 C16 1.526(3) . ? C13 C15 1.531(3) . ? C18 C21 1.529(3) . ? C18 C19 1.528(3) . ? C18 C20 1.530(3) . ? 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 S4 Ni1 S3 118.03(2) . . ? S4 Ni1 S1 124.52(2) . . ? S3 Ni1 S1 94.07(2) . . ? S4 Ni1 S2 125.491(19) . . ? S3 Ni1 S2 94.89(2) . . ? S1 Ni1 S2 91.79(2) . . ? C6 B1 C12 110.28(18) . . ? C6 B1 C17 106.54(17) . . ? C12 B1 C17 111.09(18) . . ? C6 B1 C7 107.51(17) . . ? C12 B1 C7 110.37(18) . . ? C17 B1 C7 110.91(18) . . ? C7 S1 C8 105.85(10) . . ? C7 S1 Ni1 105.60(8) . . ? C8 S1 Ni1 111.35(8) . . ? C12 S2 C13 107.28(11) . . ? C12 S2 Ni1 105.36(8) . . ? C13 S2 Ni1 111.01(7) . . ? C17 S3 C18 106.02(10) . . ? C17 S3 Ni1 106.52(7) . . ? C18 S3 Ni1 111.30(8) . . ? Ni1 S4 Ni1 180.0 . 2_556 ? C2 C1 C6 122.5(2) . . ? C1 C2 C3 120.1(2) . . ? C4 C3 C2 118.8(2) . . ? C3 C4 C5 120.6(2) . . ? C4 C5 C6 122.5(2) . . ? C5 C6 C1 115.5(2) . . ? C5 C6 B1 124.0(2) . . ? C1 C6 B1 120.54(19) . . ? B1 C7 S1 113.69(15) . . ? C11 C8 C10 111.3(2) . . ? C11 C8 C9 110.4(2) . . ? C10 C8 C9 110.50(19) . . ? C11 C8 S1 111.24(16) . . ? C10 C8 S1 107.39(16) . . ? C9 C8 S1 105.83(16) . . ? B1 C12 S2 112.18(15) . . ? C14 C13 C16 111.84(19) . . ? C14 C13 C15 110.0(2) . . ? C16 C13 C15 110.8(2) . . ? C14 C13 S2 104.20(16) . . ? C16 C13 S2 110.95(16) . . ? C15 C13 S2 108.77(16) . . ? B1 C17 S3 112.71(15) . . ? C21 C18 C19 110.86(19) . . ? C21 C18 C20 111.36(19) . . ? C19 C18 C20 110.06(19) . . ? C21 C18 S3 111.03(15) . . ? C19 C18 S3 105.56(15) . . ? C20 C18 S3 107.77(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S4 Ni1 S1 C7 165.51(8) . . . . ? S3 Ni1 S1 C7 -66.12(8) . . . . ? S2 Ni1 S1 C7 28.92(8) . . . . ? S4 Ni1 S1 C8 51.08(8) . . . . ? S3 Ni1 S1 C8 179.45(8) . . . . ? S2 Ni1 S1 C8 -85.51(8) . . . . ? S4 Ni1 S2 C12 153.51(8) . . . . ? S3 Ni1 S2 C12 23.70(8) . . . . ? S1 Ni1 S2 C12 -70.54(8) . . . . ? S4 Ni1 S2 C13 37.69(9) . . . . ? S3 Ni1 S2 C13 -92.12(8) . . . . ? S1 Ni1 S2 C13 173.64(8) . . . . ? S4 Ni1 S3 C17 160.57(8) . . . . ? S1 Ni1 S3 C17 27.61(8) . . . . ? S2 Ni1 S3 C17 -64.54(8) . . . . ? S4 Ni1 S3 C18 45.45(8) . . . . ? S1 Ni1 S3 C18 -87.52(8) . . . . ? S2 Ni1 S3 C18 -179.67(8) . . . . ? S3 Ni1 S4 Ni1 -41(4) . . . 2_556 ? S1 Ni1 S4 Ni1 76(4) . . . 2_556 ? S2 Ni1 S4 Ni1 -161(4) . . . 2_556 ? C6 C1 C2 C3 0.1(3) . . . . ? C1 C2 C3 C4 1.0(3) . . . . ? C2 C3 C4 C5 -0.5(3) . . . . ? C3 C4 C5 C6 -1.0(4) . . . . ? C4 C5 C6 C1 1.9(3) . . . . ? C4 C5 C6 B1 -179.6(2) . . . . ? C2 C1 C6 C5 -1.5(3) . . . . ? C2 C1 C6 B1 180.0(2) . . . . ? C12 B1 C6 C5 9.1(3) . . . . ? C17 B1 C6 C5 -111.5(2) . . . . ? C7 B1 C6 C5 129.5(2) . . . . ? C12 B1 C6 C1 -172.43(19) . . . . ? C17 B1 C6 C1 66.9(2) . . . . ? C7 B1 C6 C1 -52.0(3) . . . . ? C6 B1 C7 S1 152.88(15) . . . . ? C12 B1 C7 S1 -86.8(2) . . . . ? C17 B1 C7 S1 36.8(2) . . . . ? C8 S1 C7 B1 156.73(16) . . . . ? Ni1 S1 C7 B1 38.55(17) . . . . ? C7 S1 C8 C11 -61.96(19) . . . . ? Ni1 S1 C8 C11 52.32(18) . . . . ? C7 S1 C8 C10 60.03(18) . . . . ? Ni1 S1 C8 C10 174.31(14) . . . . ? C7 S1 C8 C9 178.08(16) . . . . ? Ni1 S1 C8 C9 -67.64(16) . . . . ? C6 B1 C12 S2 152.37(15) . . . . ? C17 B1 C12 S2 -89.73(19) . . . . ? C7 B1 C12 S2 33.7(2) . . . . ? C13 S2 C12 B1 161.32(15) . . . . ? Ni1 S2 C12 B1 42.97(16) . . . . ? C12 S2 C13 C14 164.41(16) . . . . ? Ni1 S2 C13 C14 -80.97(16) . . . . ? C12 S2 C13 C16 -75.08(18) . . . . ? Ni1 S2 C13 C16 39.55(18) . . . . ? C12 S2 C13 C15 47.08(19) . . . . ? Ni1 S2 C13 C15 161.71(15) . . . . ? C6 B1 C17 S3 156.59(15) . . . . ? C12 B1 C17 S3 36.4(2) . . . . ? C7 B1 C17 S3 -86.70(19) . . . . ? C18 S3 C17 B1 157.34(15) . . . . ? Ni1 S3 C17 B1 38.70(16) . . . . ? C17 S3 C18 C21 -68.15(18) . . . . ? Ni1 S3 C18 C21 47.28(17) . . . . ? C17 S3 C18 C19 171.65(15) . . . . ? Ni1 S3 C18 C19 -72.92(16) . . . . ? C17 S3 C18 C20 54.05(18) . . . . ? Ni1 S3 C18 C20 169.49(13) . . . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.619 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.082