# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Mariano Laguna' _publ_contact_author_email MLAGUNA@UNIZAR.ES _publ_section_title ; S,C- and S,S-coupling via dithiolate transfer reactions from tin to nickel complexes ; loop_ _publ_author_name 'Mariano Laguna' 'Elena Cerrada' 'Ana Moreno' # Attachment 'compounds3-13revised.txt' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 718386' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H33 Ni P S5' _chemical_formula_weight 751.63 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' 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' _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 10.329(3) _cell_length_b 18.632(4) _cell_length_c 18.775(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.72(3) _cell_angle_gamma 90.00 _cell_volume 3605.6(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 37872 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular block' _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 0.900 _exptl_absorpt_correction_type 'Semi-empirical from equivalents' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Crysta (1995), A51, 33-38 ; _exptl_special_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Phi+Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37872 _diffrn_reflns_av_R_equivalents 0.1010 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.04 _reflns_number_total 6362 _reflns_number_gt 4710 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO and COLLECT(Hooft,1998)' _computing_cell_refinement 'DENZO and COLLECT' _computing_data_reduction 'DENZO and COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v.5 (Siemens)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+2.1898P] 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 6362 _refine_ls_number_parameters 420 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1210 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _refine_ls_shift/su_max 0.005 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.21334(4) 0.46017(2) 0.23610(2) 0.02542(14) Uani 1 d . . . S1 S 0.07450(8) 0.46326(4) 0.32005(4) 0.0258(2) Uani 1 d . . . S2 S 0.10112(9) 0.37420(5) 0.17692(5) 0.0347(2) Uani 1 d . . . S3 S -0.15227(9) 0.30338(5) 0.20713(5) 0.0372(2) Uani 1 d . . . S4 S -0.37319(9) 0.26787(5) 0.29549(6) 0.0458(3) Uani 1 d . . . S5 S -0.17346(9) 0.37640(5) 0.34120(5) 0.0361(2) Uani 1 d . . . P1 P 0.34029(8) 0.47568(4) 0.14950(5) 0.0256(2) Uani 1 d . . . C1 C -0.0402(3) 0.39779(17) 0.29285(17) 0.0269(7) Uani 1 d . . . C2 C -0.0281(3) 0.36444(17) 0.23067(18) 0.0299(8) Uani 1 d . . . C3 C -0.2413(3) 0.31350(17) 0.2821(2) 0.0331(8) Uani 1 d . . . C4 C 0.1338(3) 0.43323(17) 0.40701(17) 0.0275(7) Uani 1 d . . . C5 C 0.1603(3) 0.36065(17) 0.42220(18) 0.0316(8) Uani 1 d . . . C6 C 0.1891(3) 0.34192(19) 0.4932(2) 0.0381(9) Uani 1 d . . . H6 H 0.2031 0.2938 0.5043 0.046 Uiso 1 calc R . . C7 C 0.1979(3) 0.3919(2) 0.54808(19) 0.0374(9) Uani 1 d . . . C8 C 0.1811(3) 0.46322(18) 0.52987(19) 0.0351(8) Uani 1 d . . . H8 H 0.1930 0.4976 0.5656 0.042 Uiso 1 calc R . . C9 C 0.1471(3) 0.48610(18) 0.46042(18) 0.0298(8) Uani 1 d . . . C10 C 0.1300(4) 0.56440(17) 0.44721(19) 0.0352(8) Uani 1 d . . . H10A H 0.2112 0.5850 0.4357 0.053 Uiso 1 calc R . . H10B H 0.1010 0.5870 0.4893 0.053 Uiso 1 calc R . . H10C H 0.0667 0.5717 0.4081 0.053 Uiso 1 calc R . . C11 C 0.1639(4) 0.30245(18) 0.3666(2) 0.0453(10) Uani 1 d . . . H11A H 0.2230 0.2655 0.3833 0.068 Uiso 1 calc R . . H11B H 0.1922 0.3224 0.3231 0.068 Uiso 1 calc R . . H11C H 0.0787 0.2824 0.3579 0.068 Uiso 1 calc R . . C12 C 0.2205(4) 0.3698(2) 0.6246(2) 0.0522(11) Uani 1 d . . . H12A H 0.2165 0.3184 0.6280 0.078 Uiso 1 calc R . . H12B H 0.1550 0.3907 0.6521 0.078 Uiso 1 calc R . . H12C H 0.3045 0.3861 0.6427 0.078 Uiso 1 calc R . . C13 C 0.3030(3) 0.53465(16) 0.29154(18) 0.0263(7) Uani 1 d . . . C14 C 0.2631(3) 0.60648(17) 0.28782(18) 0.0294(8) Uani 1 d . . . C15 C 0.3231(3) 0.65673(18) 0.33316(19) 0.0341(8) Uani 1 d . . . H15 H 0.2992 0.7047 0.3283 0.041 Uiso 1 calc R . . C16 C 0.4171(3) 0.63789(19) 0.3851(2) 0.0385(9) Uani 1 d . . . C17 C 0.4565(3) 0.56618(19) 0.3888(2) 0.0374(9) Uani 1 d . . . H17 H 0.5199 0.5525 0.4236 0.045 Uiso 1 calc R . . C18 C 0.4034(3) 0.51494(17) 0.34195(18) 0.0294(8) Uani 1 d . . . C19 C 0.4546(4) 0.43874(18) 0.3459(2) 0.0393(9) Uani 1 d . . . H19A H 0.3834 0.4057 0.3400 0.059 Uiso 1 calc R . . H19B H 0.5001 0.4310 0.3914 0.059 Uiso 1 calc R . . H19C H 0.5126 0.4312 0.3087 0.059 Uiso 1 calc R . . C20 C 0.4699(4) 0.6923(2) 0.4398(2) 0.0577(12) Uani 1 d . . . H20A H 0.5618 0.6973 0.4365 0.087 Uiso 1 calc R . . H20B H 0.4526 0.6762 0.4869 0.087 Uiso 1 calc R . . H20C H 0.4285 0.7379 0.4307 0.087 Uiso 1 calc R . . C21 C 0.1528(4) 0.63115(19) 0.2360(2) 0.0420(9) Uani 1 d . . . C31 C 0.3595(3) 0.39312(17) 0.09690(17) 0.0274(7) Uani 1 d . . . H31 H 0.3509 0.4360 0.1214 0.033 Uiso 1 calc R . . C32 C 0.3275(3) 0.38987(19) 0.02458(19) 0.0356(8) Uani 1 d . . . H32 H 0.2975 0.4306 0.0002 0.043 Uiso 1 calc R . . C33 C 0.3400(4) 0.3258(2) -0.0117(2) 0.0452(10) Uani 1 d . . . H33 H 0.3163 0.3233 -0.0603 0.054 Uiso 1 calc R . . C34 C 0.3872(4) 0.26560(19) 0.0238(2) 0.0464(10) Uani 1 d . . . H34 H 0.3972 0.2230 -0.0011 0.056 Uiso 1 calc R . . C35 C 0.4194(4) 0.26843(19) 0.0956(2) 0.0422(9) Uani 1 d . . . H35 H 0.4512 0.2277 0.1195 0.051 Uiso 1 calc R . . C36 C 0.4046(4) 0.33217(18) 0.1331(2) 0.0377(9) Uani 1 d . . . H36 H 0.4249 0.3339 0.1820 0.045 Uiso 1 calc R . . C41 C 0.2665(3) 0.53973(16) 0.08411(18) 0.0284(8) Uani 1 d . . . H41 H 0.3059 0.5085 0.1175 0.034 Uiso 1 calc R . . C42 C 0.1320(4) 0.54189(19) 0.0734(2) 0.0384(9) Uani 1 d . . . H42 H 0.0810 0.5115 0.0992 0.046 Uiso 1 calc R . . C43 C 0.0739(4) 0.5892(2) 0.0242(2) 0.0473(10) Uani 1 d . . . H43 H -0.0159 0.5904 0.0166 0.057 Uiso 1 calc R . . C44 C 0.1496(4) 0.6344(2) -0.0132(2) 0.0490(11) Uani 1 d . . . H44 H 0.1107 0.6668 -0.0456 0.059 Uiso 1 calc R . . C45 C 0.2810(4) 0.63207(19) -0.0031(2) 0.0451(10) Uani 1 d . . . H45 H 0.3313 0.6630 -0.0288 0.054 Uiso 1 calc R . . C46 C 0.3407(4) 0.58452(18) 0.04468(19) 0.0378(9) Uani 1 d . . . H46 H 0.4307 0.5826 0.0504 0.045 Uiso 1 calc R . . C51 C 0.5078(3) 0.50957(18) 0.16514(18) 0.0299(8) Uani 1 d . . . H51 H 0.4243 0.4910 0.1587 0.036 Uiso 1 calc R . . C52 C 0.5276(3) 0.57859(18) 0.19117(19) 0.0355(8) Uani 1 d . . . H52 H 0.4571 0.6063 0.2027 0.043 Uiso 1 calc R . . C53 C 0.6511(4) 0.6063(2) 0.20002(19) 0.0411(9) Uani 1 d . . . H53 H 0.6637 0.6529 0.2168 0.049 Uiso 1 calc R . . C54 C 0.7564(4) 0.5651(2) 0.1840(2) 0.0465(10) Uani 1 d . . . H54 H 0.8399 0.5837 0.1904 0.056 Uiso 1 calc R . . C55 C 0.7374(4) 0.4966(2) 0.1587(2) 0.0490(10) Uani 1 d . . . H55 H 0.8083 0.4687 0.1480 0.059 Uiso 1 calc R . . C56 C 0.6133(3) 0.46870(19) 0.1489(2) 0.0385(9) Uani 1 d . . . H56 H 0.6010 0.4223 0.1314 0.046 Uiso 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 0.0276(2) 0.0238(2) 0.0251(2) -0.00124(17) 0.00362(18) -0.00320(17) S1 0.0275(4) 0.0244(4) 0.0256(4) -0.0013(3) 0.0024(3) -0.0026(3) S2 0.0399(5) 0.0347(5) 0.0303(5) -0.0078(4) 0.0092(4) -0.0120(4) S3 0.0396(5) 0.0352(5) 0.0370(5) -0.0067(4) 0.0043(4) -0.0133(4) S4 0.0322(5) 0.0374(5) 0.0686(7) -0.0025(5) 0.0094(5) -0.0092(4) S5 0.0317(5) 0.0373(5) 0.0403(5) -0.0075(4) 0.0100(4) -0.0078(4) P1 0.0274(5) 0.0232(4) 0.0265(5) -0.0002(3) 0.0030(4) -0.0018(3) C1 0.0240(18) 0.0257(17) 0.0314(19) -0.0019(15) 0.0038(14) -0.0033(13) C2 0.0286(19) 0.0271(17) 0.0336(19) 0.0022(15) -0.0002(15) -0.0067(14) C3 0.0296(19) 0.0265(17) 0.043(2) 0.0005(16) -0.0007(16) -0.0006(15) C4 0.0286(18) 0.0279(17) 0.0262(18) 0.0015(14) 0.0052(14) -0.0031(14) C5 0.0328(19) 0.0282(18) 0.034(2) 0.0022(15) 0.0027(15) 0.0022(15) C6 0.036(2) 0.0328(19) 0.045(2) 0.0087(17) 0.0001(17) 0.0027(16) C7 0.033(2) 0.046(2) 0.033(2) 0.0051(17) -0.0018(16) 0.0016(16) C8 0.037(2) 0.041(2) 0.0272(19) -0.0045(16) 0.0005(16) -0.0047(16) C9 0.0257(18) 0.0313(18) 0.033(2) 0.0002(15) 0.0059(15) -0.0035(14) C10 0.042(2) 0.0277(18) 0.037(2) -0.0058(16) 0.0101(17) -0.0052(16) C11 0.060(3) 0.0278(19) 0.048(2) -0.0015(17) 0.000(2) 0.0084(18) C12 0.053(3) 0.069(3) 0.034(2) 0.014(2) -0.0013(19) 0.001(2) C13 0.0260(18) 0.0254(17) 0.0280(18) -0.0015(14) 0.0068(14) -0.0033(13) C14 0.0292(19) 0.0268(17) 0.0330(19) -0.0006(15) 0.0077(15) 0.0001(14) C15 0.036(2) 0.0244(17) 0.043(2) -0.0013(16) 0.0116(17) -0.0017(15) C16 0.033(2) 0.036(2) 0.047(2) -0.0097(17) 0.0055(18) -0.0075(16) C17 0.0290(19) 0.043(2) 0.040(2) -0.0046(17) -0.0011(16) -0.0030(16) C18 0.0261(18) 0.0296(17) 0.0328(19) 0.0002(15) 0.0049(15) -0.0010(14) C19 0.036(2) 0.0350(19) 0.046(2) -0.0005(17) -0.0025(17) 0.0053(16) C20 0.057(3) 0.046(2) 0.069(3) -0.020(2) -0.002(2) -0.008(2) C21 0.047(2) 0.036(2) 0.042(2) 0.0018(17) -0.0057(18) 0.0132(18) C31 0.0283(18) 0.0229(16) 0.0319(19) -0.0035(14) 0.0098(15) -0.0025(13) C32 0.040(2) 0.0316(18) 0.035(2) 0.0000(16) 0.0041(16) -0.0037(16) C33 0.060(3) 0.039(2) 0.037(2) -0.0104(18) 0.0070(19) -0.0062(19) C34 0.056(3) 0.0274(19) 0.059(3) -0.0105(19) 0.022(2) -0.0021(18) C35 0.046(2) 0.0260(18) 0.056(3) 0.0029(18) 0.017(2) 0.0017(16) C36 0.044(2) 0.0325(19) 0.038(2) 0.0041(17) 0.0097(17) 0.0012(16) C41 0.036(2) 0.0208(16) 0.0277(18) 0.0006(14) -0.0008(15) 0.0018(14) C42 0.037(2) 0.039(2) 0.039(2) 0.0003(17) -0.0006(17) -0.0030(17) C43 0.045(2) 0.044(2) 0.050(3) 0.000(2) -0.013(2) 0.0059(19) C44 0.073(3) 0.033(2) 0.040(2) 0.0051(18) -0.006(2) 0.015(2) C45 0.066(3) 0.031(2) 0.038(2) 0.0073(17) 0.007(2) -0.0002(19) C46 0.047(2) 0.0283(18) 0.040(2) 0.0034(16) 0.0138(18) 0.0013(16) C51 0.0256(18) 0.0350(18) 0.0292(18) 0.0022(15) 0.0019(14) -0.0061(15) C52 0.037(2) 0.0325(19) 0.038(2) -0.0033(16) 0.0123(16) -0.0038(16) C53 0.049(2) 0.041(2) 0.033(2) -0.0044(17) 0.0044(18) -0.0171(18) C54 0.034(2) 0.058(3) 0.047(2) 0.003(2) -0.0030(18) -0.0121(19) C55 0.031(2) 0.051(2) 0.064(3) 0.003(2) -0.0010(19) 0.0040(18) C56 0.033(2) 0.0347(19) 0.048(2) -0.0007(17) 0.0025(17) -0.0010(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C13 1.934(3) . ? Ni1 P1 2.1732(9) . ? Ni1 S1 2.1995(9) . ? Ni1 S2 2.2308(9) . ? S1 C1 1.753(3) . ? S1 C4 1.796(3) . ? S2 C2 1.734(3) . ? S3 C3 1.740(4) . ? S3 C2 1.750(3) . ? S4 C3 1.639(3) . ? S5 C3 1.731(3) . ? S5 C1 1.743(3) . ? P1 C41 1.842(3) . ? P1 C31 1.846(3) . ? P1 C51 1.848(3) . ? C1 C2 1.336(5) . ? C4 C5 1.405(5) . ? C4 C9 1.406(5) . ? C5 C6 1.391(5) . ? C5 C11 1.507(5) . ? C6 C7 1.388(5) . ? C7 C8 1.380(5) . ? C7 C12 1.498(5) . ? C8 C9 1.395(5) . ? C9 C10 1.488(5) . ? C13 C14 1.401(4) . ? C13 C18 1.407(5) . ? C14 C15 1.385(5) . ? C14 C21 1.519(5) . ? C15 C16 1.377(5) . ? C16 C17 1.397(5) . ? C16 C20 1.519(5) . ? C17 C18 1.387(5) . ? C18 C19 1.515(5) . ? C31 C32 1.378(5) . ? C31 C36 1.388(5) . ? C32 C33 1.385(5) . ? C33 C34 1.377(5) . ? C34 C35 1.369(5) . ? C35 C36 1.393(5) . ? C41 C46 1.381(5) . ? C41 C42 1.391(5) . ? C42 C43 1.385(5) . ? C43 C44 1.372(6) . ? C44 C45 1.359(6) . ? C45 C46 1.378(5) . ? C51 C56 1.379(5) . ? C51 C52 1.386(5) . ? C52 C53 1.376(5) . ? C53 C54 1.380(5) . ? C54 C55 1.372(6) . ? C55 C56 1.385(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Ni1 P1 90.92(10) . . ? C13 Ni1 S1 84.68(10) . . ? P1 Ni1 S1 170.32(4) . . ? C13 Ni1 S2 176.62(10) . . ? P1 Ni1 S2 92.41(3) . . ? S1 Ni1 S2 91.94(3) . . ? C1 S1 C4 103.44(15) . . ? C1 S1 Ni1 103.46(11) . . ? C4 S1 Ni1 116.32(11) . . ? C2 S2 Ni1 100.37(11) . . ? C3 S3 C2 98.20(16) . . ? C3 S5 C1 96.96(16) . . ? C41 P1 C31 103.75(15) . . ? C41 P1 C51 103.15(15) . . ? C31 P1 C51 103.76(15) . . ? C41 P1 Ni1 109.94(11) . . ? C31 P1 Ni1 112.36(10) . . ? C51 P1 Ni1 122.07(11) . . ? C2 C1 S5 118.1(2) . . ? C2 C1 S1 118.6(3) . . ? S5 C1 S1 123.28(19) . . ? C1 C2 S2 125.4(3) . . ? C1 C2 S3 114.5(3) . . ? S2 C2 S3 120.0(2) . . ? S4 C3 S5 124.0(2) . . ? S4 C3 S3 123.8(2) . . ? S5 C3 S3 112.25(19) . . ? C5 C4 C9 121.4(3) . . ? C5 C4 S1 122.3(3) . . ? C9 C4 S1 116.2(2) . . ? C6 C5 C4 117.6(3) . . ? C6 C5 C11 118.0(3) . . ? C4 C5 C11 124.4(3) . . ? C7 C6 C5 122.9(3) . . ? C8 C7 C6 117.5(3) . . ? C8 C7 C12 120.8(3) . . ? C6 C7 C12 121.7(3) . . ? C7 C8 C9 123.1(3) . . ? C8 C9 C4 117.4(3) . . ? C8 C9 C10 118.4(3) . . ? C4 C9 C10 124.2(3) . . ? C14 C13 C18 119.0(3) . . ? C14 C13 Ni1 122.0(2) . . ? C18 C13 Ni1 118.8(2) . . ? C15 C14 C13 119.8(3) . . ? C15 C14 C21 118.4(3) . . ? C13 C14 C21 121.8(3) . . ? C16 C15 C14 122.0(3) . . ? C15 C16 C17 118.0(3) . . ? C15 C16 C20 121.0(3) . . ? C17 C16 C20 121.0(3) . . ? C18 C17 C16 121.6(3) . . ? C17 C18 C13 119.4(3) . . ? C17 C18 C19 119.4(3) . . ? C13 C18 C19 121.1(3) . . ? C32 C31 C36 119.8(3) . . ? C32 C31 P1 122.4(2) . . ? C36 C31 P1 117.7(3) . . ? C31 C32 C33 119.9(3) . . ? C34 C33 C32 120.4(4) . . ? C35 C34 C33 120.1(3) . . ? C34 C35 C36 120.1(3) . . ? C31 C36 C35 119.7(3) . . ? C46 C41 C42 119.2(3) . . ? C46 C41 P1 121.9(3) . . ? C42 C41 P1 118.8(3) . . ? C43 C42 C41 120.0(4) . . ? C44 C43 C42 119.7(4) . . ? C45 C44 C43 120.4(4) . . ? C44 C45 C46 120.8(4) . . ? C45 C46 C41 119.8(4) . . ? C56 C51 C52 119.3(3) . . ? C56 C51 P1 121.4(3) . . ? C52 C51 P1 119.2(3) . . ? C53 C52 C51 120.3(3) . . ? C52 C53 C54 120.2(3) . . ? C55 C54 C53 119.7(3) . . ? C54 C55 C56 120.4(4) . . ? C51 C56 C55 120.1(3) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.474 _refine_diff_density_min -0.750 _refine_diff_density_rms 0.111 #===END data_compound5 _database_code_depnum_ccdc_archive 'CCDC 718387' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H46 S10' _chemical_formula_weight 799.33 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.147(2) _cell_length_b 12.389(3) _cell_length_c 15.000(3) _cell_angle_alpha 74.124(4) _cell_angle_beta 75.996(4) _cell_angle_gamma 70.253(4) _cell_volume 2015.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1141 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 20.40 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 0.572 _exptl_absorpt_correction_type 'multi-scan correction' _exptl_absorpt_correction_T_min 0.911 _exptl_absorpt_correction_T_max 0.972 _exptl_absorpt_process_details ? _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 13552 _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_sigmaI/netI 0.2109 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 28.30 _reflns_number_total 9109 _reflns_number_gt 3481 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXTL' _computing_publication_material 'WinGX v1.10.01' _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^)+(0.0700P)^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 geometrically _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0080(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9109 _refine_ls_number_parameters 428 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1587 _refine_ls_R_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.2030 _refine_ls_wR_factor_gt 0.1574 _refine_ls_goodness_of_fit_ref 0.818 _refine_ls_restrained_S_all 0.818 _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 S1 S 0.83172(14) -0.11954(15) 0.19988(11) 0.0442(5) Uani 1 1 d . . . S2 S 1.00584(14) 0.01770(15) 0.16825(11) 0.0433(5) Uani 1 1 d . . . S3 S 0.91892(14) 0.18048(14) 0.00523(11) 0.0418(5) Uani 1 1 d . . . S4 S 0.72106(14) 0.07756(14) 0.01897(11) 0.0402(4) Uani 1 1 d . . . S5 S 0.58518(13) 0.20821(14) 0.07573(10) 0.0387(4) Uani 1 1 d . . . S6 S 0.66191(14) 0.41936(14) -0.04093(11) 0.0401(4) Uani 1 1 d . . . S7 S 0.65767(16) 0.62537(16) -0.19824(13) 0.0569(6) Uani 1 1 d . . . S8 S 0.50537(14) 0.47289(14) -0.17372(11) 0.0429(5) Uani 1 1 d . . . S9 S 0.39394(15) 0.27974(15) -0.06705(12) 0.0483(5) Uani 1 1 d . . . S10 S 1.13287(15) 0.19135(16) 0.06341(14) 0.0567(5) Uani 1 1 d . . . C1 C 0.8546(5) -0.1257(5) 0.3148(4) 0.0397(16) Uani 1 1 d . . . C2 C 0.7806(5) -0.0374(5) 0.3628(4) 0.0425(17) Uani 1 1 d . . . C3 C 0.8031(6) -0.0425(6) 0.4502(4) 0.0491(19) Uani 1 1 d . . . H3 H 0.7556 0.0177 0.4830 0.059 Uiso 1 1 calc R . . C4 C 0.8934(5) -0.1331(6) 0.4926(4) 0.0432(17) Uani 1 1 d . . . C5 C 0.9636(6) -0.2174(6) 0.4433(4) 0.0462(18) Uani 1 1 d . . . H5 H 1.0263 -0.2775 0.4705 0.055 Uiso 1 1 calc R . . C6 C 0.9468(5) -0.2188(5) 0.3544(4) 0.0405(16) Uani 1 1 d . . . C7 C 0.6803(5) 0.0647(6) 0.3229(5) 0.054(2) Uani 1 1 d . . . H7 H 0.6872 0.0619 0.2558 0.065 Uiso 1 1 calc R . . C8 C 0.9096(7) -0.1333(6) 0.5889(5) 0.059(2) Uani 1 1 d . . . H8 H 0.8868 -0.0499 0.5950 0.071 Uiso 1 1 calc R . . C9 C 1.0269(6) -0.3150(6) 0.3045(5) 0.055(2) Uani 1 1 d . . . H9 H 0.9884 -0.3142 0.2524 0.066 Uiso 1 1 calc R . . C10 C 0.6859(8) 0.1835(7) 0.3238(8) 0.133(5) Uani 1 1 d . . . H10A H 0.6727 0.1921 0.3889 0.199 Uiso 1 1 calc R . . H10B H 0.6246 0.2442 0.2908 0.199 Uiso 1 1 calc R . . H10C H 0.7642 0.1918 0.2921 0.199 Uiso 1 1 calc R . . C11 C 0.5639(6) 0.0472(7) 0.3725(6) 0.080(3) Uani 1 1 d . . . H11A H 0.5507 0.0564 0.4375 0.120 Uiso 1 1 calc R . . H11B H 0.5636 -0.0318 0.3725 0.120 Uiso 1 1 calc R . . H11C H 0.5005 0.1054 0.3403 0.120 Uiso 1 1 calc R . . C12 C 0.8273(7) -0.1924(8) 0.6627(5) 0.086(3) Uani 1 1 d . . . H12A H 0.7465 -0.1579 0.6485 0.129 Uiso 1 1 calc R . . H12B H 0.8288 -0.1812 0.7245 0.129 Uiso 1 1 calc R . . H12C H 0.8533 -0.2765 0.6630 0.129 Uiso 1 1 calc R . . C13 C 1.0357(7) -0.1912(8) 0.6077(5) 0.090(3) Uani 1 1 d . . . H13A H 1.0504 -0.2765 0.6256 0.135 Uiso 1 1 calc R . . H13B H 1.0470 -0.1630 0.6589 0.135 Uiso 1 1 calc R . . H13C H 1.0911 -0.1715 0.5508 0.135 Uiso 1 1 calc R . . C14 C 1.0470(6) -0.4357(6) 0.3676(5) 0.059(2) Uani 1 1 d . . . H14A H 1.0895 -0.4404 0.4170 0.088 Uiso 1 1 calc R . . H14B H 1.0941 -0.4948 0.3304 0.088 Uiso 1 1 calc R . . H14C H 0.9704 -0.4501 0.3963 0.088 Uiso 1 1 calc R . . C15 C 1.1464(7) -0.2944(6) 0.2612(6) 0.094(3) Uani 1 1 d . . . H15A H 1.1348 -0.2160 0.2205 0.141 Uiso 1 1 calc R . . H15B H 1.1932 -0.3536 0.2241 0.141 Uiso 1 1 calc R . . H15C H 1.1885 -0.3002 0.3112 0.141 Uiso 1 1 calc R . . C16 C 0.8849(5) -0.0004(5) 0.1375(4) 0.0362(15) Uani 1 1 d . . . C17 C 1.0258(5) 0.1347(5) 0.0767(4) 0.0385(16) Uani 1 1 d . . . C18 C 0.8424(5) 0.0774(5) 0.0625(4) 0.0369(15) Uani 1 1 d . . . C19 C 0.5743(5) 0.3287(5) -0.0209(4) 0.0349(15) Uani 1 1 d . . . C20 C 0.6104(5) 0.5128(5) -0.1407(4) 0.0391(16) Uani 1 1 d . . . C21 C 0.4986(5) 0.3528(5) -0.0817(4) 0.0360(15) Uani 1 1 d . . . C22 C 0.3656(6) 0.3153(5) -0.1840(4) 0.0414(16) Uani 1 1 d . . . C23 C 0.4496(6) 0.2571(5) -0.2522(5) 0.0460(17) Uani 1 1 d . . . C24 C 0.4264(6) 0.2878(6) -0.3428(5) 0.0520(19) Uani 1 1 d . . . H24 H 0.4828 0.2506 -0.3895 0.062 Uiso 1 1 calc R . . C25 C 0.3226(6) 0.3719(6) -0.3682(5) 0.0472(18) Uani 1 1 d . . . C26 C 0.2434(6) 0.4233(6) -0.2995(4) 0.0477(18) Uani 1 1 d . . . H26 H 0.1720 0.4796 -0.3162 0.057 Uiso 1 1 calc R . . C27 C 0.2596(5) 0.3992(5) -0.2074(4) 0.0394(16) Uani 1 1 d . . . C28 C 0.5631(6) 0.1611(6) -0.2256(5) 0.0533(19) Uani 1 1 d . . . H28 H 0.5945 0.1876 -0.1822 0.064 Uiso 1 1 calc R . . C29 C 0.3003(7) 0.4074(7) -0.4684(5) 0.060(2) Uani 1 1 d . . . H29 H 0.2123 0.4411 -0.4642 0.072 Uiso 1 1 calc R . . C30 C 0.1666(6) 0.4630(6) -0.1387(5) 0.0507(19) Uani 1 1 d . . . H30 H 0.1869 0.4231 -0.0747 0.061 Uiso 1 1 calc R . . C31 C 0.5368(7) 0.0446(6) -0.1734(6) 0.080(3) Uani 1 1 d . . . H31A H 0.4863 0.0543 -0.1126 0.120 Uiso 1 1 calc R . . H31B H 0.6114 -0.0167 -0.1633 0.120 Uiso 1 1 calc R . . H31C H 0.4958 0.0222 -0.2111 0.120 Uiso 1 1 calc R . . C32 C 0.6602(6) 0.1402(7) -0.3114(5) 0.079(3) Uani 1 1 d . . . H32A H 0.6395 0.0972 -0.3478 0.118 Uiso 1 1 calc R . . H32B H 0.7361 0.0942 -0.2904 0.118 Uiso 1 1 calc R . . H32C H 0.6671 0.2158 -0.3509 0.118 Uiso 1 1 calc R . . C33 C 0.3321(8) 0.3109(7) -0.5162(5) 0.094(3) Uani 1 1 d . . . H33A H 0.3177 0.3419 -0.5811 0.141 Uiso 1 1 calc R . . H33B H 0.2838 0.2579 -0.4835 0.141 Uiso 1 1 calc R . . H33C H 0.4162 0.2679 -0.5160 0.141 Uiso 1 1 calc R . . C34 C 0.3495(10) 0.5035(8) -0.5237(6) 0.120(4) Uani 1 1 d . . . H34A H 0.4355 0.4782 -0.5257 0.180 Uiso 1 1 calc R . . H34B H 0.3136 0.5718 -0.4944 0.180 Uiso 1 1 calc R . . H34C H 0.3321 0.5247 -0.5878 0.180 Uiso 1 1 calc R . . C35 C 0.0421(6) 0.4612(7) -0.1372(5) 0.065(2) Uani 1 1 d . . . H35A H 0.0164 0.5060 -0.1972 0.097 Uiso 1 1 calc R . . H35B H -0.0120 0.4964 -0.0859 0.097 Uiso 1 1 calc R . . H35C H 0.0413 0.3799 -0.1276 0.097 Uiso 1 1 calc R . . C36 C 0.1705(6) 0.5867(7) -0.1560(5) 0.071(2) Uani 1 1 d . . . H36A H 0.2507 0.5865 -0.1543 0.106 Uiso 1 1 calc R . . H36B H 0.1141 0.6254 -0.1073 0.106 Uiso 1 1 calc R . . H36C H 0.1492 0.6292 -0.2178 0.106 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 S1 0.0424(10) 0.0504(11) 0.0370(10) 0.0014(8) -0.0158(8) -0.0122(8) S2 0.0399(9) 0.0486(11) 0.0370(10) -0.0020(8) -0.0115(7) -0.0091(8) S3 0.0412(9) 0.0366(10) 0.0368(9) -0.0036(7) -0.0066(7) -0.0007(7) S4 0.0394(9) 0.0344(9) 0.0412(10) -0.0098(7) -0.0157(7) 0.0038(7) S5 0.0334(8) 0.0385(10) 0.0317(9) -0.0030(7) -0.0056(7) 0.0022(7) S6 0.0377(9) 0.0378(10) 0.0410(10) -0.0079(7) -0.0104(7) -0.0038(7) S7 0.0572(12) 0.0450(11) 0.0567(12) -0.0036(9) 0.0036(9) -0.0146(9) S8 0.0477(10) 0.0402(10) 0.0341(9) -0.0015(7) -0.0106(8) -0.0067(8) S9 0.0522(11) 0.0523(11) 0.0414(10) 0.0036(8) -0.0204(8) -0.0182(9) S10 0.0423(10) 0.0528(12) 0.0686(13) -0.0053(10) -0.0076(9) -0.0128(9) C1 0.028(3) 0.050(4) 0.029(3) -0.001(3) -0.004(3) -0.004(3) C2 0.031(3) 0.046(4) 0.038(4) 0.001(3) -0.004(3) -0.004(3) C3 0.048(4) 0.046(4) 0.038(4) -0.011(3) -0.002(3) 0.003(3) C4 0.047(4) 0.049(4) 0.030(4) -0.006(3) -0.002(3) -0.013(3) C5 0.047(4) 0.050(4) 0.035(4) -0.005(3) -0.019(3) 0.001(3) C6 0.037(4) 0.048(4) 0.028(3) -0.003(3) -0.007(3) -0.004(3) C7 0.042(4) 0.059(5) 0.036(4) 0.002(3) -0.007(3) 0.008(4) C8 0.078(5) 0.047(5) 0.045(4) -0.012(3) -0.018(4) -0.001(4) C9 0.048(4) 0.056(5) 0.044(4) -0.011(3) -0.018(3) 0.013(4) C10 0.078(6) 0.047(6) 0.255(14) 0.035(7) -0.086(8) -0.006(5) C11 0.048(5) 0.082(6) 0.094(7) -0.004(5) -0.017(4) -0.007(4) C12 0.108(7) 0.126(8) 0.028(4) -0.006(5) 0.001(4) -0.056(6) C13 0.092(7) 0.121(8) 0.067(6) -0.030(5) -0.042(5) -0.015(6) C14 0.054(4) 0.037(4) 0.078(6) -0.011(4) -0.010(4) -0.005(3) C15 0.088(6) 0.051(5) 0.081(6) 0.002(4) 0.038(5) 0.010(4) C16 0.032(3) 0.038(4) 0.036(4) -0.007(3) -0.006(3) -0.006(3) C17 0.041(4) 0.038(4) 0.031(3) -0.013(3) -0.005(3) 0.000(3) C18 0.036(3) 0.035(4) 0.034(4) -0.011(3) -0.006(3) 0.000(3) C19 0.033(3) 0.033(4) 0.029(3) -0.005(3) -0.010(3) 0.005(3) C20 0.037(4) 0.035(4) 0.036(4) -0.014(3) 0.003(3) -0.002(3) C21 0.042(4) 0.035(4) 0.025(3) -0.004(3) -0.007(3) -0.003(3) C22 0.049(4) 0.036(4) 0.042(4) 0.000(3) -0.020(3) -0.013(3) C23 0.043(4) 0.036(4) 0.057(5) -0.012(3) -0.013(3) -0.005(3) C24 0.053(4) 0.054(5) 0.052(5) -0.025(4) -0.010(4) -0.007(4) C25 0.052(4) 0.049(4) 0.041(4) -0.007(3) -0.015(3) -0.011(4) C26 0.057(4) 0.042(4) 0.042(4) -0.012(3) -0.015(3) -0.003(3) C27 0.042(4) 0.035(4) 0.039(4) -0.010(3) -0.014(3) -0.003(3) C28 0.043(4) 0.041(4) 0.081(5) -0.017(4) -0.027(4) -0.004(3) C29 0.059(5) 0.073(6) 0.047(5) -0.016(4) -0.014(4) -0.011(4) C30 0.061(5) 0.038(4) 0.051(4) -0.015(3) -0.023(4) 0.003(3) C31 0.072(5) 0.042(5) 0.114(7) -0.003(5) -0.026(5) -0.004(4) C32 0.055(5) 0.081(6) 0.091(7) -0.038(5) -0.010(5) 0.006(4) C33 0.156(9) 0.086(7) 0.038(5) -0.011(5) -0.027(5) -0.027(6) C34 0.203(12) 0.100(8) 0.086(7) 0.030(6) -0.077(8) -0.082(8) C35 0.063(5) 0.076(6) 0.049(5) -0.021(4) -0.003(4) -0.010(4) C36 0.061(5) 0.069(6) 0.091(6) -0.043(5) -0.023(4) -0.003(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 S1 C16 1.752(6) . ? S1 C1 1.789(6) . ? S2 C17 1.742(6) . ? S2 C16 1.740(6) . ? S3 C17 1.732(6) . ? S3 C18 1.746(6) . ? S4 C18 1.750(6) . ? S4 S5 2.083(2) . ? S5 C19 1.767(6) . ? S6 C19 1.719(7) . ? S6 C20 1.728(6) . ? S7 C20 1.632(6) . ? S8 C20 1.727(7) . ? S8 C21 1.740(6) . ? S9 C21 1.738(7) . ? S9 C22 1.777(6) . ? S10 C17 1.624(7) . ? C1 C2 1.406(8) . ? C1 C6 1.417(7) . ? C2 C3 1.384(8) . ? C2 C7 1.530(8) . ? C3 C4 1.407(8) . ? C4 C5 1.372(8) . ? C4 C8 1.504(9) . ? C5 C6 1.402(8) . ? C6 C9 1.511(8) . ? C7 C11 1.488(9) . ? C7 C10 1.499(11) . ? C8 C12 1.508(10) . ? C8 C13 1.515(9) . ? C9 C14 1.510(8) . ? C9 C15 1.515(10) . ? C16 C18 1.346(7) . ? C19 C21 1.354(7) . ? C22 C27 1.406(8) . ? C22 C23 1.418(8) . ? C23 C24 1.379(8) . ? C23 C28 1.540(8) . ? C24 C25 1.396(8) . ? C25 C26 1.363(8) . ? C25 C29 1.511(9) . ? C26 C27 1.380(8) . ? C27 C30 1.497(8) . ? C28 C32 1.535(9) . ? C28 C31 1.539(9) . ? C29 C33 1.454(10) . ? C29 C34 1.471(11) . ? C30 C36 1.498(9) . ? C30 C35 1.515(9) . ? 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 C16 S1 C1 99.2(3) . . ? C17 S2 C16 98.0(3) . . ? C17 S3 C18 98.0(3) . . ? C18 S4 S5 101.7(2) . . ? C19 S5 S4 101.81(19) . . ? C19 S6 C20 97.1(3) . . ? C20 S8 C21 97.8(3) . . ? C21 S9 C22 100.3(3) . . ? C2 C1 C6 122.1(6) . . ? C2 C1 S1 118.7(4) . . ? C6 C1 S1 119.2(5) . . ? C3 C2 C1 117.3(5) . . ? C3 C2 C7 118.7(6) . . ? C1 C2 C7 124.0(6) . . ? C2 C3 C4 122.7(6) . . ? C5 C4 C3 118.1(6) . . ? C5 C4 C8 122.8(6) . . ? C3 C4 C8 119.2(6) . . ? C4 C5 C6 122.8(6) . . ? C5 C6 C1 117.0(6) . . ? C5 C6 C9 119.9(5) . . ? C1 C6 C9 123.1(5) . . ? C11 C7 C10 111.3(7) . . ? C11 C7 C2 109.7(6) . . ? C10 C7 C2 114.3(6) . . ? C4 C8 C12 109.8(7) . . ? C4 C8 C13 114.0(6) . . ? C12 C8 C13 109.5(6) . . ? C6 C9 C14 113.1(6) . . ? C6 C9 C15 111.4(6) . . ? C14 C9 C15 108.6(5) . . ? C18 C16 S2 116.0(5) . . ? C18 C16 S1 124.5(5) . . ? S2 C16 S1 119.4(3) . . ? S10 C17 S3 125.8(4) . . ? S10 C17 S2 122.4(4) . . ? S3 C17 S2 111.8(4) . . ? C16 C18 S3 116.1(5) . . ? C16 C18 S4 124.3(5) . . ? S3 C18 S4 119.6(3) . . ? C21 C19 S6 117.7(4) . . ? C21 C19 S5 122.1(5) . . ? S6 C19 S5 120.1(3) . . ? S7 C20 S8 123.8(4) . . ? S7 C20 S6 123.5(4) . . ? S8 C20 S6 112.8(3) . . ? C19 C21 S9 124.3(5) . . ? C19 C21 S8 114.5(5) . . ? S9 C21 S8 121.0(3) . . ? C27 C22 C23 120.9(6) . . ? C27 C22 S9 119.7(5) . . ? C23 C22 S9 119.4(5) . . ? C24 C23 C22 118.2(6) . . ? C24 C23 C28 120.9(6) . . ? C22 C23 C28 120.9(6) . . ? C23 C24 C25 122.1(6) . . ? C26 C25 C24 117.4(6) . . ? C26 C25 C29 121.2(6) . . ? C24 C25 C29 121.4(6) . . ? C25 C26 C27 124.6(6) . . ? C26 C27 C22 116.8(6) . . ? C26 C27 C30 119.5(5) . . ? C22 C27 C30 123.7(6) . . ? C32 C28 C31 109.4(6) . . ? C32 C28 C23 112.4(6) . . ? C31 C28 C23 111.3(6) . . ? C33 C29 C34 112.8(7) . . ? C33 C29 C25 114.9(6) . . ? C34 C29 C25 112.1(7) . . ? C27 C30 C36 110.3(6) . . ? C27 C30 C35 114.3(6) . . ? C36 C30 C35 110.3(5) . . ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.530 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.150 #===END data_compound12 _database_code_depnum_ccdc_archive 'CCDC 718388' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H38 Ni3 P2 S6' _chemical_formula_weight 997.17 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.788(4) _cell_length_b 11.471(3) _cell_length_c 19.393(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.476(6) _cell_angle_gamma 90.00 _cell_volume 4171.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1651 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 20.59 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 1.750 _exptl_absorpt_correction_type 'multi-scan correction' _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_process_details ? _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 25949 _diffrn_reflns_av_R_equivalents 0.0856 _diffrn_reflns_av_sigmaI/netI 0.1666 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.00 _reflns_number_total 9036 _reflns_number_gt 4756 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXTL' _computing_publication_material 'WinGX v1.10.01' _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^)+(0.0102P)^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 9036 _refine_ls_number_parameters 498 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0991 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.0790 _refine_ls_wR_factor_gt 0.0688 _refine_ls_goodness_of_fit_ref 0.696 _refine_ls_restrained_S_all 0.696 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.31368(3) 1.16214(5) 0.14880(3) 0.02163(16) Uani 1 1 d . . . Ni2 Ni 0.32745(3) 0.94518(5) 0.13909(3) 0.02044(16) Uani 1 1 d . . . Ni3 Ni 0.21272(3) 1.02575(5) 0.17333(3) 0.02006(16) Uani 1 1 d . . . P1 P 0.40469(7) 0.81007(11) 0.10635(6) 0.0204(3) Uani 1 1 d . . . P2 P 0.10218(7) 1.01544(11) 0.20807(6) 0.0217(3) Uani 1 1 d . . . S1 S 0.21138(7) 1.19375(10) 0.09332(6) 0.0232(3) Uani 1 1 d . . . S2 S 0.36072(7) 1.09184(10) 0.05798(6) 0.0233(3) Uani 1 1 d . . . S3 S 0.40508(7) 1.08416(10) 0.20544(6) 0.0237(3) Uani 1 1 d . . . S4 S 0.25763(7) 1.19119(11) 0.24217(6) 0.0235(3) Uani 1 1 d . . . S5 S 0.21702(7) 0.89489(10) 0.08438(6) 0.0212(3) Uani 1 1 d . . . S6 S 0.27185(7) 0.87803(10) 0.23375(6) 0.0215(3) Uani 1 1 d . . . C1 C 0.2237(3) 1.1407(4) 0.0101(2) 0.0204(12) Uani 1 1 d . . . C2 C 0.1683(3) 1.1414(4) -0.0415(3) 0.0274(13) Uani 1 1 d . . . H2 H 0.1234 1.1685 -0.0314 0.033 Uiso 1 1 calc R . . C3 C 0.1798(3) 1.1020(4) -0.1072(3) 0.0305(14) Uani 1 1 d . . . H3 H 0.1428 1.1037 -0.1413 0.037 Uiso 1 1 calc R . . C4 C 0.2452(3) 1.0606(4) -0.1225(3) 0.0321(14) Uani 1 1 d . . . H4 H 0.2523 1.0354 -0.1671 0.039 Uiso 1 1 calc R . . C5 C 0.3010(3) 1.0556(4) -0.0725(2) 0.0279(13) Uani 1 1 d . . . H5 H 0.3449 1.0255 -0.0833 0.034 Uiso 1 1 calc R . . C6 C 0.2907(3) 1.0962(4) -0.0057(2) 0.0214(12) Uani 1 1 d . . . C7 C 0.3187(3) 1.1417(4) 0.3085(2) 0.0214(12) Uani 1 1 d . . . C8 C 0.3032(3) 1.1546(4) 0.3778(2) 0.0239(12) Uani 1 1 d . . . H8 H 0.2606 1.1890 0.3890 0.029 Uiso 1 1 calc R . . C9 C 0.3517(3) 1.1160(4) 0.4299(3) 0.0280(13) Uani 1 1 d . . . H9 H 0.3418 1.1254 0.4760 0.034 Uiso 1 1 calc R . . C10 C 0.4142(3) 1.0639(4) 0.4130(2) 0.0282(13) Uani 1 1 d . . . H10 H 0.4462 1.0368 0.4479 0.034 Uiso 1 1 calc R . . C11 C 0.4300(3) 1.0514(4) 0.3452(2) 0.0243(12) Uani 1 1 d . . . H11 H 0.4726 1.0164 0.3346 0.029 Uiso 1 1 calc R . . C12 C 0.3826(3) 1.0910(4) 0.2920(2) 0.0197(12) Uani 1 1 d . . . C13 C 0.2295(2) 0.7547(4) 0.1963(2) 0.0198(11) Uani 1 1 d . . . C14 C 0.2061(2) 0.7619(4) 0.1263(2) 0.0198(11) Uani 1 1 d . . . C15 C 0.1770(2) 0.6634(4) 0.0942(2) 0.0234(12) Uani 1 1 d . . . H15 H 0.1620 0.6669 0.0476 0.028 Uiso 1 1 calc R . . C16 C 0.1697(3) 0.5600(4) 0.1298(3) 0.0315(13) Uani 1 1 d . . . H16 H 0.1506 0.4944 0.1074 0.038 Uiso 1 1 calc R . . C17 C 0.1913(3) 0.5556(4) 0.1995(3) 0.0308(13) Uani 1 1 d . . . H17 H 0.1857 0.4866 0.2238 0.037 Uiso 1 1 calc R . . C18 C 0.2209(3) 0.6508(4) 0.2333(2) 0.0256(12) Uani 1 1 d . . . H18 H 0.2349 0.6466 0.2800 0.031 Uiso 1 1 calc R . . C19 C 0.4008(3) 0.7821(4) 0.0148(2) 0.0192(11) Uani 1 1 d . . . C20 C 0.3354(3) 0.7526(4) -0.0184(2) 0.0283(13) Uani 1 1 d . . . H20 H 0.2947 0.7529 0.0067 0.034 Uiso 1 1 calc R . . C21 C 0.3293(3) 0.7229(4) -0.0875(2) 0.0294(13) Uani 1 1 d . . . H21 H 0.2851 0.7026 -0.1084 0.035 Uiso 1 1 calc R . . C22 C 0.3886(3) 0.7234(4) -0.1248(2) 0.0303(14) Uani 1 1 d . . . H22 H 0.3852 0.7031 -0.1713 0.036 Uiso 1 1 calc R . . C23 C 0.4533(3) 0.7543(4) -0.0932(3) 0.0412(16) Uani 1 1 d . . . H23 H 0.4935 0.7555 -0.1189 0.049 Uiso 1 1 calc R . . C24 C 0.4597(3) 0.7834(4) -0.0243(2) 0.0277(13) Uani 1 1 d . . . H24 H 0.5040 0.8040 -0.0039 0.033 Uiso 1 1 calc R . . C25 C 0.4961(2) 0.8520(4) 0.1285(2) 0.0261(12) Uani 1 1 d . . . H25A H 0.5275 0.7901 0.1166 0.039 Uiso 1 1 calc R . . H25B H 0.5021 0.8670 0.1772 0.039 Uiso 1 1 calc R . . H25C H 0.5073 0.9212 0.1035 0.039 Uiso 1 1 calc R . . C26 C 0.3974(2) 0.6667(4) 0.1453(2) 0.0217(12) Uani 1 1 d . . . C27 C 0.3737(3) 0.5679(4) 0.1094(2) 0.0285(13) Uani 1 1 d . . . H27 H 0.3627 0.5720 0.0621 0.034 Uiso 1 1 calc R . . C28 C 0.3666(3) 0.4629(4) 0.1443(3) 0.0369(15) Uani 1 1 d . . . H28 H 0.3517 0.3968 0.1197 0.044 Uiso 1 1 calc R . . C29 C 0.3813(3) 0.4552(4) 0.2145(3) 0.0306(13) Uani 1 1 d . . . H29 H 0.3751 0.3850 0.2373 0.037 Uiso 1 1 calc R . . C30 C 0.4052(2) 0.5521(4) 0.2506(2) 0.0253(12) Uani 1 1 d . . . H30 H 0.4162 0.5474 0.2979 0.030 Uiso 1 1 calc R . . C31 C 0.4127(2) 0.6563(4) 0.2164(2) 0.0244(12) Uani 1 1 d . . . H31 H 0.4285 0.7215 0.2414 0.029 Uiso 1 1 calc R . . C32 C 0.0910(3) 1.0526(4) 0.2979(2) 0.0214(12) Uani 1 1 d . . . C33 C 0.0303(3) 1.1046(4) 0.3213(2) 0.0272(13) Uani 1 1 d . . . H33 H -0.0059 1.1275 0.2894 0.033 Uiso 1 1 calc R . . C34 C 0.0224(3) 1.1231(4) 0.3907(3) 0.0286(13) Uani 1 1 d . . . H34 H -0.0189 1.1578 0.4052 0.034 Uiso 1 1 calc R . . C35 C 0.0759(3) 1.0901(4) 0.4386(3) 0.0289(14) Uani 1 1 d . . . H35 H 0.0706 1.1021 0.4854 0.035 Uiso 1 1 calc R . . C36 C 0.1375(3) 1.0391(4) 0.4169(2) 0.0304(13) Uani 1 1 d . . . H36 H 0.1740 1.0176 0.4489 0.036 Uiso 1 1 calc R . . C37 C 0.1441(3) 1.0205(4) 0.3470(2) 0.0260(13) Uani 1 1 d . . . H37 H 0.1853 0.9855 0.3326 0.031 Uiso 1 1 calc R . . C38 C 0.0621(3) 0.8716(4) 0.2019(2) 0.0268(13) Uani 1 1 d . . . H38A H 0.0138 0.8757 0.2153 0.040 Uiso 1 1 calc R . . H38B H 0.0887 0.8189 0.2320 0.040 Uiso 1 1 calc R . . H38C H 0.0625 0.8441 0.1552 0.040 Uiso 1 1 calc R . . C39 C 0.0405(3) 1.1089(4) 0.1573(2) 0.0232(12) Uani 1 1 d . . . C40 C -0.0088(3) 1.0649(5) 0.1085(3) 0.0362(14) Uani 1 1 d . . . H40 H -0.0145 0.9847 0.1041 0.043 Uiso 1 1 calc R . . C41 C -0.0502(3) 1.1393(5) 0.0659(3) 0.0483(17) Uani 1 1 d . . . H41 H -0.0823 1.1087 0.0323 0.058 Uiso 1 1 calc R . . C42 C -0.0435(3) 1.2568(5) 0.0735(3) 0.0435(16) Uani 1 1 d . . . H42 H -0.0717 1.3066 0.0456 0.052 Uiso 1 1 calc R . . C43 C 0.0050(3) 1.3020(4) 0.1224(3) 0.0321(14) Uani 1 1 d . . . H43 H 0.0096 1.3822 0.1278 0.039 Uiso 1 1 calc R . . C44 C 0.0465(3) 1.2286(4) 0.1632(2) 0.0271(13) Uani 1 1 d . . . H44 H 0.0797 1.2599 0.1956 0.033 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 0.0227(4) 0.0213(4) 0.0210(4) -0.0010(3) 0.0021(3) -0.0017(3) Ni2 0.0207(4) 0.0211(4) 0.0195(4) -0.0003(3) 0.0015(3) -0.0001(3) Ni3 0.0206(4) 0.0207(4) 0.0190(4) 0.0005(3) 0.0024(3) 0.0003(3) P1 0.0202(8) 0.0224(8) 0.0184(7) -0.0010(6) 0.0008(6) -0.0007(6) P2 0.0215(8) 0.0215(8) 0.0221(8) 0.0002(6) 0.0025(6) 0.0006(6) S1 0.0249(8) 0.0206(7) 0.0239(8) 0.0016(6) 0.0007(6) 0.0008(6) S2 0.0253(8) 0.0255(8) 0.0192(7) -0.0002(5) 0.0026(6) -0.0023(6) S3 0.0224(8) 0.0268(8) 0.0220(8) -0.0013(6) 0.0019(6) -0.0031(6) S4 0.0250(8) 0.0229(7) 0.0227(8) -0.0017(6) 0.0029(6) 0.0004(6) S5 0.0220(8) 0.0207(7) 0.0209(7) 0.0012(5) -0.0004(6) -0.0004(6) S6 0.0241(8) 0.0200(7) 0.0202(7) -0.0005(5) 0.0001(6) -0.0004(6) C1 0.022(3) 0.015(3) 0.024(3) 0.009(2) -0.002(2) -0.002(2) C2 0.023(3) 0.024(3) 0.034(3) 0.008(3) -0.002(3) -0.004(2) C3 0.033(4) 0.031(3) 0.027(3) 0.004(2) -0.006(3) -0.007(3) C4 0.046(4) 0.028(3) 0.022(3) 0.000(3) 0.000(3) -0.006(3) C5 0.030(3) 0.021(3) 0.033(3) 0.004(3) 0.008(3) -0.001(3) C6 0.029(3) 0.018(3) 0.017(3) 0.002(2) 0.001(2) -0.004(2) C7 0.023(3) 0.016(3) 0.025(3) -0.004(2) 0.002(2) -0.007(2) C8 0.026(3) 0.020(3) 0.027(3) -0.002(2) 0.004(3) -0.004(2) C9 0.035(4) 0.027(3) 0.023(3) 0.002(2) 0.005(3) -0.005(3) C10 0.029(3) 0.030(3) 0.025(3) 0.004(2) -0.009(3) -0.006(3) C11 0.022(3) 0.025(3) 0.027(3) -0.001(2) 0.005(2) -0.002(2) C12 0.022(3) 0.018(3) 0.019(3) -0.001(2) -0.005(2) -0.006(2) C13 0.017(3) 0.019(3) 0.023(3) 0.003(2) 0.004(2) 0.001(2) C14 0.013(3) 0.025(3) 0.022(3) -0.002(2) 0.004(2) 0.005(2) C15 0.025(3) 0.027(3) 0.017(3) 0.001(2) -0.011(2) -0.002(2) C16 0.027(3) 0.024(3) 0.043(4) 0.000(3) 0.001(3) -0.006(3) C17 0.034(4) 0.020(3) 0.038(4) 0.010(3) 0.000(3) -0.001(3) C18 0.023(3) 0.027(3) 0.026(3) 0.004(2) -0.001(2) 0.005(2) C19 0.020(3) 0.017(3) 0.020(3) 0.003(2) -0.001(2) 0.002(2) C20 0.027(3) 0.034(3) 0.024(3) -0.004(3) 0.005(3) 0.008(3) C21 0.025(3) 0.038(3) 0.024(3) -0.003(3) -0.007(3) -0.002(3) C22 0.045(4) 0.033(3) 0.013(3) -0.002(2) 0.001(3) -0.009(3) C23 0.053(5) 0.047(4) 0.025(4) -0.005(3) 0.016(3) -0.021(3) C24 0.026(3) 0.033(3) 0.024(3) -0.002(2) 0.006(3) -0.006(3) C25 0.017(3) 0.029(3) 0.032(3) -0.001(2) 0.003(2) 0.002(2) C26 0.017(3) 0.022(3) 0.026(3) -0.007(2) 0.002(2) 0.001(2) C27 0.035(3) 0.032(3) 0.019(3) -0.001(2) -0.002(2) -0.006(3) C28 0.048(4) 0.026(3) 0.035(4) -0.003(3) -0.009(3) -0.005(3) C29 0.028(3) 0.028(3) 0.036(3) 0.009(3) -0.001(3) 0.000(3) C30 0.029(3) 0.027(3) 0.020(3) 0.002(2) 0.001(2) 0.007(3) C31 0.021(3) 0.025(3) 0.027(3) -0.006(2) -0.002(2) 0.003(2) C32 0.027(3) 0.017(3) 0.020(3) 0.005(2) 0.005(2) -0.001(2) C33 0.025(3) 0.029(3) 0.028(3) 0.005(2) 0.003(3) -0.001(3) C34 0.030(3) 0.023(3) 0.033(4) 0.002(2) 0.010(3) 0.001(3) C35 0.037(4) 0.029(3) 0.022(3) -0.003(2) 0.004(3) -0.002(3) C36 0.031(3) 0.031(3) 0.029(3) 0.004(3) 0.002(3) -0.007(3) C37 0.027(3) 0.032(3) 0.020(3) 0.000(2) 0.004(2) 0.001(3) C38 0.024(3) 0.023(3) 0.034(3) 0.002(2) 0.008(3) -0.006(2) C39 0.020(3) 0.025(3) 0.024(3) 0.001(2) 0.003(2) 0.003(2) C40 0.028(3) 0.033(3) 0.046(4) -0.001(3) -0.013(3) -0.005(3) C41 0.048(4) 0.049(4) 0.046(4) 0.002(3) -0.017(3) 0.010(3) C42 0.038(4) 0.054(4) 0.038(4) 0.012(3) -0.006(3) 0.018(3) C43 0.041(4) 0.026(3) 0.031(4) 0.004(3) 0.007(3) 0.011(3) C44 0.033(4) 0.030(3) 0.018(3) -0.002(2) 0.002(3) 0.003(3) _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 S2 2.1731(14) . ? Ni1 S3 2.1742(15) . ? Ni1 S4 2.1748(14) . ? Ni1 S1 2.1753(15) . ? Ni1 Ni2 2.5104(10) . ? Ni1 Ni3 2.5262(9) . ? Ni2 P1 2.2410(14) . ? Ni2 S6 2.2994(14) . ? Ni2 S5 2.3443(15) . ? Ni2 S2 2.4113(14) . ? Ni2 S3 2.4692(14) . ? Ni2 Ni3 2.4729(10) . ? Ni3 P2 2.2250(15) . ? Ni3 S5 2.2917(14) . ? Ni3 S6 2.3066(14) . ? Ni3 S4 2.4411(14) . ? Ni3 S1 2.4732(14) . ? P1 C19 1.802(5) . ? P1 C25 1.811(4) . ? P1 C26 1.819(5) . ? P2 C38 1.815(4) . ? P2 C32 1.818(4) . ? P2 C39 1.822(5) . ? S1 C1 1.753(5) . ? S2 C6 1.750(5) . ? S3 C12 1.757(5) . ? S4 C7 1.765(5) . ? S5 C14 1.746(5) . ? S6 C13 1.758(5) . ? C1 C2 1.399(6) . ? C1 C6 1.409(6) . ? C2 C3 1.382(6) . ? C3 C4 1.366(6) . ? C4 C5 1.384(6) . ? C5 C6 1.402(6) . ? C7 C12 1.390(6) . ? C7 C8 1.400(6) . ? C8 C9 1.390(6) . ? C9 C10 1.376(6) . ? C10 C11 1.373(5) . ? C11 C12 1.397(6) . ? C13 C14 1.404(6) . ? C13 C18 1.406(6) . ? C14 C15 1.387(6) . ? C15 C16 1.384(6) . ? C16 C17 1.388(6) . ? C17 C18 1.373(6) . ? C19 C24 1.378(6) . ? C19 C20 1.395(6) . ? C20 C21 1.381(6) . ? C21 C22 1.364(6) . ? C22 C23 1.374(7) . ? C23 C24 1.377(6) . ? C26 C27 1.389(6) . ? C26 C31 1.395(6) . ? C27 C28 1.391(6) . ? C28 C29 1.376(6) . ? C29 C30 1.374(6) . ? C30 C31 1.378(6) . ? C32 C37 1.386(6) . ? C32 C33 1.388(6) . ? C33 C34 1.380(6) . ? C34 C35 1.379(6) . ? C35 C36 1.384(6) . ? C36 C37 1.386(6) . ? C39 C40 1.380(6) . ? C39 C44 1.382(6) . ? C40 C41 1.391(7) . ? C41 C42 1.362(7) . ? C42 C43 1.377(7) . ? C43 C44 1.366(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 S2 Ni1 S3 84.79(5) . . ? S2 Ni1 S4 166.63(6) . . ? S3 Ni1 S4 92.86(5) . . ? S2 Ni1 S1 92.95(5) . . ? S3 Ni1 S1 164.91(6) . . ? S4 Ni1 S1 85.89(5) . . ? S2 Ni1 Ni2 61.48(4) . . ? S3 Ni1 Ni2 63.14(4) . . ? S4 Ni1 Ni2 105.76(4) . . ? S1 Ni1 Ni2 102.72(4) . . ? S2 Ni1 Ni3 105.65(4) . . ? S3 Ni1 Ni3 103.25(4) . . ? S4 Ni1 Ni3 62.04(4) . . ? S1 Ni1 Ni3 62.96(4) . . ? Ni2 Ni1 Ni3 58.81(3) . . ? P1 Ni2 S6 109.13(5) . . ? P1 Ni2 S5 105.79(5) . . ? S6 Ni2 S5 81.17(5) . . ? P1 Ni2 S2 95.73(5) . . ? S6 Ni2 S2 154.53(5) . . ? S5 Ni2 S2 97.69(5) . . ? P1 Ni2 S3 102.82(5) . . ? S6 Ni2 S3 94.75(5) . . ? S5 Ni2 S3 150.84(5) . . ? S2 Ni2 S3 73.81(5) . . ? P1 Ni2 Ni3 157.59(5) . . ? S6 Ni2 Ni3 57.67(4) . . ? S5 Ni2 Ni3 56.74(4) . . ? S2 Ni2 Ni3 100.32(4) . . ? S3 Ni2 Ni3 96.65(4) . . ? P1 Ni2 Ni1 141.11(5) . . ? S6 Ni2 Ni1 102.61(4) . . ? S5 Ni2 Ni1 100.69(4) . . ? S2 Ni2 Ni1 52.36(3) . . ? S3 Ni2 Ni1 51.77(4) . . ? Ni3 Ni2 Ni1 60.91(2) . . ? P2 Ni3 S5 105.62(5) . . ? P2 Ni3 S6 103.70(5) . . ? S5 Ni3 S6 82.14(5) . . ? P2 Ni3 S4 100.01(5) . . ? S5 Ni3 S4 153.38(5) . . ? S6 Ni3 S4 98.82(5) . . ? P2 Ni3 Ni2 154.99(5) . . ? S5 Ni3 Ni2 58.80(4) . . ? S6 Ni3 Ni2 57.39(4) . . ? S4 Ni3 Ni2 99.17(4) . . ? P2 Ni3 S1 104.91(5) . . ? S5 Ni3 S1 92.16(5) . . ? S6 Ni3 S1 151.32(5) . . ? S4 Ni3 S1 74.18(5) . . ? Ni2 Ni3 S1 95.66(4) . . ? P2 Ni3 Ni1 144.61(5) . . ? S5 Ni3 Ni1 101.70(4) . . ? S6 Ni3 Ni1 101.92(4) . . ? S4 Ni3 Ni1 51.90(3) . . ? Ni2 Ni3 Ni1 60.28(3) . . ? S1 Ni3 Ni1 51.57(4) . . ? C19 P1 C25 105.2(2) . . ? C19 P1 C26 104.4(2) . . ? C25 P1 C26 103.7(2) . . ? C19 P1 Ni2 114.48(16) . . ? C25 P1 Ni2 111.73(15) . . ? C26 P1 Ni2 116.16(15) . . ? C38 P2 C32 101.8(2) . . ? C38 P2 C39 104.6(2) . . ? C32 P2 C39 105.9(2) . . ? C38 P2 Ni3 114.82(15) . . ? C32 P2 Ni3 116.20(17) . . ? C39 P2 Ni3 112.32(16) . . ? C1 S1 Ni1 103.61(17) . . ? C1 S1 Ni3 108.08(15) . . ? Ni1 S1 Ni3 65.47(4) . . ? C6 S2 Ni1 103.66(17) . . ? C6 S2 Ni2 105.46(15) . . ? Ni1 S2 Ni2 66.17(4) . . ? C12 S3 Ni1 103.66(17) . . ? C12 S3 Ni2 110.97(16) . . ? Ni1 S3 Ni2 65.09(4) . . ? C7 S4 Ni1 103.39(16) . . ? C7 S4 Ni3 109.65(15) . . ? Ni1 S4 Ni3 66.07(4) . . ? C14 S5 Ni3 102.20(16) . . ? C14 S5 Ni2 97.47(17) . . ? Ni3 S5 Ni2 64.46(4) . . ? C13 S6 Ni2 98.93(15) . . ? C13 S6 Ni3 100.90(16) . . ? Ni2 S6 Ni3 64.94(4) . . ? C2 C1 C6 118.8(4) . . ? C2 C1 S1 121.5(4) . . ? C6 C1 S1 119.7(4) . . ? C3 C2 C1 120.5(5) . . ? C4 C3 C2 120.4(5) . . ? C3 C4 C5 121.1(5) . . ? C4 C5 C6 119.4(5) . . ? C5 C6 C1 119.8(5) . . ? C5 C6 S2 120.2(4) . . ? C1 C6 S2 120.0(4) . . ? C12 C7 C8 119.9(5) . . ? C12 C7 S4 120.0(4) . . ? C8 C7 S4 120.2(4) . . ? C9 C8 C7 119.9(5) . . ? C10 C9 C8 119.8(5) . . ? C11 C10 C9 120.7(5) . . ? C10 C11 C12 120.6(5) . . ? C7 C12 C11 119.1(4) . . ? C7 C12 S3 120.0(4) . . ? C11 C12 S3 120.8(4) . . ? C14 C13 C18 120.3(4) . . ? C14 C13 S6 117.4(3) . . ? C18 C13 S6 122.3(4) . . ? C15 C14 C13 118.6(4) . . ? C15 C14 S5 123.8(4) . . ? C13 C14 S5 117.6(4) . . ? C16 C15 C14 121.5(5) . . ? C15 C16 C17 119.1(5) . . ? C18 C17 C16 121.4(5) . . ? C17 C18 C13 119.1(5) . . ? C24 C19 C20 117.6(4) . . ? C24 C19 P1 123.7(4) . . ? C20 C19 P1 118.6(4) . . ? C21 C20 C19 121.8(5) . . ? C22 C21 C20 119.4(5) . . ? C21 C22 C23 119.6(5) . . ? C22 C23 C24 121.2(5) . . ? C23 C24 C19 120.3(5) . . ? C27 C26 C31 117.8(4) . . ? C27 C26 P1 124.0(4) . . ? C31 C26 P1 118.1(4) . . ? C26 C27 C28 120.0(5) . . ? C29 C28 C27 121.1(5) . . ? C30 C29 C28 119.5(5) . . ? C29 C30 C31 119.7(5) . . ? C30 C31 C26 121.9(5) . . ? C37 C32 C33 117.4(4) . . ? C37 C32 P2 118.4(4) . . ? C33 C32 P2 124.0(4) . . ? C34 C33 C32 121.7(5) . . ? C35 C34 C33 119.8(5) . . ? C34 C35 C36 120.0(5) . . ? C35 C36 C37 119.2(5) . . ? C32 C37 C36 121.9(5) . . ? C40 C39 C44 117.9(5) . . ? C40 C39 P2 122.3(4) . . ? C44 C39 P2 119.6(4) . . ? C39 C40 C41 120.7(5) . . ? C42 C41 C40 119.9(6) . . ? C41 C42 C43 119.9(5) . . ? C44 C43 C42 119.9(5) . . ? C43 C44 C39 121.6(5) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.877 _refine_diff_density_min -0.602 _refine_diff_density_rms 0.103 #===END data_compound13 _database_code_depnum_ccdc_archive 'CCDC 718389' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 Ni S4' _chemical_formula_weight 577.49 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' 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 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 9.97(17) _cell_length_b 11.228(3) _cell_length_c 11.940(3) _cell_angle_alpha 90.00(9) _cell_angle_beta 94.46(3) _cell_angle_gamma 90.00 _cell_volume 1332(23) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1180 _cell_measurement_theta_min 20.06 _cell_measurement_theta_max 46.17 _exptl_crystal_description 'prismatic block' _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 1.060 _exptl_absorpt_correction_type 'Semi-empirical from equivalents psi-scans correction' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; 'The low C-C bond precision is a result of weak scattering by the crystal' ; _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4832 _diffrn_reflns_av_R_equivalents 0.0840 _diffrn_reflns_av_sigmaI/netI 0.0780 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.01 _diffrn_reflns_theta_max 25.03 _reflns_number_total 2343 _reflns_number_gt 2033 _reflns_threshold_expression >2sigma(I) _computing_data_collection DIF4 _computing_cell_refinement DIF4 _computing_data_reduction REDU4 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXTL' _computing_publication_material 'WinGX v1.10.01' _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^)+(0.0000P)^2^+0.5137P] 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 2343 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0336 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0687 _refine_ls_wR_factor_gt 0.0663 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _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 0.0000 1.0000 0.0000 0.02587(13) Uani 1 2 d S . . S1 S 0.13981(5) 1.10192(6) 0.10755(4) 0.02692(15) Uani 1 1 d . . . S2 S -0.01428(6) 0.86707(7) 0.13308(4) 0.03643(17) Uani 1 1 d . . . C1 C 0.27591(19) 1.0202(2) 0.17512(15) 0.0261(5) Uani 1 1 d . . . C2 C 0.35632(19) 0.9455(2) 0.11492(15) 0.0276(5) Uani 1 1 d . . . C3 C 0.4616(2) 0.8865(2) 0.17439(17) 0.0311(5) Uani 1 1 d . . . H3 H 0.5180 0.8381 0.1357 0.037 Uiso 1 1 calc R . . C4 C 0.4852(2) 0.8981(2) 0.29126(17) 0.0312(5) Uani 1 1 d . . . C5 C 0.4012(2) 0.9709(3) 0.34697(16) 0.0332(5) Uani 1 1 d . . . H5 H 0.4157 0.9780 0.4246 0.040 Uiso 1 1 calc R . . C6 C 0.2962(2) 1.0339(2) 0.29207(16) 0.0293(5) Uani 1 1 d . . . C7 C 0.3310(2) 0.9234(3) -0.00987(16) 0.0346(6) Uani 1 1 d . . . H7A H 0.4019 0.8748 -0.0352 0.052 Uiso 1 1 calc R . . H7B H 0.3286 0.9981 -0.0491 0.052 Uiso 1 1 calc R . . H7C H 0.2464 0.8833 -0.0245 0.052 Uiso 1 1 calc R . . C8 C 0.5995(2) 0.8310(3) 0.35330(19) 0.0417(6) Uani 1 1 d . . . H8A H 0.6819 0.8741 0.3482 0.063 Uiso 1 1 calc R . . H8B H 0.6073 0.7535 0.3203 0.063 Uiso 1 1 calc R . . H8C H 0.5818 0.8226 0.4308 0.063 Uiso 1 1 calc R . . C9 C 0.2108(2) 1.1143(3) 0.35688(17) 0.0413(6) Uani 1 1 d . . . H9A H 0.2299 1.1005 0.4359 0.062 Uiso 1 1 calc R . . H9B H 0.1175 1.0981 0.3365 0.062 Uiso 1 1 calc R . . H9C H 0.2301 1.1958 0.3399 0.062 Uiso 1 1 calc R . . C10 C -0.1509(2) 0.7760(2) 0.08561(17) 0.0312(5) Uani 1 1 d . . . C11 C -0.2178(2) 0.7955(2) -0.02057(17) 0.0293(5) Uani 1 1 d . . . C12 C -0.3282(2) 0.7295(3) -0.05887(19) 0.0354(5) Uani 1 1 d . . . H12 H -0.3705 0.7434 -0.1298 0.042 Uiso 1 1 calc R . . C13 C -0.3754(2) 0.6421(3) 0.0095(2) 0.0424(6) Uani 1 1 d . . . H13 H -0.4518 0.5987 -0.0143 0.051 Uiso 1 1 calc R . . C14 C -0.3088(2) 0.6192(3) 0.1139(2) 0.0436(6) Uani 1 1 d . . . H14 H -0.3402 0.5595 0.1591 0.052 Uiso 1 1 calc R . . C15 C -0.1974(2) 0.6836(3) 0.15074(19) 0.0388(6) Uani 1 1 d . . . H15 H -0.1522 0.6657 0.2198 0.047 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 0.0228(2) 0.0257(3) 0.02797(18) 0.00475(16) -0.00531(13) -0.00341(18) S1 0.0236(2) 0.0261(3) 0.0301(2) 0.0013(2) -0.00365(18) -0.0009(3) S2 0.0370(3) 0.0364(4) 0.0340(3) 0.0113(3) -0.0088(2) -0.0080(3) C1 0.0218(9) 0.0246(13) 0.0306(9) 0.0011(9) -0.0051(7) -0.0042(11) C2 0.0259(10) 0.0243(13) 0.0320(9) -0.0015(9) -0.0016(8) -0.0060(12) C3 0.0267(10) 0.0257(13) 0.0407(11) -0.0016(10) 0.0003(8) -0.0011(12) C4 0.0267(10) 0.0259(14) 0.0393(10) 0.0015(10) -0.0082(8) -0.0033(12) C5 0.0318(10) 0.0358(15) 0.0303(9) -0.0020(10) -0.0076(8) -0.0027(13) C6 0.0277(10) 0.0274(13) 0.0320(9) -0.0009(10) -0.0027(8) -0.0036(12) C7 0.0361(11) 0.0349(15) 0.0322(10) -0.0037(10) -0.0001(9) 0.0025(13) C8 0.0347(11) 0.0411(17) 0.0470(12) 0.0040(12) -0.0106(9) 0.0052(14) C9 0.0432(13) 0.0464(18) 0.0334(10) -0.0065(11) -0.0031(9) 0.0084(15) C10 0.0277(10) 0.0259(14) 0.0401(11) 0.0029(10) 0.0027(8) -0.0004(12) C11 0.0262(10) 0.0210(13) 0.0406(10) -0.0010(10) 0.0018(8) 0.0003(11) C12 0.0287(11) 0.0281(14) 0.0490(12) -0.0059(11) 0.0005(9) -0.0024(12) C13 0.0308(12) 0.0266(15) 0.0704(15) -0.0035(13) 0.0074(11) -0.0026(13) C14 0.0410(13) 0.0234(15) 0.0688(15) 0.0059(12) 0.0202(11) -0.0016(13) C15 0.0376(12) 0.0308(15) 0.0485(12) 0.0094(12) 0.0071(10) 0.0052(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S1 2.150(15) . ? Ni1 S1 2.150(15) 3_575 ? Ni1 S2 2.1927(19) 3_575 ? Ni1 S2 2.1927(19) . ? S1 C11 1.770(7) 3_575 ? S1 C1 1.778(17) . ? S2 C10 1.761(18) . ? C1 C2 1.397(9) . ? C1 C6 1.404(3) . ? C2 C3 1.388(13) . ? C2 C7 1.512(3) . ? C3 C4 1.403(3) . ? C4 C5 1.377(10) . ? C4 C8 1.511(15) . ? C5 C6 1.386(14) . ? C6 C9 1.496(10) . ? C10 C15 1.397(5) . ? C10 C11 1.403(6) . ? C11 C12 1.375(15) . ? C11 S1 1.770(7) 3_575 ? C12 C13 1.382(5) . ? C13 C14 1.389(6) . ? C14 C15 1.369(16) . ? 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 S1 Ni1 S1 180.0 . 3_575 ? S1 Ni1 S2 89.71(12) . 3_575 ? S1 Ni1 S2 90.29(12) 3_575 3_575 ? S1 Ni1 S2 90.29(12) . . ? S1 Ni1 S2 89.71(12) 3_575 . ? S2 Ni1 S2 180.000(18) 3_575 . ? C11 S1 C1 104.3(9) 3_575 . ? C11 S1 Ni1 106.8(4) 3_575 . ? C1 S1 Ni1 115.6(6) . . ? C10 S2 Ni1 104.73(8) . . ? C2 C1 C6 122.3(4) . . ? C2 C1 S1 121.6(5) . . ? C6 C1 S1 116.1(2) . . ? C3 C2 C1 117.7(5) . . ? C3 C2 C7 119.2(2) . . ? C1 C2 C7 123.1(5) . . ? C2 C3 C4 121.7(3) . . ? C5 C4 C3 118.3(5) . . ? C5 C4 C8 121.5(5) . . ? C3 C4 C8 120.2(2) . . ? C4 C5 C6 122.7(5) . . ? C5 C6 C1 117.3(2) . . ? C5 C6 C9 120.2(5) . . ? C1 C6 C9 122.5(4) . . ? C15 C10 C11 117.7(6) . . ? C15 C10 S2 122.3(3) . . ? C11 C10 S2 120.1(4) . . ? C12 C11 C10 121.9(4) . . ? C12 C11 S1 122.1(4) . 3_575 ? C10 C11 S1 115.6(7) . 3_575 ? C11 C12 C13 119.1(3) . . ? C12 C13 C14 120.0(6) . . ? C15 C14 C13 120.6(4) . . ? C14 C15 C10 120.6(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.256 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.053