# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'Tian-Lu Sheng' ; Fujian Institute of Research on the Structure of Matter, The Chinese Academy of Sciences ; 'Chun-Hong Tan' ; Fujian Institute of Research on the Structure of Matter, The Chinese Academy of Sciences ; 'Mei-Liang Jin' ; Fujian Institute of Research on the Structure of Matter, The Chinese Academy of Sciences ; 'Xiao Ma' ; Fujian Institute of Research on the Structure of Matter, The Chinese Academy of Sciences ; 'Qi-Long Zhu' ; Fujian Institute of Research on the Structure of Matter, The Chinese Academy of Sciences ; ; Yi-Hui Huang ; ; Fujian Institute of Research on the Structure of Matter, The Chinese Academy of Sciences ; 'Sheng-Min Hu' ; Fujian Institute of Research on the Structure of Matter, The Chinese Academy of Sciences ; 'Yan-Long Wang' ; Fujian Institute of Research on the Structure of Matter, The Chinese Academy of Sciences ; 'Xin-Tao Wu' ; Fujian Institute of Research on the Structure of Matter, The Chinese Academy of Sciences ; _publ_contact_author_address ; Fujian Institute of Research on the Structure of Matter, The Chinese Academy of Sciences ; _publ_contact_author_email Tsheng@fjirsm.ac.cn _publ_contact_author_fax 86-591-83714946 _publ_contact_author_phone 86-591-83792294 _publ_contact_author_name 'Tian-Lu Sheng' data_a #TrackingRef '- 1.CIF' _database_code_depnum_ccdc_archive 'CCDC 848529' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H60 Ni6 S12' _chemical_formula_weight 1085.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 9.827(12) _cell_length_b 12.125(12) _cell_length_c 12.340(12) _cell_angle_alpha 118.865(18) _cell_angle_beta 92.29(2) _cell_angle_gamma 108.796(12) _cell_volume 1185(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.2527 _cell_measurement_theta_max 27.4623 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 2.880 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6402 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'RIGAKU/MSC(2004), CrystalClear Version 1.3.6' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Saturn724+ (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10046 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0676 _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 -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 27.38 _reflns_number_total 5286 _reflns_number_gt 3245 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0554P)^2^+0.7435P] 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 5286 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1298 _refine_ls_R_factor_gt 0.0749 _refine_ls_wR_factor_ref 0.1716 _refine_ls_wR_factor_gt 0.1420 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 0.10941(10) 0.63872(10) -0.13587(9) 0.0695(3) Uani 1 1 d . . . Ni2 Ni 0.24876(10) 0.76310(10) 0.13448(9) 0.0699(3) Uani 1 1 d . . . Ni3 Ni 0.14060(10) 0.62596(10) 0.27201(8) 0.0701(3) Uani 1 1 d . . . S1 S 0.1509(2) 0.8381(2) 0.03444(19) 0.0792(6) Uani 1 1 d . . . S2 S 0.3287(2) 0.6753(2) -0.0412(2) 0.0764(5) Uani 1 1 d . . . S3 S 0.3603(2) 0.7022(2) 0.2406(2) 0.0835(6) Uani 1 1 d . . . S4 S 0.1391(2) 0.8181(2) 0.29504(19) 0.0783(6) Uani 1 1 d . . . S5 S -0.0743(2) 0.5533(2) 0.31257(19) 0.0808(6) Uani 1 1 d . . . S6 S 0.1253(2) 0.4182(2) 0.21393(18) 0.0767(5) Uani 1 1 d . . . C1 C -0.0188(9) 0.8607(9) 0.0786(8) 0.103(3) Uani 1 1 d . . . H1A H -0.0558 0.8935 0.0319 0.154 Uiso 1 1 calc R . . H1B H 0.0027 0.9258 0.1683 0.154 Uiso 1 1 calc R . . H1C H -0.0919 0.7747 0.0589 0.154 Uiso 1 1 calc R . . C2 C 0.4678(10) 0.8209(9) -0.0406(9) 0.095(3) Uani 1 1 d . . . H2A H 0.4290 0.8923 -0.0176 0.114 Uiso 1 1 calc R . . C3 C 0.6068(11) 0.8776(13) 0.0593(13) 0.167(5) Uani 1 1 d . . . H3A H 0.6801 0.9535 0.0607 0.250 Uiso 1 1 calc R . . H3B H 0.6441 0.8076 0.0391 0.250 Uiso 1 1 calc R . . H3C H 0.5841 0.9078 0.1413 0.250 Uiso 1 1 calc R . . C4 C 0.4965(15) 0.7755(12) -0.1697(12) 0.179(6) Uani 1 1 d . . . H4A H 0.5687 0.8514 -0.1689 0.269 Uiso 1 1 calc R . . H4B H 0.4062 0.7413 -0.2298 0.269 Uiso 1 1 calc R . . H4C H 0.5330 0.7043 -0.1939 0.269 Uiso 1 1 calc R . . C5 C 0.4222(10) 0.5682(10) 0.1419(10) 0.114(3) Uani 1 1 d . . . H5A H 0.4699 0.5466 0.1942 0.171 Uiso 1 1 calc R . . H5B H 0.4909 0.5988 0.0995 0.171 Uiso 1 1 calc R . . H5C H 0.3388 0.4882 0.0797 0.171 Uiso 1 1 calc R . . C6 C 0.2818(10) 0.9617(9) 0.4383(8) 0.100(3) Uani 1 1 d . . . H6A H 0.3696 0.9406 0.4412 0.120 Uiso 1 1 calc R . . C7 C 0.2234(13) 0.9799(11) 0.5551(9) 0.145(4) Uani 1 1 d . . . H7A H 0.2975 1.0547 0.6303 0.218 Uiso 1 1 calc R . . H7B H 0.1994 0.8976 0.5569 0.218 Uiso 1 1 calc R . . H7C H 0.1362 0.9990 0.5522 0.218 Uiso 1 1 calc R . . C8 C 0.3231(13) 1.0903(10) 0.4303(10) 0.142(4) Uani 1 1 d . . . H8A H 0.3978 1.1659 0.5047 0.213 Uiso 1 1 calc R . . H8B H 0.2371 1.1105 0.4255 0.213 Uiso 1 1 calc R . . H8C H 0.3604 1.0750 0.3557 0.213 Uiso 1 1 calc R . . C9 C -0.1943(9) 0.6362(9) 0.3009(9) 0.109(3) Uani 1 1 d . . . H9A H -0.2863 0.6001 0.3197 0.164 Uiso 1 1 calc R . . H9B H -0.2128 0.6193 0.2162 0.164 Uiso 1 1 calc R . . H9C H -0.1472 0.7329 0.3608 0.164 Uiso 1 1 calc R . . C10 C 0.1358(11) 0.4086(10) 0.3588(8) 0.097(3) Uani 1 1 d . . . H10A H 0.0737 0.4513 0.4103 0.116 Uiso 1 1 calc R . . C11 C 0.2944(14) 0.4857(16) 0.4331(12) 0.186(6) Uani 1 1 d . . . H11A H 0.3030 0.4823 0.5091 0.278 Uiso 1 1 calc R . . H11B H 0.3262 0.5793 0.4556 0.278 Uiso 1 1 calc R . . H11C H 0.3553 0.4448 0.3820 0.278 Uiso 1 1 calc R . . C12 C 0.0803(18) 0.2606(13) 0.3191(12) 0.189(6) Uani 1 1 d . . . H12A H 0.0850 0.2539 0.3934 0.284 Uiso 1 1 calc R . . H12B H 0.1407 0.2188 0.2680 0.284 Uiso 1 1 calc R . . H12C H -0.0203 0.2145 0.2704 0.284 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 0.0681(6) 0.0620(6) 0.0685(6) 0.0259(5) 0.0196(5) 0.0269(5) Ni2 0.0597(6) 0.0609(6) 0.0739(6) 0.0250(5) 0.0125(4) 0.0232(5) Ni3 0.0632(6) 0.0683(6) 0.0644(6) 0.0235(5) 0.0147(4) 0.0274(5) S1 0.0836(14) 0.0620(12) 0.0795(13) 0.0260(10) 0.0143(10) 0.0324(11) S2 0.0686(12) 0.0662(12) 0.0860(13) 0.0326(10) 0.0227(10) 0.0278(10) S3 0.0620(12) 0.0932(16) 0.0946(15) 0.0462(12) 0.0182(10) 0.0345(12) S4 0.0699(12) 0.0705(13) 0.0752(13) 0.0226(10) 0.0145(10) 0.0304(11) S5 0.0757(13) 0.0741(13) 0.0739(13) 0.0229(10) 0.0273(10) 0.0321(11) S6 0.0748(12) 0.0778(14) 0.0717(12) 0.0314(10) 0.0192(10) 0.0355(11) C1 0.103(7) 0.099(7) 0.096(6) 0.032(5) 0.021(5) 0.060(6) C2 0.079(6) 0.086(6) 0.109(7) 0.050(5) 0.028(5) 0.018(5) C3 0.076(7) 0.168(13) 0.241(16) 0.126(12) 0.003(8) 0.005(8) C4 0.222(15) 0.128(11) 0.159(12) 0.074(10) 0.103(11) 0.031(10) C5 0.110(7) 0.133(9) 0.161(9) 0.092(8) 0.071(7) 0.090(7) C6 0.098(7) 0.088(7) 0.079(6) 0.022(5) 0.000(5) 0.033(6) C7 0.164(11) 0.123(10) 0.084(7) 0.024(6) 0.019(7) 0.031(8) C8 0.161(11) 0.081(8) 0.125(9) 0.031(7) 0.003(8) 0.018(7) C9 0.084(6) 0.084(6) 0.124(8) 0.022(5) 0.024(5) 0.046(5) C10 0.105(7) 0.107(7) 0.086(6) 0.052(6) 0.021(5) 0.048(6) C11 0.133(11) 0.28(2) 0.135(11) 0.116(12) 0.011(9) 0.071(12) C12 0.30(2) 0.131(12) 0.149(12) 0.089(10) 0.037(12) 0.074(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 S5 2.194(3) 2_565 ? Ni1 S1 2.195(3) . ? Ni1 S6 2.209(3) 2_565 ? Ni1 S2 2.211(3) . ? Ni1 Ni3 2.923(3) 2_565 ? Ni1 Ni2 2.954(3) . ? Ni2 S3 2.192(3) . ? Ni2 S1 2.197(3) . ? Ni2 S4 2.211(3) . ? Ni2 S2 2.213(3) . ? Ni2 Ni3 2.916(2) . ? Ni3 S3 2.189(3) . ? Ni3 S5 2.190(3) . ? Ni3 S6 2.211(3) . ? Ni3 S4 2.211(3) . ? Ni3 Ni1 2.923(3) 2_565 ? S1 C1 1.837(8) . ? S2 C2 1.848(9) . ? S3 C5 1.811(8) . ? S4 C6 1.838(9) . ? S5 C9 1.820(8) . ? S5 Ni1 2.194(3) 2_565 ? S6 C10 1.847(9) . ? S6 Ni1 2.209(3) 2_565 ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C4 1.487(12) . ? C2 C3 1.516(12) . ? C2 H2A 0.9800 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.516(12) . ? C6 C8 1.533(12) . ? C6 H6A 0.9800 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C12 1.503(14) . ? C10 C11 1.505(14) . ? C10 H10A 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? 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 Ni1 S1 176.17(9) 2_565 . ? S5 Ni1 S6 82.02(9) 2_565 2_565 ? S1 Ni1 S6 98.43(9) . 2_565 ? S5 Ni1 S2 97.98(9) 2_565 . ? S1 Ni1 S2 82.24(9) . . ? S6 Ni1 S2 169.86(9) 2_565 . ? S5 Ni1 Ni3 48.14(8) 2_565 2_565 ? S1 Ni1 Ni3 134.60(8) . 2_565 ? S6 Ni1 Ni3 48.63(8) 2_565 2_565 ? S2 Ni1 Ni3 124.64(9) . 2_565 ? S5 Ni1 Ni2 134.71(8) 2_565 . ? S1 Ni1 Ni2 47.77(7) . . ? S6 Ni1 Ni2 125.78(7) 2_565 . ? S2 Ni1 Ni2 48.14(6) . . ? Ni3 Ni1 Ni2 120.55(5) 2_565 . ? S3 Ni2 S1 175.88(9) . . ? S3 Ni2 S4 81.88(11) . . ? S1 Ni2 S4 98.64(11) . . ? S3 Ni2 S2 98.01(11) . . ? S1 Ni2 S2 82.13(11) . . ? S4 Ni2 S2 170.74(9) . . ? S3 Ni2 Ni3 48.23(9) . . ? S1 Ni2 Ni3 134.75(9) . . ? S4 Ni2 Ni3 48.74(8) . . ? S2 Ni2 Ni3 125.00(9) . . ? S3 Ni2 Ni1 134.89(9) . . ? S1 Ni2 Ni1 47.70(8) . . ? S4 Ni2 Ni1 126.53(10) . . ? S2 Ni2 Ni1 48.07(9) . . ? Ni3 Ni2 Ni1 121.03(8) . . ? S3 Ni3 S5 177.32(9) . . ? S3 Ni3 S6 97.96(9) . . ? S5 Ni3 S6 82.08(9) . . ? S3 Ni3 S4 81.94(9) . . ? S5 Ni3 S4 98.49(9) . . ? S6 Ni3 S4 170.12(9) . . ? S3 Ni3 Ni2 48.30(6) . . ? S5 Ni3 Ni2 133.71(7) . . ? S6 Ni3 Ni2 124.56(8) . . ? S4 Ni3 Ni2 48.75(7) . . ? S3 Ni3 Ni1 133.45(8) . 2_565 ? S5 Ni3 Ni1 48.26(7) . 2_565 ? S6 Ni3 Ni1 48.58(9) . 2_565 ? S4 Ni3 Ni1 125.26(10) . 2_565 ? Ni2 Ni3 Ni1 118.42(8) . 2_565 ? C1 S1 Ni1 113.5(3) . . ? C1 S1 Ni2 113.6(3) . . ? Ni1 S1 Ni2 84.52(11) . . ? C2 S2 Ni1 107.9(3) . . ? C2 S2 Ni2 106.6(3) . . ? Ni1 S2 Ni2 83.79(11) . . ? C5 S3 Ni3 113.6(3) . . ? C5 S3 Ni2 113.8(3) . . ? Ni3 S3 Ni2 83.46(10) . . ? C6 S4 Ni3 107.9(3) . . ? C6 S4 Ni2 107.0(3) . . ? Ni3 S4 Ni2 82.51(8) . . ? C9 S5 Ni3 113.5(3) . . ? C9 S5 Ni1 113.6(3) . 2_565 ? Ni3 S5 Ni1 83.60(9) . 2_565 ? C10 S6 Ni1 107.6(3) . 2_565 ? C10 S6 Ni3 107.4(3) . . ? Ni1 S6 Ni3 82.79(7) 2_565 . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 C3 112.1(9) . . ? C4 C2 S2 109.8(7) . . ? C3 C2 S2 108.6(7) . . ? C4 C2 H2A 108.8 . . ? C3 C2 H2A 108.8 . . ? S2 C2 H2A 108.8 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? S3 C5 H5A 109.5 . . ? S3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? S3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C8 112.0(8) . . ? C7 C6 S4 109.1(7) . . ? C8 C6 S4 108.8(7) . . ? C7 C6 H6A 109.0 . . ? C8 C6 H6A 109.0 . . ? S4 C6 H6A 109.0 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? S5 C9 H9A 109.5 . . ? S5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? S5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 111.9(10) . . ? C12 C10 S6 108.4(7) . . ? C11 C10 S6 107.8(8) . . ? C12 C10 H10A 109.6 . . ? C11 C10 H10A 109.6 . . ? S6 C10 H10A 109.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.38 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.307 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.075 # Attachment '- 2.CIF' data_2 #TrackingRef '- 2.CIF' _database_code_depnum_ccdc_archive 'CCDC 848530' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H72 Ni6 S12' _chemical_formula_weight 1169.86 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7339(17) _cell_length_b 11.6999(18) _cell_length_c 11.915(2) _cell_angle_alpha 114.975(5) _cell_angle_beta 109.973(4) _cell_angle_gamma 91.486(2) _cell_volume 1249.2(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.0467 _cell_measurement_theta_max 27.3717 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 2.737 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6238 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'RIGAKU/MSC(2004), CrystalClear Version 1.3.6' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Mercury2 (1x1 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9851 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0683 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.44 _reflns_number_total 5482 _reflns_number_gt 3380 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0426P)^2^+0.9660P] 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 5482 _refine_ls_number_parameters 280 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1108 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.1473 _refine_ls_wR_factor_gt 0.1216 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.65892(8) 0.58680(8) 0.28645(8) 0.0661(3) Uani 1 1 d . . . Ni2 Ni 0.71562(8) 0.74881(7) 0.17516(7) 0.0635(2) Uani 1 1 d . . . Ni3 Ni 0.55269(8) 0.65673(7) -0.11323(7) 0.0631(2) Uani 1 1 d . . . S1 S 0.84875(17) 0.65569(18) 0.28124(18) 0.0782(5) Uani 1 1 d . . . S2 S 0.62954(17) 0.78446(16) 0.32795(17) 0.0710(4) Uani 1 1 d . A . S3 S 0.57866(18) 0.83711(16) 0.06567(16) 0.0724(5) Uani 1 1 d . . . S4 S 0.76817(17) 0.67324(16) -0.00207(16) 0.0700(4) Uani 1 1 d . B . S5 S 0.52901(18) 0.47973(16) -0.29439(17) 0.0756(5) Uani 1 1 d . . . S6 S 0.33071(17) 0.61845(16) -0.20832(17) 0.0736(5) Uani 1 1 d . . . C1 C 0.9091(8) 0.5280(8) 0.1738(8) 0.107(3) Uani 1 1 d . . . H1A H 0.9918 0.5632 0.1754 0.160 Uiso 1 1 calc R . . H1B H 0.8423 0.4883 0.0835 0.160 Uiso 1 1 calc R . . H1C H 0.9252 0.4647 0.2058 0.160 Uiso 1 1 calc R . . C2 C 0.7437(9) 0.9048(7) 0.5012(7) 0.090(2) Uani 1 1 d . . . C3 C 0.884(2) 0.880(2) 0.560(3) 0.156(14) Uani 0.50 1 d P A 1 H3A H 0.9325 0.9482 0.6493 0.234 Uiso 0.50 1 calc PR A 1 H3B H 0.9326 0.8751 0.5047 0.234 Uiso 0.50 1 calc PR A 1 H3C H 0.8755 0.7996 0.5642 0.234 Uiso 0.50 1 calc PR A 1 C4 C 0.661(3) 0.891(3) 0.584(2) 0.135(8) Uani 0.50 1 d P A 1 H4A H 0.7096 0.9497 0.6775 0.203 Uiso 0.50 1 calc PR A 1 H4B H 0.6508 0.8047 0.5720 0.203 Uiso 0.50 1 calc PR A 1 H4C H 0.5740 0.9113 0.5525 0.203 Uiso 0.50 1 calc PR A 1 C5 C 0.748(3) 1.030(2) 0.497(2) 0.117(8) Uani 0.50 1 d P A 1 H5A H 0.8053 1.0977 0.5840 0.175 Uiso 0.50 1 calc PR A 1 H5B H 0.6585 1.0477 0.4723 0.175 Uiso 0.50 1 calc PR A 1 H5C H 0.7837 1.0266 0.4320 0.175 Uiso 0.50 1 calc PR A 1 C3B C 0.794(5) 0.838(3) 0.584(3) 0.26(3) Uani 0.50 1 d P A 2 H3BA H 0.8526 0.8997 0.6736 0.393 Uiso 0.50 1 calc PR A 2 H3BB H 0.8423 0.7756 0.5454 0.393 Uiso 0.50 1 calc PR A 2 H3BC H 0.7182 0.7956 0.5878 0.393 Uiso 0.50 1 calc PR A 2 C4B C 0.658(4) 0.998(4) 0.548(3) 0.233(17) Uani 0.50 1 d P A 2 H4BA H 0.7102 1.0632 0.6381 0.349 Uiso 0.50 1 calc PR A 2 H4BB H 0.5812 0.9528 0.5475 0.349 Uiso 0.50 1 calc PR A 2 H4BC H 0.6275 1.0365 0.4897 0.349 Uiso 0.50 1 calc PR A 2 C5B C 0.854(4) 0.979(3) 0.495(3) 0.204(14) Uani 0.50 1 d P A 2 H5BA H 0.9124 1.0410 0.5838 0.306 Uiso 0.50 1 calc PR A 2 H5BB H 0.8152 1.0220 0.4421 0.306 Uiso 0.50 1 calc PR A 2 H5BC H 0.9050 0.9208 0.4537 0.306 Uiso 0.50 1 calc PR A 2 C6 C 0.4261(7) 0.8596(8) 0.1001(7) 0.099(3) Uani 1 1 d . . . H6A H 0.4444 0.9398 0.1790 0.148 Uiso 1 1 calc R . . H6B H 0.3978 0.7902 0.1146 0.148 Uiso 1 1 calc R . . H6C H 0.3557 0.8607 0.0249 0.148 Uiso 1 1 calc R . . C7 C 0.8764(8) 0.7925(8) -0.0088(8) 0.091(2) Uani 1 1 d D . . C8 C 0.860(4) 0.9244(14) 0.071(4) 0.125(13) Uani 0.50 1 d PD B 1 H8A H 0.9170 0.9857 0.0662 0.187 Uiso 0.50 1 calc PR B 1 H8B H 0.8863 0.9417 0.1630 0.187 Uiso 0.50 1 calc PR B 1 H8C H 0.7677 0.9313 0.0356 0.187 Uiso 0.50 1 calc PR B 1 C8B C 0.842(5) 0.920(2) 0.013(5) 0.18(2) Uani 0.50 1 d PD B 2 H8BA H 0.9090 0.9697 0.0058 0.263 Uiso 0.50 1 calc PR B 2 H8BB H 0.8414 0.9645 0.1017 0.263 Uiso 0.50 1 calc PR B 2 H8BC H 0.7550 0.9092 -0.0526 0.263 Uiso 0.50 1 calc PR B 2 C9 C 1.0211(9) 0.7877(10) 0.0708(11) 0.157(4) Uani 1 1 d . B . H9A H 1.0845 0.8472 0.0710 0.236 Uiso 1 1 calc R . . H9B H 1.0370 0.7022 0.0297 0.236 Uiso 1 1 calc R . . H9C H 1.0321 0.8106 0.1616 0.236 Uiso 1 1 calc R . . C10 C 0.8603(10) 0.7385(10) -0.1543(11) 0.148(4) Uani 1 1 d . B . H10A H 0.9153 0.7972 -0.1637 0.222 Uiso 1 1 calc R . . H10B H 0.7672 0.7269 -0.2101 0.222 Uiso 1 1 calc R . . H10C H 0.8882 0.6571 -0.1814 0.222 Uiso 1 1 calc R . . C11 C 0.6567(7) 0.3869(7) -0.2626(8) 0.098(2) Uani 1 1 d . . . H11A H 0.6419 0.3110 -0.3445 0.146 Uiso 1 1 calc R . . H11B H 0.6512 0.3627 -0.1966 0.146 Uiso 1 1 calc R . . H11C H 0.7446 0.4378 -0.2299 0.146 Uiso 1 1 calc R . . C12 C 0.2758(9) 0.6684(8) -0.3454(9) 0.095(2) Uani 1 1 d . . . C13 C 0.241(4) 0.559(3) -0.475(3) 0.129(13) Uani 0.50 1 d P C 1 H13A H 0.2137 0.5865 -0.5438 0.194 Uiso 0.50 1 calc PR C 1 H13B H 0.1680 0.4975 -0.4910 0.194 Uiso 0.50 1 calc PR C 1 H13C H 0.3182 0.5197 -0.4773 0.194 Uiso 0.50 1 calc PR C 1 C14 C 0.158(5) 0.717(6) -0.338(4) 0.20(3) Uani 0.50 1 d P C 1 H14A H 0.1235 0.7460 -0.4055 0.294 Uiso 0.50 1 calc PR C 1 H14B H 0.1797 0.7883 -0.2509 0.294 Uiso 0.50 1 calc PR C 1 H14C H 0.0906 0.6508 -0.3536 0.294 Uiso 0.50 1 calc PR C 1 C15 C 0.404(5) 0.761(5) -0.315(5) 0.27(4) Uani 0.50 1 d P C 1 H15A H 0.3834 0.7922 -0.3815 0.404 Uiso 0.50 1 calc PR C 1 H15B H 0.4769 0.7160 -0.3187 0.404 Uiso 0.50 1 calc PR C 1 H15C H 0.4302 0.8331 -0.2277 0.404 Uiso 0.50 1 calc PR C 1 C13B C 0.198(6) 0.547(5) -0.480(4) 0.26(3) Uani 0.50 1 d P C 2 H13D H 0.1694 0.5705 -0.5520 0.389 Uiso 0.50 1 calc PR C 2 H13E H 0.1203 0.5089 -0.4765 0.389 Uiso 0.50 1 calc PR C 2 H13F H 0.2562 0.4862 -0.4964 0.389 Uiso 0.50 1 calc PR C 2 C14B C 0.189(7) 0.770(6) -0.302(6) 0.23(3) Uani 0.50 1 d P C 2 H14D H 0.1568 0.8018 -0.3665 0.343 Uiso 0.50 1 calc PR C 2 H14E H 0.2431 0.8403 -0.2154 0.343 Uiso 0.50 1 calc PR C 2 H14F H 0.1132 0.7311 -0.2956 0.343 Uiso 0.50 1 calc PR C 2 C15B C 0.386(4) 0.728(4) -0.365(4) 0.142(13) Uani 0.50 1 d P C 2 H15D H 0.3473 0.7503 -0.4368 0.213 Uiso 0.50 1 calc PR C 2 H15E H 0.4439 0.6684 -0.3869 0.213 Uiso 0.50 1 calc PR C 2 H15F H 0.4381 0.8046 -0.2837 0.213 Uiso 0.50 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0665(5) 0.0680(5) 0.0597(5) 0.0280(4) 0.0215(4) 0.0133(4) Ni2 0.0633(5) 0.0658(5) 0.0582(5) 0.0280(4) 0.0204(4) 0.0139(4) Ni3 0.0692(5) 0.0619(5) 0.0581(5) 0.0271(4) 0.0250(4) 0.0156(4) S1 0.0633(10) 0.0957(13) 0.0826(12) 0.0502(10) 0.0239(9) 0.0217(9) S2 0.0733(11) 0.0729(11) 0.0658(10) 0.0299(9) 0.0283(8) 0.0168(8) S3 0.0834(12) 0.0664(10) 0.0637(10) 0.0272(8) 0.0270(9) 0.0254(8) S4 0.0724(11) 0.0712(10) 0.0679(10) 0.0304(9) 0.0305(8) 0.0193(8) S5 0.0807(12) 0.0729(11) 0.0682(11) 0.0224(9) 0.0366(9) 0.0102(8) S6 0.0710(11) 0.0722(11) 0.0716(11) 0.0301(9) 0.0244(9) 0.0193(8) C1 0.097(6) 0.132(7) 0.144(7) 0.094(6) 0.066(6) 0.066(5) C2 0.109(6) 0.075(5) 0.065(5) 0.019(4) 0.026(4) 0.010(4) C3 0.099(16) 0.091(17) 0.16(2) 0.017(16) -0.031(15) 0.024(12) C4 0.17(2) 0.18(2) 0.086(13) 0.078(15) 0.057(14) 0.042(18) C5 0.13(2) 0.086(13) 0.116(16) 0.046(12) 0.033(14) 0.026(12) C3B 0.34(6) 0.13(2) 0.09(2) 0.007(17) -0.11(3) -0.04(3) C4B 0.25(4) 0.22(4) 0.20(3) 0.03(3) 0.13(3) 0.11(3) C5B 0.27(4) 0.14(3) 0.113(19) 0.019(19) 0.04(3) -0.07(3) C6 0.087(5) 0.121(6) 0.084(5) 0.038(5) 0.037(4) 0.055(5) C7 0.079(5) 0.104(6) 0.080(5) 0.031(5) 0.036(4) 0.004(4) C8 0.14(2) 0.075(14) 0.18(3) 0.057(13) 0.093(18) -0.013(13) C8B 0.27(4) 0.11(2) 0.30(6) 0.12(2) 0.24(4) 0.11(2) C9 0.095(7) 0.164(10) 0.175(11) 0.057(8) 0.041(7) -0.014(6) C10 0.158(10) 0.177(10) 0.151(10) 0.099(8) 0.081(8) 0.006(7) C11 0.080(5) 0.078(5) 0.123(7) 0.030(5) 0.048(5) 0.022(4) C12 0.092(6) 0.095(6) 0.090(6) 0.052(5) 0.012(5) 0.020(5) C13 0.21(3) 0.13(3) 0.068(17) 0.07(2) 0.04(2) 0.06(3) C14 0.17(3) 0.35(8) 0.18(4) 0.21(5) 0.08(3) 0.17(4) C15 0.26(4) 0.25(4) 0.23(5) 0.21(4) -0.10(3) -0.15(3) C13B 0.25(5) 0.17(4) 0.15(3) 0.07(3) -0.13(3) -0.08(3) C14B 0.33(8) 0.18(3) 0.29(5) 0.15(3) 0.19(5) 0.20(4) C15B 0.11(2) 0.23(4) 0.12(2) 0.12(2) 0.027(19) 0.04(2) _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 S5 2.190(2) 2_665 ? Ni1 S6 2.2006(18) 2_665 ? Ni1 S1 2.202(2) . ? Ni1 S2 2.2070(19) . ? Ni1 Ni2 2.8871(12) . ? Ni2 S4 2.1959(19) . ? Ni2 S3 2.1994(18) . ? Ni2 S1 2.1991(18) . ? Ni2 S2 2.2068(19) . ? Ni2 Ni3 2.9491(12) . ? Ni3 S4 2.1930(19) . ? Ni3 S6 2.1985(19) . ? Ni3 S5 2.1989(18) . ? Ni3 S3 2.2000(18) . ? S1 C1 1.815(7) . ? S2 C2 1.863(7) . ? S3 C6 1.819(7) . ? S4 C7 1.838(8) . ? S5 C11 1.808(7) . ? S5 Ni1 2.1898(19) 2_665 ? S6 C12 1.878(8) . ? S6 Ni1 2.2006(18) 2_665 ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C5 1.49(2) . ? C2 C3B 1.48(3) . ? C2 C4B 1.49(2) . ? C2 C5B 1.49(3) . ? C2 C3 1.53(2) . ? C2 C4 1.58(2) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C3B H3BA 0.9600 . ? C3B H3BB 0.9600 . ? C3B H3BC 0.9600 . ? C4B H4BA 0.9600 . ? C4B H4BB 0.9600 . ? C4B H4BC 0.9600 . ? C5B H5BA 0.9600 . ? C5B H5BB 0.9600 . ? C5B H5BC 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8B 1.482(14) . ? C7 C8 1.484(14) . ? C7 C10 1.516(11) . ? C7 C9 1.536(11) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C8B H8BA 0.9600 . ? C8B H8BB 0.9600 . ? C8B H8BC 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C14 1.42(4) . ? C12 C13 1.44(3) . ? C12 C15B 1.49(4) . ? C12 C13B 1.55(5) . ? C12 C14B 1.56(5) . ? C12 C15 1.57(5) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C13B H13D 0.9600 . ? C13B H13E 0.9600 . ? C13B H13F 0.9600 . ? C14B H14D 0.9600 . ? C14B H14E 0.9600 . ? C14B H14F 0.9600 . ? C15B H15D 0.9600 . ? C15B H15E 0.9600 . ? C15B H15F 0.9600 . ? 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 Ni1 S6 83.11(7) 2_665 2_665 ? S5 Ni1 S1 179.24(8) 2_665 . ? S6 Ni1 S1 97.38(8) 2_665 . ? S5 Ni1 S2 96.91(7) 2_665 . ? S6 Ni1 S2 170.07(7) 2_665 . ? S1 Ni1 S2 82.71(7) . . ? S5 Ni1 Ni2 131.17(6) 2_665 . ? S6 Ni1 Ni2 124.22(6) 2_665 . ? S1 Ni1 Ni2 48.96(5) . . ? S2 Ni1 Ni2 49.14(5) . . ? S4 Ni2 S3 83.00(7) . . ? S4 Ni2 S1 96.70(7) . . ? S3 Ni2 S1 178.50(8) . . ? S4 Ni2 S2 167.30(7) . . ? S3 Ni2 S2 97.18(7) . . ? S1 Ni2 S2 82.78(7) . . ? S4 Ni2 Ni1 121.83(6) . . ? S3 Ni2 Ni1 129.95(6) . . ? S1 Ni2 Ni1 49.05(5) . . ? S2 Ni2 Ni1 49.15(5) . . ? S4 Ni2 Ni3 47.74(5) . . ? S3 Ni2 Ni3 47.92(5) . . ? S1 Ni2 Ni3 130.96(6) . . ? S2 Ni2 Ni3 124.21(6) . . ? Ni1 Ni2 Ni3 115.17(3) . . ? S4 Ni3 S6 169.69(8) . . ? S4 Ni3 S5 96.75(7) . . ? S6 Ni3 S5 82.94(7) . . ? S4 Ni3 S3 83.06(7) . . ? S6 Ni3 S3 97.55(7) . . ? S5 Ni3 S3 178.31(8) . . ? S4 Ni3 Ni2 47.83(5) . . ? S6 Ni3 Ni2 126.07(6) . . ? S5 Ni3 Ni2 132.94(6) . . ? S3 Ni3 Ni2 47.90(5) . . ? C1 S1 Ni2 113.1(3) . . ? C1 S1 Ni1 113.0(3) . . ? Ni2 S1 Ni1 81.99(6) . . ? C2 S2 Ni1 111.9(3) . . ? C2 S2 Ni2 114.1(3) . . ? Ni1 S2 Ni2 81.70(6) . . ? C6 S3 Ni2 114.2(3) . . ? C6 S3 Ni3 113.8(3) . . ? Ni2 S3 Ni3 84.19(6) . . ? C7 S4 Ni3 112.2(3) . . ? C7 S4 Ni2 114.4(3) . . ? Ni3 S4 Ni2 84.43(7) . . ? C11 S5 Ni1 112.7(3) . 2_665 ? C11 S5 Ni3 112.7(3) . . ? Ni1 S5 Ni3 86.44(7) 2_665 . ? C12 S6 Ni3 110.4(3) . . ? C12 S6 Ni1 111.9(3) . 2_665 ? Ni3 S6 Ni1 86.19(6) . 2_665 ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C5 C2 C3B 145.9(14) . . ? C5 C2 C4B 57.2(17) . . ? C3B C2 C4B 113(3) . . ? C5 C2 C5B 51.8(16) . . ? C3B C2 C5B 114(2) . . ? C4B C2 C5B 106(2) . . ? C5 C2 C3 112.8(16) . . ? C3B C2 C3 49(2) . . ? C4B C2 C3 137.5(18) . . ? C5B C2 C3 65.7(18) . . ? C5 C2 C4 113.4(15) . . ? C3B C2 C4 61(2) . . ? C4B C2 C4 57.1(18) . . ? C5B C2 C4 149.1(14) . . ? C3 C2 C4 107.2(18) . . ? C5 C2 S2 104.9(10) . . ? C3B C2 S2 109.2(11) . . ? C4B C2 S2 104.4(14) . . ? C5B C2 S2 109.5(11) . . ? C3 C2 S2 117.7(11) . . ? C4 C2 S2 100.4(10) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C2 C3B H3BA 109.5 . . ? C2 C3B H3BB 109.5 . . ? H3BA C3B H3BB 109.5 . . ? C2 C3B H3BC 109.5 . . ? H3BA C3B H3BC 109.5 . . ? H3BB C3B H3BC 109.5 . . ? C2 C4B H4BA 109.5 . . ? C2 C4B H4BB 109.5 . . ? H4BA C4B H4BB 109.5 . . ? C2 C4B H4BC 109.5 . . ? H4BA C4B H4BC 109.5 . . ? H4BB C4B H4BC 109.5 . . ? C2 C5B H5BA 109.5 . . ? C2 C5B H5BB 109.5 . . ? H5BA C5B H5BB 109.5 . . ? C2 C5B H5BC 109.5 . . ? H5BA C5B H5BC 109.5 . . ? H5BB C5B H5BC 109.5 . . ? S3 C6 H6A 109.5 . . ? S3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? S3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8B C7 C8 24(3) . . ? C8B C7 C10 99.7(19) . . ? C8 C7 C10 123.8(18) . . ? C8B C7 C9 118(2) . . ? C8 C7 C9 104.2(17) . . ? C10 C7 C9 106.6(7) . . ? C8B C7 S4 120.6(15) . . ? C8 C7 S4 110.3(12) . . ? C10 C7 S4 105.9(6) . . ? C9 C7 S4 104.3(6) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C8B H8BA 109.5 . . ? C7 C8B H8BB 109.5 . . ? H8BA C8B H8BB 109.5 . . ? C7 C8B H8BC 109.5 . . ? H8BA C8B H8BC 109.5 . . ? H8BB C8B H8BC 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? S5 C11 H11A 109.5 . . ? S5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? S5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C13 109(3) . . ? C14 C12 C15B 125(3) . . ? C13 C12 C15B 90(2) . . ? C14 C12 C13B 94(3) . . ? C13 C12 C13B 17(4) . . ? C15B C12 C13B 106(3) . . ? C14 C12 C14B 22(5) . . ? C13 C12 C14B 128(3) . . ? C15B C12 C14B 108(3) . . ? C13B C12 C14B 115(3) . . ? C14 C12 C15 119(4) . . ? C13 C12 C15 109(3) . . ? C15B C12 C15 19(3) . . ? C13B C12 C15 125(3) . . ? C14B C12 C15 99(4) . . ? C14 C12 S6 104.2(17) . . ? C13 C12 S6 110.8(11) . . ? C15B C12 S6 116.2(14) . . ? C13B C12 S6 108.2(17) . . ? C14B C12 S6 104(2) . . ? C15 C12 S6 104.5(14) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C13B H13D 109.5 . . ? C12 C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? C12 C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? C12 C14B H14D 109.5 . . ? C12 C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C12 C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? C12 C15B H15D 109.5 . . ? C12 C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? C12 C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.436 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.077 # Attachment '- 3.CIF' data_3 #TrackingRef '- 3.CIF' _database_code_depnum_ccdc_archive 'CCDC 848531' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H72 Ni6 S12' _chemical_formula_weight 1169.86 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M P2(1)/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 10.042(8) _cell_length_b 21.578(14) _cell_length_c 12.936(10) _cell_angle_alpha 90.00 _cell_angle_beta 112.96(5) _cell_angle_gamma 90.00 _cell_volume 2581(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.2027 _cell_measurement_theta_max 27.5010 _exptl_crystal_description cuboid _exptl_crystal_colour black _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 2.650 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8160 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'RIGAKU/MSC(2004), CrystalClear Version 1.3.6' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Saturn724+ (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16214 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0526 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4463 _reflns_number_gt 3949 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0492P)^2^+13.9810P] 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 4463 _refine_ls_number_parameters 234 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0890 _refine_ls_R_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.1585 _refine_ls_wR_factor_gt 0.1514 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.097 _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 0.01603(10) -0.36861(4) 0.49747(7) 0.0356(3) Uani 1 1 d . . . Ni2 Ni 0.00366(9) -0.42625(4) 0.29487(7) 0.0354(3) Uani 1 1 d . . . Ni3 Ni 0.01266(10) -0.44056(5) 0.69798(7) 0.0366(3) Uani 1 1 d . . . S1 S 0.1779(2) -0.37109(9) 0.42058(15) 0.0388(4) Uani 1 1 d . . . S2 S -0.1318(2) -0.35346(10) 0.32269(16) 0.0414(5) Uani 1 1 d . . . S3 S 0.13974(19) -0.49853(9) 0.26705(15) 0.0372(4) Uani 1 1 d . . . S4 S -0.1700(2) -0.49057(10) 0.19529(15) 0.0408(5) Uani 1 1 d . . . S5 S -0.1470(2) -0.38079(9) 0.57047(16) 0.0392(4) Uani 1 1 d . . . S6 S 0.1655(2) -0.37497(10) 0.67434(16) 0.0451(5) Uani 1 1 d . . . C1 C 0.2423(14) -0.2985(6) 0.2709(11) 0.100(4) Uani 1 1 d . . . H1A H 0.2265 -0.2602 0.2301 0.150 Uiso 1 1 calc R . . H1B H 0.1959 -0.3317 0.2201 0.150 Uiso 1 1 calc R . . H1C H 0.3442 -0.3065 0.3061 0.150 Uiso 1 1 calc R . . C2 C 0.2592(13) -0.2489(5) 0.4517(9) 0.082(3) Uani 1 1 d . . . H2A H 0.2697 -0.2101 0.4193 0.123 Uiso 1 1 calc R . . H2B H 0.3530 -0.2652 0.4965 0.123 Uiso 1 1 calc R . . H2C H 0.2055 -0.2426 0.4981 0.123 Uiso 1 1 calc R . . C3 C 0.1797(9) -0.2940(4) 0.3596(7) 0.0443(19) Uani 1 1 d . . . H3A H 0.0794 -0.2798 0.3231 0.053 Uiso 1 1 calc R . . C4 C -0.4190(9) -0.3562(5) 0.1769(7) 0.064(3) Uani 1 1 d . . . H4A H -0.5161 -0.3686 0.1639 0.096 Uiso 1 1 calc R . . H4B H -0.3900 -0.3750 0.1217 0.096 Uiso 1 1 calc R . . H4C H -0.4149 -0.3119 0.1716 0.096 Uiso 1 1 calc R . . C5 C -0.3185(8) -0.3768(4) 0.2926(6) 0.0454(19) Uani 1 1 d . . . H5A H -0.3231 -0.4215 0.2979 0.054 Uiso 1 1 calc R . . H5B H -0.3497 -0.3587 0.3481 0.054 Uiso 1 1 calc R . . C6 C -0.2252(16) -0.4398(7) -0.0083(11) 0.118(5) Uani 1 1 d U . . H6A H -0.2302 -0.4439 -0.0836 0.177 Uiso 1 1 calc R . . H6B H -0.1652 -0.4050 0.0273 0.177 Uiso 1 1 calc R . . H6C H -0.3207 -0.4333 -0.0100 0.177 Uiso 1 1 calc R . . C7 C -0.2324(14) -0.5546(6) 0.0003(9) 0.096(4) Uani 1 1 d U . . H7A H -0.2323 -0.5568 -0.0738 0.144 Uiso 1 1 calc R . . H7B H -0.3301 -0.5562 -0.0045 0.144 Uiso 1 1 calc R . . H7C H -0.1790 -0.5890 0.0440 0.144 Uiso 1 1 calc R . . C8 C -0.1640(9) -0.4959(4) 0.0546(6) 0.0426(18) Uani 1 1 d . . . H8A H -0.0620 -0.4976 0.0651 0.051 Uiso 1 1 calc R . . C9 C 0.4219(9) -0.4620(5) 0.3371(8) 0.061(2) Uani 1 1 d . . . H9A H 0.5173 -0.4615 0.3952 0.091 Uiso 1 1 calc R . . H9B H 0.3853 -0.4204 0.3222 0.091 Uiso 1 1 calc R . . H9C H 0.4257 -0.4795 0.2700 0.091 Uiso 1 1 calc R . . C10 C 0.3241(8) -0.5004(4) 0.3740(7) 0.0420(18) Uani 1 1 d . . . H10A H 0.3249 -0.4845 0.4443 0.050 Uiso 1 1 calc R . . H10B H 0.3587 -0.5429 0.3862 0.050 Uiso 1 1 calc R . . C11 C -0.2293(15) -0.3165(6) 0.7178(11) 0.099(4) Uani 1 1 d . . . H11A H -0.2218 -0.2798 0.7617 0.149 Uiso 1 1 calc R . . H11B H -0.1886 -0.3509 0.7670 0.149 Uiso 1 1 calc R . . H11C H -0.3292 -0.3247 0.6728 0.149 Uiso 1 1 calc R . . C12 C -0.2115(13) -0.2559(5) 0.5559(9) 0.080(3) Uani 1 1 d . . . H12A H -0.1983 -0.2166 0.5934 0.120 Uiso 1 1 calc R . . H12B H -0.3129 -0.2634 0.5153 0.120 Uiso 1 1 calc R . . H12C H -0.1637 -0.2555 0.5045 0.120 Uiso 1 1 calc R . . C13 C -0.1476(10) -0.3071(4) 0.6422(7) 0.054(2) Uani 1 1 d . . . H13A H -0.0474 -0.2961 0.6891 0.064 Uiso 1 1 calc R . . C14B C 0.454(2) -0.3937(12) 0.8079(17) 0.082(7) Uani 0.50 1 d P A 1 H14A H 0.5434 -0.4131 0.8152 0.122 Uiso 0.50 1 calc PR A 1 H14B H 0.4252 -0.4087 0.8659 0.122 Uiso 0.50 1 calc PR A 1 H14C H 0.4674 -0.3496 0.8148 0.122 Uiso 0.50 1 calc PR A 1 C15B C 0.3426(8) -0.4085(5) 0.6983(7) 0.060(2) Uani 0.50 1 d P A 1 H15A H 0.3328 -0.4532 0.6911 0.072 Uiso 0.50 1 calc PR A 1 H15B H 0.3735 -0.3938 0.6404 0.072 Uiso 0.50 1 calc PR A 1 C14A C 0.454(2) -0.3556(12) 0.738(4) 0.17(2) Uani 0.50 1 d P A 2 H14D H 0.5484 -0.3716 0.7510 0.257 Uiso 0.50 1 calc PR A 2 H14E H 0.4536 -0.3381 0.8057 0.257 Uiso 0.50 1 calc PR A 2 H14F H 0.4291 -0.3242 0.6806 0.257 Uiso 0.50 1 calc PR A 2 C15A C 0.3426(8) -0.4085(5) 0.6983(7) 0.060(2) Uani 0.50 1 d P A 2 H15C H 0.3664 -0.4406 0.7552 0.072 Uiso 0.50 1 calc PR A 2 H15D H 0.3420 -0.4267 0.6296 0.072 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0337(5) 0.0387(6) 0.0329(5) 0.0008(4) 0.0114(4) -0.0022(4) Ni2 0.0298(5) 0.0446(6) 0.0313(5) 0.0010(4) 0.0115(4) 0.0008(4) Ni3 0.0343(5) 0.0454(6) 0.0298(5) 0.0006(4) 0.0121(4) -0.0052(4) S1 0.0350(10) 0.0415(11) 0.0385(10) 0.0037(8) 0.0129(8) 0.0002(8) S2 0.0317(9) 0.0535(12) 0.0370(10) 0.0050(9) 0.0113(8) 0.0057(8) S3 0.0343(9) 0.0454(11) 0.0353(9) 0.0012(8) 0.0174(8) -0.0001(8) S4 0.0339(10) 0.0560(13) 0.0304(9) 0.0014(8) 0.0104(8) -0.0021(8) S5 0.0383(10) 0.0401(11) 0.0394(10) 0.0012(8) 0.0154(8) -0.0028(8) S6 0.0394(11) 0.0537(13) 0.0371(10) 0.0012(9) 0.0094(9) -0.0111(9) C1 0.128(11) 0.080(9) 0.126(11) 0.010(8) 0.086(10) 0.007(8) C2 0.116(9) 0.051(6) 0.081(7) -0.010(5) 0.040(7) -0.026(6) C3 0.043(4) 0.044(5) 0.052(5) 0.010(4) 0.026(4) -0.004(4) C4 0.033(4) 0.091(7) 0.059(6) 0.008(5) 0.009(4) -0.006(5) C5 0.033(4) 0.060(5) 0.048(4) -0.001(4) 0.020(4) -0.003(4) C6 0.152(9) 0.124(8) 0.089(7) 0.012(6) 0.060(7) 0.033(7) C7 0.123(8) 0.104(7) 0.064(6) -0.013(5) 0.039(6) -0.037(6) C8 0.047(4) 0.052(5) 0.026(3) 0.003(3) 0.011(3) -0.001(4) C9 0.037(5) 0.077(7) 0.069(6) 0.019(5) 0.021(4) 0.007(4) C10 0.036(4) 0.045(5) 0.048(4) 0.009(4) 0.021(4) 0.000(3) C11 0.135(11) 0.078(8) 0.118(10) 0.004(7) 0.086(10) 0.006(8) C12 0.115(9) 0.055(6) 0.083(7) 0.001(5) 0.053(7) 0.011(6) C13 0.064(6) 0.052(5) 0.049(5) -0.010(4) 0.027(4) -0.006(4) C14B 0.042(11) 0.11(2) 0.075(14) 0.029(13) 0.007(10) -0.004(12) C15B 0.033(4) 0.091(7) 0.055(5) 0.017(5) 0.017(4) -0.011(4) C14A 0.036(12) 0.09(2) 0.31(5) 0.08(3) -0.01(2) -0.027(12) C15A 0.033(4) 0.091(7) 0.055(5) 0.017(5) 0.017(4) -0.011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S2 2.192(3) . ? Ni1 S6 2.197(3) . ? Ni1 S5 2.202(3) . ? Ni1 S1 2.212(3) . ? Ni1 Ni2 2.859(2) . ? Ni2 S3 2.194(2) . ? Ni2 S2 2.197(2) . ? Ni2 S4 2.208(2) . ? Ni2 S1 2.214(3) . ? Ni2 Ni3 2.882(2) 3_546 ? Ni3 S3 2.194(2) 3_546 ? Ni3 S6 2.195(2) . ? Ni3 S5 2.212(3) . ? Ni3 S4 2.216(2) 3_546 ? Ni3 Ni2 2.882(2) 3_546 ? S1 C3 1.844(8) . ? S2 C5 1.830(7) . ? S3 C10 1.829(8) . ? S3 Ni3 2.194(2) 3_546 ? S4 C8 1.848(7) . ? S4 Ni3 2.216(2) 3_546 ? S5 C13 1.843(8) . ? S6 C15B 1.831(9) . ? C1 C3 1.511(13) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.504(12) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9800 . ? C4 C5 1.509(11) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C8 1.455(14) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.481(13) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9800 . ? C9 C10 1.499(11) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C13 1.516(13) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.522(12) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9800 . ? C14B C15B 1.46(2) . ? C14B H14A 0.9600 . ? C14B H14B 0.9600 . ? C14B H14C 0.9600 . ? C15B H15A 0.9700 . ? C15B H15B 0.9700 . ? C14A H14D 0.9600 . ? C14A H14E 0.9600 . ? C14A H14F 0.9600 . ? 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 S6 175.00(9) . . ? S2 Ni1 S5 98.19(10) . . ? S6 Ni1 S5 82.31(10) . . ? S2 Ni1 S1 81.99(10) . . ? S6 Ni1 S1 98.24(10) . . ? S5 Ni1 S1 171.70(9) . . ? S2 Ni1 Ni2 49.44(7) . . ? S6 Ni1 Ni2 134.03(8) . . ? S5 Ni1 Ni2 124.58(7) . . ? S1 Ni1 Ni2 49.79(7) . . ? S3 Ni2 S2 179.69(9) . . ? S3 Ni2 S4 81.85(10) . . ? S2 Ni2 S4 98.40(10) . . ? S3 Ni2 S1 97.95(10) . . ? S2 Ni2 S1 81.83(10) . . ? S4 Ni2 S1 169.88(8) . . ? S3 Ni2 Ni1 130.72(7) . . ? S2 Ni2 Ni1 49.26(6) . . ? S4 Ni2 Ni1 123.38(8) . . ? S1 Ni2 Ni1 49.73(7) . . ? S3 Ni2 Ni3 48.94(6) . 3_546 ? S2 Ni2 Ni3 131.36(7) . 3_546 ? S4 Ni2 Ni3 49.46(6) . 3_546 ? S1 Ni2 Ni3 123.43(7) . 3_546 ? Ni1 Ni2 Ni3 112.77(5) . 3_546 ? S3 Ni3 S6 175.39(9) 3_546 . ? S3 Ni3 S5 98.17(10) 3_546 . ? S6 Ni3 S5 82.13(10) . . ? S3 Ni3 S4 81.66(10) 3_546 3_546 ? S6 Ni3 S4 98.73(10) . 3_546 ? S5 Ni3 S4 171.54(8) . 3_546 ? S3 Ni3 Ni2 48.93(6) 3_546 3_546 ? S6 Ni3 Ni2 134.34(8) . 3_546 ? S5 Ni3 Ni2 124.86(7) . 3_546 ? S4 Ni3 Ni2 49.22(7) 3_546 3_546 ? C3 S1 Ni1 107.6(3) . . ? C3 S1 Ni2 107.9(3) . . ? Ni1 S1 Ni2 80.48(9) . . ? C5 S2 Ni1 113.8(3) . . ? C5 S2 Ni2 114.6(3) . . ? Ni1 S2 Ni2 81.30(8) . . ? C10 S3 Ni2 113.8(3) . . ? C10 S3 Ni3 114.3(2) . 3_546 ? Ni2 S3 Ni3 82.12(9) . 3_546 ? C8 S4 Ni2 107.0(3) . . ? C8 S4 Ni3 106.4(3) . 3_546 ? Ni2 S4 Ni3 81.32(9) . 3_546 ? C13 S5 Ni1 105.2(3) . . ? C13 S5 Ni3 105.8(3) . . ? Ni1 S5 Ni3 86.87(9) . . ? C15B S6 Ni3 114.0(3) . . ? C15B S6 Ni1 115.2(3) . . ? Ni3 S6 Ni1 87.39(9) . . ? C3 C1 H1A 109.5 . . ? C3 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C3 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C2 C3 C1 113.2(8) . . ? C2 C3 S1 109.6(6) . . ? C1 C3 S1 110.1(7) . . ? C2 C3 H3A 107.9 . . ? C1 C3 H3A 107.9 . . ? S1 C3 H3A 107.9 . . ? C5 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C5 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C4 C5 S2 111.3(6) . . ? C4 C5 H5A 109.4 . . ? S2 C5 H5A 109.4 . . ? C4 C5 H5B 109.4 . . ? S2 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C8 C6 H6A 109.5 . . ? C8 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C8 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 C7 115.5(9) . . ? C6 C8 S4 109.2(7) . . ? C7 C8 S4 109.5(6) . . ? C6 C8 H8A 107.4 . . ? C7 C8 H8A 107.4 . . ? S4 C8 H8A 107.4 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C9 C10 S3 110.0(5) . . ? C9 C10 H10A 109.7 . . ? S3 C10 H10A 109.7 . . ? C9 C10 H10B 109.7 . . ? S3 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? C13 C11 H11A 109.5 . . ? C13 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C13 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C13 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 C12 113.0(9) . . ? C11 C13 S5 108.6(7) . . ? C12 C13 S5 109.8(6) . . ? C11 C13 H13A 108.4 . . ? C12 C13 H13A 108.4 . . ? S5 C13 H13A 108.4 . . ? C15B C14B H14A 109.5 . . ? C15B C14B H14B 109.5 . . ? H14A C14B H14B 109.5 . . ? C15B C14B H14C 109.5 . . ? H14A C14B H14C 109.5 . . ? H14B C14B H14C 109.5 . . ? C14B C15B S6 113.9(11) . . ? C14B C15B H15A 108.8 . . ? S6 C15B H15A 108.8 . . ? C14B C15B H15B 108.8 . . ? S6 C15B H15B 108.8 . . ? H15A C15B H15B 107.7 . . ? H14D C14A H14E 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.060 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.109 # Attachment '- 4 .CIF' data_x #TrackingRef '- 4 .CIF' _database_code_depnum_ccdc_archive 'CCDC 848532' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H140 Ni10 S20' _chemical_formula_weight 2090.02 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M P21/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 10.110(8) _cell_length_b 26.08(2) _cell_length_c 20.156(14) _cell_angle_alpha 90.00 _cell_angle_beta 117.22(3) _cell_angle_gamma 90.00 _cell_volume 4726(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cuboid _exptl_crystal_colour black _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2200 _exptl_absorpt_coefficient_mu 2.417 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8210 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'RIGAKU/MSC(2004), CrystalClear Version 1.3.6' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28556 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_sigmaI/netI 0.0678 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8023 _reflns_number_gt 4581 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0234P)^2^+15.2725P] 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 8023 _refine_ls_number_parameters 491 _refine_ls_number_restraints 362 _refine_ls_R_factor_all 0.1279 _refine_ls_R_factor_gt 0.0726 _refine_ls_wR_factor_ref 0.1468 _refine_ls_wR_factor_gt 0.1203 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.018 _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 -0.18104(12) 0.33535(4) 0.00841(6) 0.0826(3) Uani 1 1 d . . . Ni2 Ni 0.05134(12) 0.35065(4) 0.17947(6) 0.0820(3) Uani 1 1 d . . . Ni3 Ni 0.27052(12) 0.42940(4) 0.28885(6) 0.0809(3) Uani 1 1 d . B . Ni4 Ni 0.38130(12) 0.53807(4) 0.27886(6) 0.0849(4) Uani 1 1 d . C . Ni5 Ni 0.34292(13) 0.62438(4) 0.16085(6) 0.0851(4) Uani 1 1 d . C . S1 S 0.0453(3) 0.30782(10) 0.08327(14) 0.0976(7) Uani 1 1 d . A . S2 S -0.1910(3) 0.34695(9) 0.11423(14) 0.0904(7) Uani 1 1 d . . . S3 S 0.0526(3) 0.39925(9) 0.26947(13) 0.0868(7) Uani 1 1 d . B . S4 S 0.2935(3) 0.35354(9) 0.24791(14) 0.0907(7) Uani 1 1 d . . . S5 S 0.4832(3) 0.46117(9) 0.30142(14) 0.0913(7) Uani 1 1 d . . . S6 S 0.2453(3) 0.50580(9) 0.32867(13) 0.0855(6) Uani 1 1 d . . . S7 S 0.2736(3) 0.61359(9) 0.24948(15) 0.0978(8) Uani 1 1 d . . . S8 S 0.5169(3) 0.56960(10) 0.22924(15) 0.1009(8) Uani 1 1 d . . . S9 S 0.4016(2) 0.63236(9) 0.06736(13) 0.0870(7) Uani 1 1 d . . . S10 S 0.1702(3) 0.68037(9) 0.09622(14) 0.0926(7) Uani 1 1 d . . . C1 C 0.0295(13) 0.2396(4) 0.0974(7) 0.143(4) Uani 1 1 d D . . C2 C -0.1289(15) 0.2218(10) 0.0648(15) 0.189(9) Uani 0.50 1 d PDU A 1 H2A H -0.1309 0.1857 0.0741 0.283 Uiso 0.50 1 calc PR A 1 H2B H -0.1771 0.2279 0.0120 0.283 Uiso 0.50 1 calc PR A 1 H2C H -0.1798 0.2402 0.0875 0.283 Uiso 0.50 1 calc PR A 1 C3 C 0.112(3) 0.2194(10) 0.1736(8) 0.182(9) Uani 0.50 1 d PDU A 1 H3A H 0.0923 0.1834 0.1737 0.273 Uiso 0.50 1 calc PR A 1 H3B H 0.0811 0.2370 0.2060 0.273 Uiso 0.50 1 calc PR A 1 H3C H 0.2167 0.2247 0.1909 0.273 Uiso 0.50 1 calc PR A 1 C4 C 0.092(3) 0.2141(10) 0.0499(13) 0.191(10) Uani 0.50 1 d PDU A 1 H4A H 0.0866 0.1775 0.0536 0.287 Uiso 0.50 1 calc PR A 1 H4B H 0.1935 0.2242 0.0672 0.287 Uiso 0.50 1 calc PR A 1 H4C H 0.0345 0.2243 -0.0012 0.287 Uiso 0.50 1 calc PR A 1 C2B C -0.030(3) 0.2031(10) 0.0333(11) 0.201(11) Uani 0.50 1 d PDU A 2 H2BA H -0.0321 0.1692 0.0512 0.301 Uiso 0.50 1 calc PR A 2 H2BB H 0.0329 0.2035 0.0092 0.301 Uiso 0.50 1 calc PR A 2 H2BC H -0.1289 0.2132 -0.0017 0.301 Uiso 0.50 1 calc PR A 2 C3B C -0.061(3) 0.2313(11) 0.1390(16) 0.215(10) Uani 0.50 1 d PDU A 2 H3BA H -0.0684 0.1953 0.1465 0.322 Uiso 0.50 1 calc PR A 2 H3BB H -0.1593 0.2452 0.1104 0.322 Uiso 0.50 1 calc PR A 2 H3BC H -0.0140 0.2483 0.1865 0.322 Uiso 0.50 1 calc PR A 2 C4B C 0.1831(17) 0.2209(12) 0.1507(14) 0.204(10) Uani 0.50 1 d PDU A 2 H4BA H 0.1791 0.1850 0.1599 0.306 Uiso 0.50 1 calc PR A 2 H4BB H 0.2186 0.2395 0.1968 0.306 Uiso 0.50 1 calc PR A 2 H4BC H 0.2492 0.2264 0.1291 0.306 Uiso 0.50 1 calc PR A 2 C5 C -0.2721(12) 0.4088(4) 0.1124(6) 0.123(4) Uani 1 1 d . . . H5A H -0.3765 0.4078 0.0764 0.147 Uiso 1 1 calc R . . H5B H -0.2663 0.4153 0.1611 0.147 Uiso 1 1 calc R . . C6 C -0.1995(14) 0.4521(4) 0.0931(6) 0.141(4) Uani 1 1 d . . . H6A H -0.2486 0.4836 0.0930 0.211 Uiso 1 1 calc R . . H6B H -0.2066 0.4464 0.0445 0.211 Uiso 1 1 calc R . . H6C H -0.0967 0.4541 0.1293 0.211 Uiso 1 1 calc R . . C7 C 0.0685(12) 0.3608(4) 0.3475(5) 0.116(3) Uani 1 1 d D . . C8 C -0.057(2) 0.3239(8) 0.3271(15) 0.175(9) Uani 0.50 1 d PDU B 1 H8A H -0.0418 0.3040 0.3701 0.263 Uiso 0.50 1 calc PR B 1 H8B H -0.0622 0.3016 0.2882 0.263 Uiso 0.50 1 calc PR B 1 H8C H -0.1490 0.3426 0.3100 0.263 Uiso 0.50 1 calc PR B 1 C9 C 0.2108(18) 0.3315(8) 0.3839(14) 0.162(8) Uani 0.50 1 d PDU B 1 H9A H 0.2125 0.3116 0.4244 0.243 Uiso 0.50 1 calc PR B 1 H9B H 0.2930 0.3550 0.4028 0.243 Uiso 0.50 1 calc PR B 1 H9C H 0.2185 0.3090 0.3481 0.243 Uiso 0.50 1 calc PR B 1 C10 C 0.067(3) 0.3964(10) 0.4062(13) 0.169(9) Uani 0.50 1 d PDU B 1 H10A H 0.0768 0.3768 0.4485 0.254 Uiso 0.50 1 calc PR B 1 H10B H -0.0252 0.4150 0.3859 0.254 Uiso 0.50 1 calc PR B 1 H10C H 0.1483 0.4201 0.4215 0.254 Uiso 0.50 1 calc PR B 1 C8B C -0.0900(15) 0.3499(10) 0.3318(18) 0.181(9) Uani 0.50 1 d PDU B 2 H8BA H -0.0901 0.3287 0.3706 0.271 Uiso 0.50 1 calc PR B 2 H8BB H -0.1409 0.3326 0.2847 0.271 Uiso 0.50 1 calc PR B 2 H8BC H -0.1397 0.3816 0.3299 0.271 Uiso 0.50 1 calc PR B 2 C9B C 0.143(3) 0.3102(7) 0.3558(16) 0.178(10) Uani 0.50 1 d PDU B 2 H9BA H 0.1437 0.2922 0.3976 0.268 Uiso 0.50 1 calc PR B 2 H9BB H 0.2430 0.3154 0.3639 0.268 Uiso 0.50 1 calc PR B 2 H9BC H 0.0893 0.2904 0.3112 0.268 Uiso 0.50 1 calc PR B 2 C10B C 0.142(3) 0.3881(11) 0.4207(12) 0.170(9) Uani 0.50 1 d PDU B 2 H10D H 0.1489 0.3655 0.4598 0.255 Uiso 0.50 1 calc PR B 2 H10E H 0.0846 0.4177 0.4193 0.255 Uiso 0.50 1 calc PR B 2 H10F H 0.2401 0.3986 0.4301 0.255 Uiso 0.50 1 calc PR B 2 C11 C 0.3894(11) 0.3570(4) 0.1888(6) 0.117(4) Uani 1 1 d . . . H11A H 0.3178 0.3513 0.1372 0.141 Uiso 1 1 calc R . . H11B H 0.4310 0.3910 0.1926 0.141 Uiso 1 1 calc R . . C12 C 0.5050(18) 0.3201(7) 0.2103(10) 0.258(10) Uani 1 1 d . . . H12A H 0.5518 0.3229 0.1784 0.387 Uiso 1 1 calc R . . H12B H 0.4641 0.2863 0.2060 0.387 Uiso 1 1 calc R . . H12C H 0.5774 0.3261 0.2611 0.387 Uiso 1 1 calc R . . C13 C 0.6266(14) 0.4575(5) 0.4001(6) 0.124(4) Uani 1 1 d . . . C14 C 0.6595(19) 0.4019(6) 0.4205(9) 0.245(9) Uani 1 1 d . . . H14A H 0.7333 0.3991 0.4717 0.368 Uiso 1 1 calc R . . H14B H 0.6960 0.3863 0.3890 0.368 Uiso 1 1 calc R . . H14C H 0.5701 0.3848 0.4139 0.368 Uiso 1 1 calc R . . C15 C 0.5886(18) 0.4812(9) 0.4524(8) 0.297(14) Uani 1 1 d . . . H15A H 0.6692 0.4773 0.5017 0.446 Uiso 1 1 calc R . . H15B H 0.5009 0.4653 0.4500 0.446 Uiso 1 1 calc R . . H15C H 0.5700 0.5170 0.4409 0.446 Uiso 1 1 calc R . . C16 C 0.7618(16) 0.4847(8) 0.4041(10) 0.288(12) Uani 1 1 d . . . H16A H 0.8398 0.4840 0.4546 0.432 Uiso 1 1 calc R . . H16B H 0.7367 0.5196 0.3883 0.432 Uiso 1 1 calc R . . H16C H 0.7949 0.4677 0.3721 0.432 Uiso 1 1 calc R . . C17 C 0.0536(10) 0.5287(3) 0.2814(5) 0.099(3) Uani 0.50 1 d PD C 1 H17A H 0.0365 0.5454 0.2351 0.119 Uiso 0.50 1 calc PR C 1 H17B H -0.0134 0.4997 0.2691 0.119 Uiso 0.50 1 calc PR C 1 C18 C 0.019(3) 0.5660(10) 0.3286(15) 0.148(10) Uani 0.50 1 d PDU C 1 H18A H -0.0824 0.5771 0.3016 0.222 Uiso 0.50 1 calc PR C 1 H18B H 0.0840 0.5951 0.3402 0.222 Uiso 0.50 1 calc PR C 1 H18C H 0.0335 0.5494 0.3739 0.222 Uiso 0.50 1 calc PR C 1 C17B C 0.0536(10) 0.5287(3) 0.2814(5) 0.099(3) Uani 0.50 1 d P C 2 H17C H 0.0483 0.5589 0.2522 0.119 Uiso 0.50 1 calc PR C 2 H17D H -0.0093 0.5025 0.2477 0.119 Uiso 0.50 1 calc PR C 2 C18B C -0.002(4) 0.5418(12) 0.3373(16) 0.159(13) Uiso 0.50 1 d PDU C 2 H18D H -0.1031 0.5533 0.3115 0.239 Uiso 0.50 1 calc PR C 2 H18E H 0.0588 0.5684 0.3699 0.239 Uiso 0.50 1 calc PR C 2 H18F H 0.0033 0.5119 0.3662 0.239 Uiso 0.50 1 calc PR C 2 C19 C 0.3789(12) 0.6574(4) 0.3251(6) 0.139(4) Uani 1 1 d DU C . C20 C 0.340(3) 0.7126(6) 0.3081(17) 0.194(9) Uani 0.50 1 d PDU C 1 H20A H 0.4013 0.7329 0.3509 0.291 Uiso 0.50 1 calc PR C 1 H20B H 0.2372 0.7177 0.2959 0.291 Uiso 0.50 1 calc PR C 1 H20C H 0.3560 0.7227 0.2666 0.291 Uiso 0.50 1 calc PR C 1 C21 C 0.336(3) 0.6423(11) 0.3855(11) 0.159(8) Uani 0.50 1 d PDU C 1 H21A H 0.3879 0.6638 0.4285 0.238 Uiso 0.50 1 calc PR C 1 H21B H 0.3623 0.6072 0.3992 0.238 Uiso 0.50 1 calc PR C 1 H21C H 0.2307 0.6466 0.3672 0.238 Uiso 0.50 1 calc PR C 1 C22 C 0.5443(15) 0.6525(10) 0.3603(15) 0.183(9) Uani 0.50 1 d PDU C 1 H22A H 0.5886 0.6775 0.3993 0.275 Uiso 0.50 1 calc PR C 1 H22B H 0.5778 0.6582 0.3234 0.275 Uiso 0.50 1 calc PR C 1 H22C H 0.5728 0.6187 0.3809 0.275 Uiso 0.50 1 calc PR C 1 C20B C 0.271(2) 0.7020(8) 0.2980(16) 0.173(9) Uani 0.50 1 d PDU C 2 H20D H 0.3113 0.7302 0.3321 0.260 Uiso 0.50 1 calc PR C 2 H20E H 0.1779 0.6918 0.2955 0.260 Uiso 0.50 1 calc PR C 2 H20F H 0.2565 0.7123 0.2494 0.260 Uiso 0.50 1 calc PR C 2 C21B C 0.412(3) 0.6470(13) 0.4044(9) 0.189(11) Uani 0.50 1 d PDU C 2 H21D H 0.4709 0.6745 0.4357 0.283 Uiso 0.50 1 calc PR C 2 H21E H 0.4663 0.6154 0.4207 0.283 Uiso 0.50 1 calc PR C 2 H21F H 0.3207 0.6444 0.4078 0.283 Uiso 0.50 1 calc PR C 2 C22B C 0.5195(18) 0.6755(10) 0.3264(13) 0.180(9) Uani 0.50 1 d PDU C 2 H22D H 0.5682 0.6991 0.3670 0.269 Uiso 0.50 1 calc PR C 2 H22E H 0.4977 0.6923 0.2802 0.269 Uiso 0.50 1 calc PR C 2 H22F H 0.5836 0.6467 0.3330 0.269 Uiso 0.50 1 calc PR C 2 C23 C 0.5386(14) 0.5217(4) 0.1686(7) 0.139(4) Uani 1 1 d . C . H23A H 0.5843 0.5378 0.1408 0.166 Uiso 1 1 calc R . . H23B H 0.6053 0.4950 0.1993 0.166 Uiso 1 1 calc R . . C24 C 0.3940(16) 0.4977(4) 0.1146(7) 0.160(5) Uani 1 1 d . . . H24A H 0.4121 0.4731 0.0843 0.239 Uiso 1 1 calc R C . H24B H 0.3281 0.5239 0.0833 0.239 Uiso 1 1 calc R . . H24C H 0.3493 0.4809 0.1417 0.239 Uiso 1 1 calc R . . C25 C 0.5432(12) 0.6849(5) 0.0930(6) 0.110(3) Uani 1 1 d . C . C26 C 0.6881(13) 0.6638(5) 0.1530(6) 0.158(5) Uani 1 1 d . . . H26A H 0.7638 0.6897 0.1676 0.237 Uiso 1 1 calc R C . H26B H 0.7175 0.6345 0.1340 0.237 Uiso 1 1 calc R . . H26C H 0.6751 0.6537 0.1954 0.237 Uiso 1 1 calc R . . C27 C 0.5595(12) 0.6967(5) 0.0229(6) 0.151(5) Uani 1 1 d . . . H27A H 0.6311 0.7236 0.0334 0.226 Uiso 1 1 calc R C . H27B H 0.4653 0.7074 -0.0163 0.226 Uiso 1 1 calc R . . H27C H 0.5924 0.6665 0.0075 0.226 Uiso 1 1 calc R . . C28 C 0.4940(15) 0.7309(5) 0.1200(9) 0.208(8) Uani 1 1 d . . . H28A H 0.5672 0.7575 0.1327 0.312 Uiso 1 1 calc R C . H28B H 0.4824 0.7219 0.1632 0.312 Uiso 1 1 calc R . . H28C H 0.4007 0.7429 0.0813 0.312 Uiso 1 1 calc R . . C29 C -0.0065(11) 0.6578(4) 0.0876(6) 0.118(4) Uani 1 1 d . C . H29A H -0.0051 0.6600 0.1360 0.141 Uiso 1 1 calc R . . H29B H -0.0848 0.6801 0.0537 0.141 Uiso 1 1 calc R . . C30 C -0.0424(12) 0.6032(5) 0.0596(7) 0.143(4) Uani 1 1 d . . . H30A H -0.1370 0.5936 0.0562 0.215 Uiso 1 1 calc R C . H30B H 0.0332 0.5806 0.0935 0.215 Uiso 1 1 calc R . . H30C H -0.0464 0.6008 0.0112 0.215 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 0.0878(8) 0.0750(7) 0.0969(9) -0.0119(6) 0.0526(7) -0.0028(6) Ni2 0.0926(8) 0.0694(7) 0.0923(8) -0.0045(6) 0.0496(7) 0.0051(6) Ni3 0.0881(8) 0.0755(7) 0.0817(8) -0.0029(6) 0.0412(6) 0.0082(6) Ni4 0.0880(8) 0.0844(8) 0.0868(8) -0.0099(6) 0.0438(7) 0.0016(6) Ni5 0.0905(8) 0.0816(7) 0.0976(9) -0.0099(6) 0.0556(7) -0.0032(6) S1 0.1015(18) 0.0918(17) 0.1055(19) -0.0146(14) 0.0525(15) 0.0136(13) S2 0.0924(17) 0.0921(16) 0.0992(18) -0.0093(13) 0.0544(15) -0.0006(13) S3 0.0994(17) 0.0763(14) 0.0961(17) -0.0025(12) 0.0546(14) 0.0031(12) S4 0.0965(17) 0.0815(15) 0.0994(18) -0.0053(13) 0.0494(15) 0.0125(12) S5 0.0842(16) 0.0887(16) 0.1003(18) -0.0083(13) 0.0417(14) 0.0056(12) S6 0.0918(16) 0.0806(14) 0.0883(16) -0.0078(12) 0.0450(13) 0.0051(12) S7 0.123(2) 0.0805(15) 0.116(2) -0.0014(14) 0.0779(18) 0.0082(14) S8 0.0968(18) 0.1130(19) 0.106(2) 0.0042(15) 0.0576(16) 0.0110(15) S9 0.0839(16) 0.0926(16) 0.0990(17) -0.0138(13) 0.0544(14) -0.0065(12) S10 0.1041(18) 0.0840(15) 0.1094(19) -0.0077(13) 0.0659(16) 0.0054(13) C1 0.123(10) 0.106(9) 0.180(13) -0.005(8) 0.051(9) 0.026(7) C2 0.195(11) 0.173(11) 0.192(11) 0.005(8) 0.085(8) -0.004(8) C3 0.191(17) 0.160(15) 0.197(16) 0.027(15) 0.090(14) 0.016(15) C4 0.209(17) 0.135(14) 0.211(16) -0.064(13) 0.079(15) 0.045(15) C2B 0.214(18) 0.142(15) 0.214(17) -0.040(14) 0.071(16) -0.013(16) C3B 0.215(12) 0.198(12) 0.217(12) -0.006(9) 0.086(8) 0.000(9) C4B 0.209(12) 0.192(11) 0.204(12) 0.011(9) 0.088(8) 0.002(9) C5 0.122(9) 0.129(9) 0.117(9) -0.020(7) 0.054(7) 0.045(7) C6 0.201(13) 0.093(8) 0.115(9) -0.008(7) 0.060(9) 0.036(8) C7 0.140(10) 0.101(8) 0.135(10) 0.001(7) 0.087(8) -0.005(7) C8 0.225(17) 0.167(17) 0.163(15) 0.022(14) 0.114(14) -0.068(15) C9 0.213(17) 0.168(16) 0.150(16) 0.048(14) 0.122(13) 0.018(15) C10 0.242(19) 0.165(16) 0.124(14) -0.007(13) 0.103(14) 0.023(16) C8B 0.192(12) 0.180(12) 0.179(11) 0.015(9) 0.092(8) -0.009(9) C9B 0.228(19) 0.137(16) 0.177(17) 0.021(14) 0.099(16) 0.028(16) C10B 0.219(19) 0.190(17) 0.133(15) 0.001(14) 0.108(14) -0.023(16) C11 0.096(7) 0.119(8) 0.158(10) -0.025(7) 0.076(7) -0.001(6) C12 0.27(2) 0.26(2) 0.37(3) 0.107(19) 0.26(2) 0.120(17) C13 0.126(10) 0.121(9) 0.084(8) 0.000(7) 0.012(7) 0.021(7) C14 0.26(2) 0.182(16) 0.187(16) 0.057(13) 0.014(14) 0.057(15) C15 0.198(17) 0.53(4) 0.107(11) -0.083(17) 0.022(11) 0.13(2) C16 0.116(13) 0.34(3) 0.28(2) 0.046(19) -0.016(14) -0.084(15) C17 0.092(7) 0.090(6) 0.125(8) 0.000(6) 0.057(6) 0.020(5) C18 0.121(17) 0.15(2) 0.20(2) -0.035(19) 0.100(15) 0.039(17) C17B 0.092(7) 0.090(6) 0.125(8) 0.000(6) 0.057(6) 0.020(5) C19 0.173(8) 0.120(7) 0.137(8) -0.015(6) 0.082(7) 0.014(6) C20 0.209(12) 0.182(12) 0.189(11) -0.003(8) 0.090(8) -0.013(9) C21 0.241(17) 0.145(14) 0.119(13) -0.037(12) 0.107(13) -0.025(15) C22 0.196(12) 0.177(12) 0.176(12) -0.009(8) 0.084(8) -0.019(8) C20B 0.187(11) 0.171(11) 0.169(11) -0.010(8) 0.088(8) -0.006(8) C21B 0.235(18) 0.169(16) 0.142(15) -0.013(14) 0.069(15) 0.002(16) C22B 0.219(17) 0.168(16) 0.145(15) -0.039(14) 0.078(14) -0.010(15) C23 0.180(12) 0.131(10) 0.157(11) 0.022(8) 0.122(10) 0.069(9) C24 0.234(16) 0.105(9) 0.120(10) -0.010(8) 0.065(11) 0.028(10) C25 0.088(7) 0.136(9) 0.110(8) -0.018(7) 0.048(7) -0.049(7) C26 0.108(9) 0.234(15) 0.124(10) -0.006(10) 0.047(8) -0.047(10) C27 0.113(9) 0.190(13) 0.142(11) 0.005(9) 0.052(8) -0.055(8) C28 0.197(14) 0.134(11) 0.36(2) -0.126(13) 0.183(16) -0.083(10) C29 0.105(8) 0.137(10) 0.149(10) 0.017(8) 0.090(8) 0.018(7) C30 0.117(9) 0.151(11) 0.176(12) 0.012(9) 0.078(9) -0.021(8) _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 S10 2.200(3) 3_565 ? Ni1 S2 2.202(3) . ? Ni1 S1 2.207(3) . ? Ni1 S9 2.213(3) 3_565 ? Ni2 S2 2.189(3) . ? Ni2 S4 2.194(3) . ? Ni2 S3 2.208(3) . ? Ni2 S1 2.214(3) . ? Ni3 S4 2.196(3) . ? Ni3 S3 2.199(3) . ? Ni3 S6 2.206(3) . ? Ni3 S5 2.208(3) . ? Ni4 S8 2.194(3) . ? Ni4 S7 2.197(3) . ? Ni4 S5 2.205(3) . ? Ni4 S6 2.207(3) . ? Ni5 S10 2.190(3) . ? Ni5 S8 2.195(3) . ? Ni5 S7 2.215(3) . ? Ni5 S9 2.229(3) . ? S1 C1 1.819(10) . ? S2 C5 1.801(10) . ? S3 C7 1.810(9) . ? S4 C11 1.850(9) . ? S5 C13 1.852(10) . ? S6 C17 1.825(9) . ? S7 C19 1.810(10) . ? S8 C23 1.830(10) . ? S9 C25 1.875(9) . ? S9 Ni1 2.213(3) 3_565 ? S10 C29 1.812(9) . ? S10 Ni1 2.200(3) 3_565 ? C1 C3 1.469(9) . ? C1 C2 1.500(9) . ? C1 C4B 1.509(10) . ? C1 C2B 1.493(9) . ? C1 C3B 1.516(9) . ? C1 C4 1.521(9) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C2B H2BA 0.9600 . ? C2B H2BB 0.9600 . ? C2B H2BC 0.9600 . ? C3B H3BA 0.9600 . ? C3B H3BB 0.9600 . ? C3B H3BC 0.9600 . ? C4B H4BA 0.9600 . ? C4B H4BB 0.9600 . ? C4B H4BC 0.9600 . ? C5 C6 1.494(13) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C9B 1.488(9) . ? C7 C9 1.492(9) . ? C7 C8 1.494(9) . ? C7 C10B 1.495(9) . ? C7 C10 1.511(9) . ? C7 C8B 1.511(9) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C8B H8BA 0.9600 . ? C8B H8BB 0.9600 . ? C8B H8BC 0.9600 . ? C9B H9BA 0.9600 . ? C9B H9BB 0.9600 . ? C9B H9BC 0.9600 . ? C10B H10D 0.9600 . ? C10B H10E 0.9600 . ? C10B H10F 0.9600 . ? C11 C12 1.420(14) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C15 1.418(15) . ? C13 C14 1.502(16) . ? C13 C16 1.508(17) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.507(9) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C18B H18D 0.9600 . ? C18B H18E 0.9600 . ? C18B H18F 0.9600 . ? C19 C20 1.491(9) . ? C19 C22B 1.487(9) . ? C19 C22 1.494(9) . ? C19 C21B 1.501(9) . ? C19 C21 1.520(9) . ? C19 C20B 1.514(9) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C20B H20D 0.9600 . ? C20B H20E 0.9600 . ? C20B H20F 0.9600 . ? C21B H21D 0.9600 . ? C21B H21E 0.9600 . ? C21B H21F 0.9600 . ? C22B H22D 0.9600 . ? C22B H22E 0.9600 . ? C22B H22F 0.9600 . ? C23 C24 1.503(14) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C28 1.493(14) . ? C25 C26 1.514(14) . ? C25 C27 1.528(13) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.512(13) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? 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 S10 Ni1 S2 177.15(10) 3_565 . ? S10 Ni1 S1 95.96(11) 3_565 . ? S2 Ni1 S1 82.82(11) . . ? S10 Ni1 S9 83.44(11) 3_565 3_565 ? S2 Ni1 S9 97.94(10) . 3_565 ? S1 Ni1 S9 176.33(11) . 3_565 ? S2 Ni2 S4 178.21(11) . . ? S2 Ni2 S3 95.91(10) . . ? S4 Ni2 S3 83.01(10) . . ? S2 Ni2 S1 82.93(10) . . ? S4 Ni2 S1 98.27(10) . . ? S3 Ni2 S1 175.15(11) . . ? S4 Ni3 S3 83.15(10) . . ? S4 Ni3 S6 179.33(11) . . ? S3 Ni3 S6 96.57(10) . . ? S4 Ni3 S5 96.69(10) . . ? S3 Ni3 S5 176.64(11) . . ? S6 Ni3 S5 83.55(10) . . ? S8 Ni4 S7 82.95(11) . . ? S8 Ni4 S5 96.00(11) . . ? S7 Ni4 S5 176.69(11) . . ? S8 Ni4 S6 179.59(11) . . ? S7 Ni4 S6 97.44(10) . . ? S5 Ni4 S6 83.61(10) . . ? S10 Ni5 S8 177.98(11) . . ? S10 Ni5 S7 95.97(11) . . ? S8 Ni5 S7 82.48(11) . . ? S10 Ni5 S9 83.29(10) . . ? S8 Ni5 S9 98.32(11) . . ? S7 Ni5 S9 176.66(11) . . ? C1 S1 Ni1 106.7(4) . . ? C1 S1 Ni2 109.0(4) . . ? Ni1 S1 Ni2 92.24(10) . . ? C5 S2 Ni2 110.3(4) . . ? C5 S2 Ni1 109.0(4) . . ? Ni2 S2 Ni1 93.06(10) . . ? C7 S3 Ni3 111.1(4) . . ? C7 S3 Ni2 111.1(3) . . ? Ni3 S3 Ni2 88.85(9) . . ? C11 S4 Ni2 111.1(4) . . ? C11 S4 Ni3 112.0(3) . . ? Ni2 S4 Ni3 89.31(9) . . ? C13 S5 Ni4 109.3(4) . . ? C13 S5 Ni3 110.3(5) . . ? Ni4 S5 Ni3 88.81(10) . . ? C17 S6 Ni3 112.2(3) . . ? C17 S6 Ni4 111.8(3) . . ? Ni3 S6 Ni4 88.81(9) . . ? C19 S7 Ni4 108.1(4) . . ? C19 S7 Ni5 108.5(4) . . ? Ni4 S7 Ni5 91.76(10) . . ? C23 S8 Ni4 109.9(4) . . ? C23 S8 Ni5 109.3(4) . . ? Ni4 S8 Ni5 92.39(11) . . ? C25 S9 Ni1 108.3(4) . 3_565 ? C25 S9 Ni5 107.5(4) . . ? Ni1 S9 Ni5 92.58(10) 3_565 . ? C29 S10 Ni5 108.8(4) . . ? C29 S10 Ni1 109.1(4) . 3_565 ? Ni5 S10 Ni1 94.01(10) . 3_565 ? C3 C1 C2 109.2(9) . . ? C3 C1 C4B 39.9(11) . . ? C2 C1 C4B 139.1(16) . . ? C3 C1 C2B 119.1(18) . . ? C2 C1 C2B 59.7(10) . . ? C4B C1 C2B 106.5(9) . . ? C3 C1 C3B 64.5(11) . . ? C2 C1 C3B 53.3(10) . . ? C4B C1 C3B 104.3(8) . . ? C2B C1 C3B 106.4(9) . . ? C3 C1 C4 107.5(8) . . ? C2 C1 C4 104.7(8) . . ? C4B C1 C4 73.6(12) . . ? C2B C1 C4 45.0(10) . . ? C3B C1 C4 144.7(15) . . ? C3 C1 S1 117.8(13) . . ? C2 C1 S1 112.8(11) . . ? C4B C1 S1 107.0(13) . . ? C2B C1 S1 121.2(13) . . ? C3B C1 S1 110.2(12) . . ? C4 C1 S1 103.8(12) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C1 C2B H2BA 109.5 . . ? C1 C2B H2BB 109.5 . . ? H2BA C2B H2BB 109.5 . . ? C1 C2B H2BC 109.5 . . ? H2BA C2B H2BC 109.5 . . ? H2BB C2B H2BC 109.5 . . ? C1 C3B H3BA 109.5 . . ? C1 C3B H3BB 109.5 . . ? H3BA C3B H3BB 109.5 . . ? C1 C3B H3BC 109.5 . . ? H3BA C3B H3BC 109.5 . . ? H3BB C3B H3BC 109.5 . . ? C1 C4B H4BA 109.5 . . ? C1 C4B H4BB 109.5 . . ? H4BA C4B H4BB 109.5 . . ? C1 C4B H4BC 109.5 . . ? H4BA C4B H4BC 109.5 . . ? H4BB C4B H4BC 109.5 . . ? C6 C5 S2 114.1(7) . . ? C6 C5 H5A 108.7 . . ? S2 C5 H5A 108.7 . . ? C6 C5 H5B 108.7 . . ? S2 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C9B C7 C9 33.7(13) . . ? C9B C7 C8 77.5(14) . . ? C9 C7 C8 108.3(8) . . ? C9B C7 C10B 108.3(9) . . ? C9 C7 C10B 79.9(14) . . ? C8 C7 C10B 124(2) . . ? C9B C7 C10 130.0(19) . . ? C9 C7 C10 106.4(8) . . ? C8 C7 C10 107.4(8) . . ? C10B C7 C10 27.4(14) . . ? C9B C7 C8B 106.8(9) . . ? C9 C7 C8B 134.3(16) . . ? C8 C7 C8B 30.0(14) . . ? C10B C7 C8B 107.3(9) . . ? C10 C7 C8B 83.7(16) . . ? C9B C7 S3 115.4(13) . . ? C9 C7 S3 113.2(12) . . ? C8 C7 S3 113.1(12) . . ? C10B C7 S3 113.6(14) . . ? C10 C7 S3 108.1(14) . . ? C8B C7 S3 104.9(14) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C8B H8BA 109.5 . . ? C7 C8B H8BB 109.5 . . ? H8BA C8B H8BB 109.5 . . ? C7 C8B H8BC 109.5 . . ? H8BA C8B H8BC 109.5 . . ? H8BB C8B H8BC 109.5 . . ? C7 C9B H9BA 109.5 . . ? C7 C9B H9BB 109.5 . . ? H9BA C9B H9BB 109.5 . . ? C7 C9B H9BC 109.5 . . ? H9BA C9B H9BC 109.5 . . ? H9BB C9B H9BC 109.5 . . ? C7 C10B H10D 109.5 . . ? C7 C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C7 C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? C12 C11 S4 111.8(9) . . ? C12 C11 H11A 109.2 . . ? S4 C11 H11A 109.2 . . ? C12 C11 H11B 109.2 . . ? S4 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 108.5(15) . . ? C15 C13 C16 107.6(14) . . ? C14 C13 C16 110.9(13) . . ? C15 C13 S5 115.5(10) . . ? C14 C13 S5 108.1(9) . . ? C16 C13 S5 106.2(10) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 S6 112.3(12) . . ? C18 C17 H17A 109.1 . . ? S6 C17 H17A 109.1 . . ? C18 C17 H17B 109.1 . . ? S6 C17 H17B 109.1 . . ? H17A C17 H17B 107.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? H18D C18B H18E 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C20 C19 C22B 81.3(14) . . ? C20 C19 C22 108.2(9) . . ? C22B C19 C22 33.4(12) . . ? C20 C19 C21B 109(2) . . ? C22B C19 C21B 106.9(9) . . ? C22 C19 C21B 79.7(14) . . ? C20 C19 C21 106.9(9) . . ? C22B C19 C21 133.5(15) . . ? C22 C19 C21 105.3(8) . . ? C21B C19 C21 26.6(14) . . ? C20 C19 C20B 26.3(14) . . ? C22B C19 C20B 106.6(9) . . ? C22 C19 C20B 134.4(15) . . ? C21B C19 C20B 107.2(9) . . ? C21 C19 C20B 93.7(17) . . ? C20 C19 S7 115.1(14) . . ? C22B C19 S7 113.9(11) . . ? C22 C19 S7 116.5(12) . . ? C21B C19 S7 122.8(14) . . ? C21 C19 S7 103.8(12) . . ? C20B C19 S7 97.7(13) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C20B H20D 109.5 . . ? C19 C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C19 C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? C19 C21B H21D 109.5 . . ? C19 C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C19 C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C19 C22B H22D 109.5 . . ? C19 C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C19 C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? C24 C23 S8 113.2(8) . . ? C24 C23 H23A 108.9 . . ? S8 C23 H23A 108.9 . . ? C24 C23 H23B 108.9 . . ? S8 C23 H23B 108.9 . . ? H23A C23 H23B 107.8 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C28 C25 C26 111.3(11) . . ? C28 C25 C27 111.7(11) . . ? C26 C25 C27 109.7(9) . . ? C28 C25 S9 110.4(7) . . ? C26 C25 S9 107.0(8) . . ? C27 C25 S9 106.5(7) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 S10 113.6(7) . . ? C30 C29 H29A 108.9 . . ? S10 C29 H29A 108.9 . . ? C30 C29 H29B 108.9 . . ? S10 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.385 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.075