Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'E. Bouwman' _publ_contact_author_address ; Leiden Institute of Chemistry Gorleaus Laboratories Leiden University Leiden PO Box 9502 Leiden 2300 RA NETHERLANDS ; _publ_contact_author_email BOUWMAN@CHEM.LEIDENUNIV.NL _publ_section_title ; Hexanuclear [Ni6L12] metallacrown framework consisting of NiS4 square-planar and NiS5 square-pyramidal building blocks ; loop_ _publ_author_name _publ_author_address R.Angamuthu ; Leiden Institute of Chemistry Gorlaeus Laboratories Leiden University P.O. Box 9502 2300 RA Leiden The Netherlands ; H.Kooijman ; Bijvoet Center for Biomolecular Research Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; M.Lutz ; Bijvoet Center for Biomolecular Research Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; A.L.Spek ; Bijvoet Center for Biomolecular Research Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; E.Bouwman ; Leiden Institute of Chemistry Gorlaeus Laboratories Leiden University P.O. Box 9502 2300 RA Leiden The Netherlands ; data_s3628b _database_code_depnum_ccdc_archive 'CCDC 655322' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H96 Cl12 Ni6 S24' _chemical_formula_sum 'C96 H96 Cl12 Ni6 S24' _chemical_formula_weight 2796.95 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' Cl Cl 0.1484 0.1585 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8667(12) _cell_length_b 13.9186(12) _cell_length_c 18.843(2) _cell_angle_alpha 75.996(11) _cell_angle_beta 76.080(11) _cell_angle_gamma 74.991(13) _cell_volume 2863.7(5) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 141538 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.622 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 1.728 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6433 _exptl_absorpt_correction_T_max 0.9663 _exptl_absorpt_process_details 'PLATON (routine MULABS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55395 _diffrn_reflns_av_R_equivalents 0.1398 _diffrn_reflns_av_sigmaI/netI 0.1216 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.25 _reflns_number_total 10355 _reflns_number_gt 6121 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _computing_structure_solution 'DIRDIF-99 (Beurskens et al., 1999)' _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^)+(0.0000P)^2^+6.6552P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 10355 _refine_ls_number_parameters 622 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1311 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1048 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.22844(6) 0.40450(6) 0.07256(4) 0.02399(19) Uani 1 1 d . . . Ni2 Ni 0.18836(6) 0.37631(6) -0.06831(4) 0.0249(2) Uani 1 1 d . . . Ni3 Ni 0.03142(7) 0.53333(6) 0.14374(4) 0.0253(2) Uani 1 1 d . . . Cl11 Cl 0.64595(19) -0.20727(18) 0.38811(12) 0.0789(7) Uani 1 1 d . . . Cl21 Cl 0.55348(19) 0.87857(17) -0.42396(10) 0.0681(6) Uani 1 1 d . . . Cl31 Cl 0.42049(15) -0.24128(13) 0.18403(10) 0.0463(5) Uani 1 1 d . . . Cl41 Cl 0.34629(17) 0.68895(15) -0.61478(10) 0.0606(6) Uani 1 1 d . . . Cl51 Cl 0.07570(17) 0.26300(14) 0.56021(10) 0.0570(5) Uani 1 1 d . . . Cl61 Cl -0.18381(16) -0.02910(15) 0.63892(10) 0.0562(5) Uani 1 1 d . . . S11 S 0.20905(13) 0.27025(11) 0.03826(8) 0.0267(4) Uani 1 1 d . . . S12 S 0.52285(15) 0.03232(13) 0.07957(9) 0.0396(4) Uani 1 1 d . . . S21 S 0.32791(13) 0.43317(11) -0.04303(8) 0.0262(4) Uani 1 1 d . . . S22 S 0.39435(15) 0.73987(12) -0.07907(9) 0.0373(4) Uani 1 1 d . . . S31 S 0.05925(13) 0.31264(11) -0.09869(8) 0.0272(4) Uani 1 1 d . . . S32 S -0.02847(14) 0.07814(12) 0.09377(9) 0.0354(4) Uani 1 1 d . . . S41 S 0.14993(13) 0.49391(11) -0.16692(8) 0.0270(4) Uani 1 1 d . . . S42 S 0.42002(16) 0.52452(16) -0.28452(10) 0.0518(5) Uani 1 1 d . . . S51 S 0.21592(13) 0.55351(11) 0.09993(8) 0.0269(4) Uani 1 1 d . . . S52 S 0.05311(15) 0.60430(13) 0.27427(10) 0.0415(5) Uani 1 1 d . . . S61 S 0.12454(13) 0.37747(11) 0.18570(8) 0.0264(4) Uani 1 1 d . . . S62 S -0.11002(16) 0.16994(14) 0.29912(9) 0.0416(5) Uani 1 1 d . . . C11 C 0.3560(5) 0.1863(4) 0.0232(3) 0.0315(16) Uani 1 1 d . . . H11A H 0.3607 0.1469 -0.0151 0.038 Uiso 1 1 calc R . . H11B H 0.4179 0.2270 0.0052 0.038 Uiso 1 1 calc R . . C12 C 0.3769(5) 0.1147(4) 0.0958(3) 0.0298(15) Uani 1 1 d . . . H12A H 0.3152 0.0738 0.1139 0.036 Uiso 1 1 calc R . . H12B H 0.3725 0.1539 0.1341 0.036 Uiso 1 1 calc R . . C13 C 0.5506(5) -0.0292(5) 0.1692(3) 0.0323(16) Uani 1 1 d . . . C14 C 0.4647(6) -0.0269(4) 0.2341(3) 0.0350(16) Uani 1 1 d . . . H14 H 0.3862 0.0117 0.2327 0.042 Uiso 1 1 calc R . . C15 C 0.4961(6) -0.0823(5) 0.3009(4) 0.0426(18) Uani 1 1 d . . . H15 H 0.4383 -0.0817 0.3456 0.051 Uiso 1 1 calc R . . C16 C 0.6091(6) -0.1378(5) 0.3035(4) 0.0436(18) Uani 1 1 d . . . C17 C 0.6954(7) -0.1392(5) 0.2398(4) 0.049(2) Uani 1 1 d . . . H17 H 0.7742 -0.1764 0.2421 0.059 Uiso 1 1 calc R . . C18 C 0.6653(6) -0.0855(5) 0.1727(4) 0.0422(18) Uani 1 1 d . . . H18 H 0.7236 -0.0871 0.1283 0.051 Uiso 1 1 calc R . . C21 C 0.3156(5) 0.5678(4) -0.0791(3) 0.0288(15) Uani 1 1 d . . . H21A H 0.3188 0.5818 -0.1335 0.035 Uiso 1 1 calc R . . H21B H 0.2382 0.6055 -0.0557 0.035 Uiso 1 1 calc R . . C22 C 0.4163(5) 0.6037(4) -0.0628(3) 0.0296(15) Uani 1 1 d . . . H22A H 0.4918 0.5765 -0.0946 0.036 Uiso 1 1 calc R . . H22B H 0.4238 0.5758 -0.0102 0.036 Uiso 1 1 calc R . . C23 C 0.4382(5) 0.7719(4) -0.1769(4) 0.0316(16) Uani 1 1 d . . . C24 C 0.5544(6) 0.7393(5) -0.2128(4) 0.0352(17) Uani 1 1 d . . . H24 H 0.6102 0.6948 -0.1846 0.042 Uiso 1 1 calc R . . C25 C 0.5900(6) 0.7702(5) -0.2880(4) 0.0427(18) Uani 1 1 d . . . H25 H 0.6688 0.7454 -0.3120 0.051 Uiso 1 1 calc R . . C26 C 0.5103(7) 0.8373(5) -0.3284(4) 0.0410(18) Uani 1 1 d . . . C27 C 0.3949(6) 0.8707(5) -0.2949(4) 0.0448(19) Uani 1 1 d . . . H27 H 0.3401 0.9162 -0.3235 0.054 Uiso 1 1 calc R . . C28 C 0.3593(6) 0.8379(5) -0.2196(4) 0.0410(18) Uani 1 1 d . . . H28 H 0.2794 0.8608 -0.1965 0.049 Uiso 1 1 calc R . . C31 C -0.0281(5) 0.2496(4) -0.0148(3) 0.0288(15) Uani 1 1 d . . . H31A H -0.0343 0.2816 0.0279 0.035 Uiso 1 1 calc R . . H31B H -0.1092 0.2551 -0.0227 0.035 Uiso 1 1 calc R . . C32 C 0.0353(5) 0.1395(4) 0.0003(3) 0.0305(15) Uani 1 1 d . . . H32A H 0.1210 0.1349 -0.0031 0.037 Uiso 1 1 calc R . . H32B H 0.0267 0.1045 -0.0374 0.037 Uiso 1 1 calc R . . C33 C 0.0986(5) -0.0151(4) 0.1180(4) 0.0301(16) Uani 1 1 d . . . C34 C 0.1837(5) -0.0624(5) 0.0651(3) 0.0317(16) Uani 1 1 d . . . H34 H 0.1736 -0.0473 0.0148 0.038 Uiso 1 1 calc R . . C35 C 0.2835(5) -0.1320(5) 0.0859(4) 0.0349(16) Uani 1 1 d . . . H35 H 0.3427 -0.1635 0.0499 0.042 Uiso 1 1 calc R . . C36 C 0.2951(5) -0.1542(5) 0.1588(4) 0.0346(16) Uani 1 1 d . . . C37 C 0.2092(6) -0.1097(5) 0.2125(4) 0.0376(17) Uani 1 1 d . . . H37 H 0.2176 -0.1277 0.2632 0.045 Uiso 1 1 calc R . . C38 C 0.1111(6) -0.0389(5) 0.1917(3) 0.0344(16) Uani 1 1 d . . . H38 H 0.0528 -0.0070 0.2279 0.041 Uiso 1 1 calc R . . C41 C 0.2277(5) 0.4282(5) -0.2434(3) 0.0317(15) Uani 1 1 d . . . H41A H 0.2054 0.3618 -0.2339 0.038 Uiso 1 1 calc R . . H41B H 0.2027 0.4685 -0.2902 0.038 Uiso 1 1 calc R . . C42 C 0.3620(5) 0.4117(5) -0.2528(3) 0.0422(18) Uani 1 1 d . . . H42A H 0.3999 0.3658 -0.2886 0.051 Uiso 1 1 calc R . . H42B H 0.3850 0.3770 -0.2043 0.051 Uiso 1 1 calc R . . C43 C 0.3939(5) 0.5657(5) -0.3765(4) 0.0371(17) Uani 1 1 d . . . C44 C 0.3675(5) 0.5061(5) -0.4172(4) 0.0381(17) Uani 1 1 d . . . H44 H 0.3604 0.4384 -0.3951 0.046 Uiso 1 1 calc R . . C45 C 0.3513(5) 0.5452(5) -0.4899(4) 0.0377(17) Uani 1 1 d . . . H45 H 0.3323 0.5043 -0.5172 0.045 Uiso 1 1 calc R . . C46 C 0.3623(6) 0.6408(6) -0.5222(4) 0.0411(18) Uani 1 1 d . . . C47 C 0.3875(6) 0.7019(5) -0.4830(4) 0.0450(18) Uani 1 1 d . . . H47 H 0.3953 0.7692 -0.5060 0.054 Uiso 1 1 calc R . . C48 C 0.4011(6) 0.6645(6) -0.4101(4) 0.0457(19) Uani 1 1 d . . . H48 H 0.4157 0.7073 -0.3824 0.055 Uiso 1 1 calc R . . C51 C 0.2739(5) 0.5391(5) 0.1847(3) 0.0317(16) Uani 1 1 d . . . H51A H 0.2717 0.4704 0.2149 0.038 Uiso 1 1 calc R . . H51B H 0.3577 0.5462 0.1708 0.038 Uiso 1 1 calc R . . C52 C 0.2013(5) 0.6179(5) 0.2305(4) 0.0382(17) Uani 1 1 d . . . H52A H 0.1968 0.6856 0.1977 0.046 Uiso 1 1 calc R . . H52B H 0.2446 0.6164 0.2697 0.046 Uiso 1 1 calc R . . C53 C 0.0708(6) 0.5070(5) 0.3527(3) 0.0352(16) Uani 1 1 d . . . C54 C 0.1792(6) 0.4497(5) 0.3724(4) 0.0424(18) Uani 1 1 d . . . H54 H 0.2522 0.4625 0.3419 0.051 Uiso 1 1 calc R . . C55 C 0.1797(6) 0.3752(5) 0.4356(4) 0.0413(17) Uani 1 1 d . . . H55 H 0.2531 0.3372 0.4489 0.050 Uiso 1 1 calc R . . C56 C 0.0747(7) 0.3555(5) 0.4794(4) 0.0399(17) Uani 1 1 d . . . C57 C -0.0323(6) 0.4097(5) 0.4612(4) 0.0424(18) Uani 1 1 d . . . H57 H -0.1047 0.3954 0.4917 0.051 Uiso 1 1 calc R . . C58 C -0.0339(6) 0.4847(5) 0.3986(4) 0.0407(18) Uani 1 1 d . . . H58 H -0.1080 0.5222 0.3863 0.049 Uiso 1 1 calc R . . C61 C 0.0369(5) 0.2812(4) 0.2030(3) 0.0288(15) Uani 1 1 d . . . H61A H -0.0231 0.3031 0.1705 0.035 Uiso 1 1 calc R . . H61B H 0.0893 0.2166 0.1916 0.035 Uiso 1 1 calc R . . C62 C -0.0244(5) 0.2660(5) 0.2843(3) 0.0327(16) Uani 1 1 d . . . H62A H -0.0774 0.3303 0.2959 0.039 Uiso 1 1 calc R . . H62B H 0.0352 0.2438 0.3170 0.039 Uiso 1 1 calc R . . C63 C -0.1268(5) 0.1193(5) 0.3955(3) 0.0312(15) Uani 1 1 d . . . C64 C -0.1094(6) 0.1643(5) 0.4489(4) 0.0398(17) Uani 1 1 d . . . H64 H -0.0861 0.2277 0.4342 0.048 Uiso 1 1 calc R . . C65 C -0.1255(6) 0.1182(6) 0.5232(4) 0.0450(19) Uani 1 1 d . . . H65 H -0.1111 0.1489 0.5591 0.054 Uiso 1 1 calc R . . C66 C -0.1623(5) 0.0280(5) 0.5451(4) 0.0365(17) Uani 1 1 d . . . C67 C -0.1809(6) -0.0178(5) 0.4936(4) 0.0420(18) Uani 1 1 d . . . H67 H -0.2068 -0.0800 0.5092 0.050 Uiso 1 1 calc R . . C68 C -0.1617(5) 0.0270(5) 0.4185(4) 0.0394(17) Uani 1 1 d . . . H68 H -0.1725 -0.0058 0.3827 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 0.0257(4) 0.0233(5) 0.0243(5) -0.0054(3) -0.0053(4) -0.0062(4) Ni2 0.0272(5) 0.0235(5) 0.0252(5) -0.0048(3) -0.0063(4) -0.0060(4) Ni3 0.0270(5) 0.0220(5) 0.0275(5) -0.0040(4) -0.0065(4) -0.0059(4) Cl11 0.0742(15) 0.0946(18) 0.0568(14) 0.0122(12) -0.0342(12) -0.0035(13) Cl21 0.0846(16) 0.0886(17) 0.0367(12) 0.0001(11) -0.0053(11) -0.0452(13) Cl31 0.0423(11) 0.0391(11) 0.0572(12) -0.0043(9) -0.0205(9) -0.0027(9) Cl41 0.0644(13) 0.0694(15) 0.0395(12) -0.0044(10) -0.0118(10) -0.0031(11) Cl51 0.0740(14) 0.0477(12) 0.0511(13) -0.0048(10) -0.0214(11) -0.0113(10) Cl61 0.0505(12) 0.0683(14) 0.0352(11) -0.0014(9) -0.0002(9) -0.0028(10) S11 0.0308(9) 0.0245(9) 0.0269(9) -0.0049(7) -0.0088(7) -0.0065(7) S12 0.0425(11) 0.0349(11) 0.0349(11) -0.0056(8) -0.0059(8) 0.0007(9) S21 0.0290(9) 0.0238(9) 0.0267(9) -0.0032(7) -0.0055(7) -0.0086(7) S22 0.0502(11) 0.0303(10) 0.0358(11) -0.0079(8) -0.0067(9) -0.0160(9) S31 0.0287(9) 0.0230(9) 0.0312(10) -0.0038(7) -0.0086(7) -0.0063(7) S32 0.0335(10) 0.0313(10) 0.0370(11) -0.0026(8) -0.0051(8) -0.0045(8) S41 0.0276(9) 0.0248(9) 0.0280(9) -0.0027(7) -0.0054(7) -0.0069(7) S42 0.0417(11) 0.0863(16) 0.0343(11) -0.0162(10) -0.0034(9) -0.0252(11) S51 0.0286(9) 0.0257(9) 0.0290(10) -0.0079(7) -0.0053(7) -0.0080(7) S52 0.0429(11) 0.0438(12) 0.0365(11) -0.0119(9) -0.0063(9) -0.0040(9) S61 0.0278(9) 0.0250(9) 0.0263(9) -0.0036(7) -0.0055(7) -0.0060(7) S62 0.0478(11) 0.0465(12) 0.0341(11) -0.0016(9) -0.0080(9) -0.0217(9) C11 0.032(4) 0.028(4) 0.037(4) -0.010(3) -0.012(3) -0.001(3) C12 0.032(4) 0.024(4) 0.035(4) -0.004(3) -0.009(3) -0.008(3) C13 0.034(4) 0.034(4) 0.033(4) -0.008(3) -0.010(3) -0.010(3) C14 0.043(4) 0.026(4) 0.032(4) 0.001(3) -0.014(4) 0.000(3) C15 0.043(5) 0.045(5) 0.041(5) -0.004(4) -0.007(4) -0.016(4) C16 0.048(5) 0.042(5) 0.041(5) 0.000(4) -0.021(4) -0.006(4) C17 0.046(5) 0.054(5) 0.049(5) -0.013(4) -0.020(4) 0.000(4) C18 0.034(4) 0.038(4) 0.051(5) -0.014(4) 0.000(4) -0.003(3) C21 0.034(4) 0.032(4) 0.023(4) -0.006(3) -0.006(3) -0.010(3) C22 0.030(4) 0.029(4) 0.032(4) -0.004(3) -0.008(3) -0.010(3) C23 0.030(4) 0.023(4) 0.043(4) -0.005(3) -0.009(3) -0.007(3) C24 0.036(4) 0.031(4) 0.043(5) -0.009(3) -0.017(4) -0.004(3) C25 0.048(5) 0.035(4) 0.047(5) -0.015(4) -0.003(4) -0.011(4) C26 0.055(5) 0.042(5) 0.033(4) -0.002(4) -0.004(4) -0.032(4) C27 0.044(5) 0.042(5) 0.051(5) 0.003(4) -0.019(4) -0.016(4) C28 0.035(4) 0.045(5) 0.045(5) -0.006(4) -0.008(4) -0.012(4) C31 0.027(4) 0.027(4) 0.030(4) -0.003(3) -0.005(3) -0.004(3) C32 0.032(4) 0.028(4) 0.033(4) -0.006(3) -0.006(3) -0.008(3) C33 0.035(4) 0.018(4) 0.041(4) -0.002(3) -0.014(3) -0.009(3) C34 0.038(4) 0.038(4) 0.024(4) -0.010(3) -0.004(3) -0.013(3) C35 0.031(4) 0.037(4) 0.038(4) -0.013(3) -0.004(3) -0.006(3) C36 0.034(4) 0.025(4) 0.046(5) -0.001(3) -0.015(4) -0.008(3) C37 0.050(5) 0.030(4) 0.034(4) -0.001(3) -0.011(4) -0.012(4) C38 0.038(4) 0.034(4) 0.033(4) -0.009(3) -0.009(3) -0.005(3) C41 0.034(4) 0.036(4) 0.023(4) -0.005(3) -0.001(3) -0.007(3) C42 0.035(4) 0.058(5) 0.027(4) -0.007(3) -0.009(3) 0.005(4) C43 0.026(4) 0.054(5) 0.033(4) -0.012(4) 0.000(3) -0.013(4) C44 0.030(4) 0.046(5) 0.034(4) -0.007(3) 0.001(3) -0.007(3) C45 0.031(4) 0.043(5) 0.039(5) -0.012(4) -0.002(3) -0.009(3) C46 0.033(4) 0.054(5) 0.034(4) -0.014(4) -0.005(3) -0.003(4) C47 0.039(4) 0.046(5) 0.044(5) -0.002(4) -0.003(4) -0.010(4) C48 0.040(4) 0.055(5) 0.049(5) -0.025(4) -0.005(4) -0.012(4) C51 0.032(4) 0.033(4) 0.036(4) -0.010(3) -0.013(3) -0.007(3) C52 0.043(4) 0.043(4) 0.036(4) -0.014(3) -0.004(3) -0.019(3) C53 0.051(5) 0.032(4) 0.027(4) -0.012(3) -0.007(4) -0.012(4) C54 0.027(4) 0.054(5) 0.047(5) -0.018(4) -0.004(3) -0.005(4) C55 0.044(5) 0.047(5) 0.032(4) -0.011(4) -0.010(4) -0.002(4) C56 0.057(5) 0.034(4) 0.032(4) -0.007(3) -0.014(4) -0.010(4) C57 0.038(4) 0.054(5) 0.042(5) -0.016(4) -0.009(4) -0.014(4) C58 0.039(4) 0.053(5) 0.031(4) -0.012(4) -0.011(4) -0.004(4) C61 0.029(4) 0.027(4) 0.032(4) -0.006(3) -0.006(3) -0.007(3) C62 0.037(4) 0.033(4) 0.028(4) -0.005(3) 0.000(3) -0.015(3) C63 0.031(4) 0.033(4) 0.030(4) -0.001(3) -0.004(3) -0.012(3) C64 0.045(4) 0.036(4) 0.038(5) -0.010(4) 0.000(3) -0.011(3) C65 0.043(4) 0.054(5) 0.037(5) -0.017(4) -0.003(4) -0.007(4) C66 0.030(4) 0.040(5) 0.033(4) -0.002(3) -0.002(3) -0.004(3) C67 0.048(5) 0.033(4) 0.044(5) 0.003(4) -0.010(4) -0.016(4) C68 0.041(4) 0.042(5) 0.037(4) -0.001(4) -0.010(3) -0.017(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 S61 2.1895(17) . ? Ni1 S11 2.2002(16) . ? Ni1 S21 2.2098(17) . ? Ni1 S51 2.2161(16) . ? Ni1 Ni3 2.8220(11) . ? Ni1 Ni2 2.9384(10) . ? Ni2 S31 2.1980(16) . ? Ni2 S21 2.1992(16) . ? Ni2 S11 2.2106(17) . ? Ni2 S41 2.2110(17) . ? Ni3 S31 2.1997(17) 2_565 ? Ni3 S41 2.2035(17) 2_565 ? Ni3 S51 2.2115(17) . ? Ni3 S61 2.2137(17) . ? Cl11 C16 1.743(7) . ? Cl21 C26 1.744(7) . ? Cl31 C36 1.743(6) . ? Cl41 C46 1.749(7) . ? Cl51 C56 1.740(7) . ? Cl61 C66 1.741(7) . ? S11 C11 1.831(6) . ? S12 C13 1.765(6) . ? S12 C12 1.815(6) . ? S21 C21 1.812(6) . ? S22 C23 1.770(7) . ? S22 C22 1.804(6) . ? S31 C31 1.831(6) . ? S31 Ni3 2.1997(17) 2_565 ? S32 C33 1.788(6) . ? S32 C32 1.835(6) . ? S41 C41 1.824(6) . ? S41 Ni3 2.2036(17) 2_565 ? S42 C43 1.765(6) . ? S42 C42 1.790(7) . ? S51 C51 1.834(5) . ? S52 C53 1.759(6) . ? S52 C52 1.791(6) . ? S61 C61 1.825(6) . ? S62 C63 1.765(6) . ? S62 C62 1.812(6) . ? C11 C12 1.517(7) . ? C13 C18 1.392(8) . ? C13 C14 1.392(8) . ? C14 C15 1.388(8) . ? C15 C16 1.368(9) . ? C16 C17 1.378(9) . ? C17 C18 1.381(9) . ? C21 C22 1.527(7) . ? C23 C28 1.388(8) . ? C23 C24 1.393(8) . ? C24 C25 1.372(9) . ? C25 C26 1.375(9) . ? C26 C27 1.373(9) . ? C27 C28 1.378(9) . ? C31 C32 1.513(7) . ? C33 C38 1.384(8) . ? C33 C34 1.391(8) . ? C34 C35 1.393(8) . ? C35 C36 1.366(8) . ? C36 C37 1.387(8) . ? C37 C38 1.384(8) . ? C41 C42 1.523(8) . ? C43 C48 1.383(9) . ? C43 C44 1.389(8) . ? C44 C45 1.387(8) . ? C45 C46 1.348(9) . ? C46 C47 1.379(9) . ? C47 C48 1.379(9) . ? C51 C52 1.518(8) . ? C53 C58 1.393(9) . ? C53 C54 1.407(8) . ? C54 C55 1.377(9) . ? C55 C56 1.372(9) . ? C56 C57 1.374(9) . ? C57 C58 1.373(9) . ? C61 C62 1.519(8) . ? C63 C64 1.385(8) . ? C63 C68 1.389(8) . ? C64 C65 1.382(9) . ? C65 C66 1.372(9) . ? C66 C67 1.368(8) . ? C67 C68 1.391(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S61 Ni1 S11 97.20(6) . . ? S61 Ni1 S21 178.15(6) . . ? S11 Ni1 S21 82.26(6) . . ? S61 Ni1 S51 82.32(6) . . ? S11 Ni1 S51 169.20(6) . . ? S21 Ni1 S51 97.88(6) . . ? S61 Ni1 Ni3 50.52(5) . . ? S11 Ni1 Ni3 121.59(5) . . ? S21 Ni1 Ni3 128.34(5) . . ? S51 Ni1 Ni3 50.33(4) . . ? S61 Ni1 Ni2 130.41(5) . . ? S11 Ni1 Ni2 48.38(4) . . ? S21 Ni1 Ni2 48.05(4) . . ? S51 Ni1 Ni2 124.60(5) . . ? Ni3 Ni1 Ni2 111.76(3) . . ? S31 Ni2 S21 175.78(7) . . ? S31 Ni2 S11 98.14(6) . . ? S21 Ni2 S11 82.26(6) . . ? S31 Ni2 S41 81.88(6) . . ? S21 Ni2 S41 98.23(6) . . ? S11 Ni2 S41 173.07(7) . . ? S31 Ni2 Ni1 134.52(5) . . ? S21 Ni2 Ni1 48.36(5) . . ? S11 Ni2 Ni1 48.07(4) . . ? S41 Ni2 Ni1 127.78(5) . . ? S31 Ni3 S41 82.01(6) 2_565 2_565 ? S31 Ni3 S51 97.50(6) 2_565 . ? S41 Ni3 S51 169.24(7) 2_565 . ? S31 Ni3 S61 178.32(7) 2_565 . ? S41 Ni3 S61 98.31(6) 2_565 . ? S51 Ni3 S61 81.88(6) . . ? S31 Ni3 Ni1 128.70(6) 2_565 . ? S41 Ni3 Ni1 121.99(5) 2_565 . ? S51 Ni3 Ni1 50.48(4) . . ? S61 Ni3 Ni1 49.76(5) . . ? C11 S11 Ni1 108.04(19) . . ? C11 S11 Ni2 107.3(2) . . ? Ni1 S11 Ni2 83.55(6) . . ? C13 S12 C12 105.0(3) . . ? C21 S21 Ni2 111.94(18) . . ? C21 S21 Ni1 111.1(2) . . ? Ni2 S21 Ni1 83.59(6) . . ? C23 S22 C22 102.6(3) . . ? C31 S31 Ni2 110.20(19) . . ? C31 S31 Ni3 113.95(19) . 2_565 ? Ni2 S31 Ni3 89.72(6) . 2_565 ? C33 S32 C32 100.5(3) . . ? C41 S41 Ni3 103.99(19) . 2_565 ? C41 S41 Ni2 102.1(2) . . ? Ni3 S41 Ni2 89.29(6) 2_565 . ? C43 S42 C42 103.1(3) . . ? C51 S51 Ni3 103.1(2) . . ? C51 S51 Ni1 111.4(2) . . ? Ni3 S51 Ni1 79.19(6) . . ? C53 S52 C52 104.5(3) . . ? C61 S61 Ni1 114.52(19) . . ? C61 S61 Ni3 114.5(2) . . ? Ni1 S61 Ni3 79.72(6) . . ? C63 S62 C62 104.7(3) . . ? C12 C11 S11 109.4(4) . . ? C11 C12 S12 108.6(4) . . ? C18 C13 C14 119.7(6) . . ? C18 C13 S12 116.2(5) . . ? C14 C13 S12 124.0(5) . . ? C15 C14 C13 118.6(6) . . ? C16 C15 C14 121.1(7) . . ? C15 C16 C17 120.9(6) . . ? C15 C16 Cl11 120.1(6) . . ? C17 C16 Cl11 119.0(5) . . ? C16 C17 C18 118.8(6) . . ? C17 C18 C13 120.9(7) . . ? C22 C21 S21 110.4(4) . . ? C21 C22 S22 113.3(4) . . ? C28 C23 C24 117.8(6) . . ? C28 C23 S22 120.3(5) . . ? C24 C23 S22 121.7(5) . . ? C25 C24 C23 121.4(6) . . ? C24 C25 C26 119.3(7) . . ? C27 C26 C25 120.9(7) . . ? C27 C26 Cl21 118.9(6) . . ? C25 C26 Cl21 120.2(6) . . ? C26 C27 C28 119.4(6) . . ? C27 C28 C23 121.2(7) . . ? C32 C31 S31 107.3(4) . . ? C31 C32 S32 109.6(4) . . ? C38 C33 C34 120.2(6) . . ? C38 C33 S32 117.9(5) . . ? C34 C33 S32 121.9(5) . . ? C33 C34 C35 120.0(6) . . ? C36 C35 C34 119.1(6) . . ? C35 C36 C37 121.5(6) . . ? C35 C36 Cl31 118.6(5) . . ? C37 C36 Cl31 120.0(5) . . ? C38 C37 C36 119.6(6) . . ? C37 C38 C33 119.6(6) . . ? C42 C41 S41 111.8(4) . . ? C41 C42 S42 115.1(4) . . ? C48 C43 C44 118.3(6) . . ? C48 C43 S42 116.9(5) . . ? C44 C43 S42 124.8(6) . . ? C45 C44 C43 120.2(6) . . ? C46 C45 C44 120.5(6) . . ? C45 C46 C47 120.6(6) . . ? C45 C46 Cl41 120.5(5) . . ? C47 C46 Cl41 118.8(6) . . ? C46 C47 C48 119.3(7) . . ? C47 C48 C43 121.1(6) . . ? C52 C51 S51 111.1(4) . . ? C51 C52 S52 116.3(4) . . ? C58 C53 C54 117.8(6) . . ? C58 C53 S52 115.7(5) . . ? C54 C53 S52 126.5(5) . . ? C55 C54 C53 120.2(6) . . ? C56 C55 C54 120.2(6) . . ? C55 C56 C57 120.7(6) . . ? C55 C56 Cl51 120.1(5) . . ? C57 C56 Cl51 119.2(6) . . ? C58 C57 C56 119.5(7) . . ? C57 C58 C53 121.5(6) . . ? C62 C61 S61 108.8(4) . . ? C61 C62 S62 107.4(4) . . ? C64 C63 C68 118.4(6) . . ? C64 C63 S62 125.5(5) . . ? C68 C63 S62 116.1(5) . . ? C65 C64 C63 120.9(6) . . ? C66 C65 C64 119.9(6) . . ? C67 C66 C65 120.5(6) . . ? C67 C66 Cl61 119.8(5) . . ? C65 C66 Cl61 119.7(5) . . ? C66 C67 C68 119.8(6) . . ? C63 C68 C67 120.5(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.538 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.109 #===END data_s3801a _database_code_depnum_ccdc_archive 'CCDC 655323' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H16 Cl2 I2 Ni2 S4' _chemical_formula_sum 'C16 H16 Cl2 I2 Ni2 S4' _chemical_formula_weight 778.65 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.4582(5) _cell_length_b 15.0185(6) _cell_length_c 9.8037(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.134(2) _cell_angle_gamma 90.00 _cell_volume 2275.16(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11557 _cell_measurement_theta_min 1.89 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 4.972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.327 _exptl_absorpt_correction_T_max 0.863 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20584 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2622 _reflns_number_gt 2179 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement Peakref _computing_data_reduction 'EvalCCD, Sadabs' _computing_structure_solution 'DIRDIF-99 (Beurskens et al., 1999)' _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^)+(0.0166P)^2^+2.3084P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2622 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0203 _refine_ls_wR_factor_ref 0.0413 _refine_ls_wR_factor_gt 0.0387 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 I1 I 0.344040(11) 0.181484(11) 0.396829(19) 0.03469(6) Uani 1 1 d . . . Ni1 Ni 0.47445(2) 0.105034(19) 0.37544(3) 0.02469(8) Uani 1 1 d . . . Cl1 Cl 0.63249(5) 0.55889(4) 0.57334(7) 0.03673(15) Uani 1 1 d . . . S1 S 0.58545(4) 0.04563(4) 0.34004(6) 0.02801(13) Uani 1 1 d . . . S2 S 0.55532(4) 0.15050(4) 0.59242(7) 0.02777(13) Uani 1 1 d . . . C1 C 0.67703(17) 0.10529(18) 0.4675(3) 0.0350(6) Uani 1 1 d . . . H1A H 0.7319 0.0744 0.4773 0.042 Uiso 1 1 calc R . . H1B H 0.6800 0.1666 0.4324 0.042 Uiso 1 1 calc R . . C2 C 0.66306(16) 0.10756(17) 0.6122(3) 0.0330(6) Uani 1 1 d . . . H2A H 0.7077 0.1458 0.6807 0.040 Uiso 1 1 calc R . . H2B H 0.6695 0.0467 0.6534 0.040 Uiso 1 1 calc R . . C3 C 0.57422(15) 0.26708(15) 0.5787(2) 0.0252(5) Uani 1 1 d . . . C4 C 0.57037(18) 0.30695(16) 0.4492(3) 0.0341(6) Uani 1 1 d . . . H4 H 0.5560 0.2725 0.3629 0.041 Uiso 1 1 calc R . . C5 C 0.58732(18) 0.39661(17) 0.4455(3) 0.0344(6) Uani 1 1 d . . . H5 H 0.5843 0.4245 0.3570 0.041 Uiso 1 1 calc R . . C6 C 0.60879(15) 0.44535(15) 0.5728(3) 0.0265(5) Uani 1 1 d . . . C7 C 0.61399(18) 0.40607(16) 0.7016(3) 0.0318(6) Uani 1 1 d . . . H7 H 0.6301 0.4403 0.7884 0.038 Uiso 1 1 calc R . . C8 C 0.59567(18) 0.31636(16) 0.7047(3) 0.0326(6) Uani 1 1 d . . . H8 H 0.5979 0.2889 0.7932 0.039 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 I1 0.02558(10) 0.03918(10) 0.03895(11) -0.00570(7) 0.01065(8) 0.00223(7) Ni1 0.02203(17) 0.02454(15) 0.02640(16) -0.00082(12) 0.00694(14) -0.00134(12) Cl1 0.0453(4) 0.0328(3) 0.0327(3) -0.0053(3) 0.0142(3) -0.0107(3) S1 0.0259(3) 0.0282(3) 0.0280(3) 0.0012(2) 0.0070(3) 0.0045(3) S2 0.0269(3) 0.0300(3) 0.0256(3) 0.0015(2) 0.0080(3) -0.0018(3) C1 0.0215(14) 0.0469(16) 0.0333(15) 0.0001(12) 0.0054(12) 0.0027(11) C2 0.0245(14) 0.0376(14) 0.0317(14) 0.0037(11) 0.0030(12) 0.0034(11) C3 0.0192(12) 0.0297(12) 0.0250(12) -0.0006(9) 0.0053(10) -0.0017(10) C4 0.0417(17) 0.0378(14) 0.0220(12) -0.0075(10) 0.0101(12) -0.0131(12) C5 0.0434(17) 0.0384(14) 0.0238(13) -0.0007(11) 0.0147(12) -0.0148(12) C6 0.0225(13) 0.0283(12) 0.0286(13) -0.0051(10) 0.0086(11) -0.0021(10) C7 0.0402(16) 0.0321(14) 0.0226(12) -0.0059(10) 0.0104(12) 0.0029(11) C8 0.0410(16) 0.0347(13) 0.0223(12) 0.0014(10) 0.0114(12) 0.0047(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Ni1 2.5057(3) . ? Ni1 S1 2.1658(7) . ? Ni1 S1 2.1902(7) 2_655 ? Ni1 S2 2.1940(7) . ? Ni1 Ni1 2.8602(6) 2_655 ? Cl1 C6 1.749(2) . ? S1 C1 1.827(3) . ? S1 Ni1 2.1902(7) 2_655 ? S2 C3 1.791(2) . ? S2 C2 1.833(2) . ? C1 C2 1.514(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.378(3) . ? C3 C4 1.385(3) . ? C4 C5 1.378(3) . ? C4 H4 0.9500 . ? C5 C6 1.383(3) . ? C5 H5 0.9500 . ? C6 C7 1.370(3) . ? C7 C8 1.383(3) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? 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 78.59(3) . 2_655 ? S1 Ni1 S2 91.14(3) . . ? S1 Ni1 S2 169.54(3) 2_655 . ? S1 Ni1 I1 175.04(2) . . ? S1 Ni1 I1 98.81(2) 2_655 . ? S2 Ni1 I1 91.58(2) . . ? S1 Ni1 Ni1 49.327(18) . 2_655 ? S1 Ni1 Ni1 48.590(18) 2_655 2_655 ? S2 Ni1 Ni1 125.02(2) . 2_655 ? I1 Ni1 Ni1 125.861(16) . 2_655 ? C1 S1 Ni1 103.37(8) . . ? C1 S1 Ni1 116.82(9) . 2_655 ? Ni1 S1 Ni1 82.08(2) . 2_655 ? C3 S2 C2 99.51(11) . . ? C3 S2 Ni1 107.12(8) . . ? C2 S2 Ni1 103.60(9) . . ? C2 C1 S1 107.22(18) . . ? C2 C1 H1A 110.3 . . ? S1 C1 H1A 110.3 . . ? C2 C1 H1B 110.3 . . ? S1 C1 H1B 110.3 . . ? H1A C1 H1B 108.5 . . ? C1 C2 S2 111.22(17) . . ? C1 C2 H2A 109.4 . . ? S2 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? S2 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C8 C3 C4 120.4(2) . . ? C8 C3 S2 117.06(18) . . ? C4 C3 S2 122.48(18) . . ? C5 C4 C3 120.0(2) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 119.0(2) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C7 C6 C5 121.3(2) . . ? C7 C6 Cl1 118.29(18) . . ? C5 C6 Cl1 120.41(18) . . ? C6 C7 C8 119.7(2) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C3 C8 C7 119.6(2) . . ? C3 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 Ni1 S1 C1 160.05(9) 2_655 . . . ? S2 Ni1 S1 C1 -21.92(9) . . . . ? Ni1 Ni1 S1 C1 115.80(9) 2_655 . . . ? S1 Ni1 S1 Ni1 44.25(3) 2_655 . . 2_655 ? S2 Ni1 S1 Ni1 -137.71(2) . . . 2_655 ? S1 Ni1 S2 C3 102.50(8) . . . . ? S1 Ni1 S2 C3 113.18(16) 2_655 . . . ? I1 Ni1 S2 C3 -73.35(8) . . . . ? Ni1 Ni1 S2 C3 63.95(8) 2_655 . . . ? S1 Ni1 S2 C2 -2.12(9) . . . . ? S1 Ni1 S2 C2 8.56(18) 2_655 . . . ? I1 Ni1 S2 C2 -177.96(8) . . . . ? Ni1 Ni1 S2 C2 -40.66(9) 2_655 . . . ? Ni1 S1 C1 C2 46.76(18) . . . . ? Ni1 S1 C1 C2 134.56(15) 2_655 . . . ? S1 C1 C2 S2 -52.1(2) . . . . ? C3 S2 C2 C1 -77.8(2) . . . . ? Ni1 S2 C2 C1 32.6(2) . . . . ? C2 S2 C3 C8 -95.2(2) . . . . ? Ni1 S2 C3 C8 157.33(18) . . . . ? C2 S2 C3 C4 83.0(2) . . . . ? Ni1 S2 C3 C4 -24.6(2) . . . . ? C8 C3 C4 C5 -0.6(4) . . . . ? S2 C3 C4 C5 -178.6(2) . . . . ? C3 C4 C5 C6 0.6(4) . . . . ? C4 C5 C6 C7 0.4(4) . . . . ? C4 C5 C6 Cl1 179.0(2) . . . . ? C5 C6 C7 C8 -1.4(4) . . . . ? Cl1 C6 C7 C8 -180.0(2) . . . . ? C4 C3 C8 C7 -0.4(4) . . . . ? S2 C3 C8 C7 177.7(2) . . . . ? C6 C7 C8 C3 1.4(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.368 _refine_diff_density_min -0.422 _refine_diff_density_rms 0.083 #===END