Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Dahl, Lawrence F.' 'Agarwa, Sorabh' 'Ivanov, Sergei A.' 'Kozee, Michael A.' 'Merrill, W. Zlex' _publ_contact_author_name 'Prof Lawrence F Dahl' _publ_contact_author_address ; Department of Chemistry University of Wisconsin-Madison Madison WI 53706 UNITED STATES OF AMERICA ; _publ_contact_author_email '?' _publ_section_title ; Cyclo-[Ni(mu2-SPh)2]9 and Cyclo-[Ni(mi2-SPh)2]11: New Oligomeric Types of Toroidal Nickel(II) Thiolates Containing Geometrically Unprecedented 9-and 1-Membereed Ring Systems ; data_dahl150nm _database_code_CSD 186293 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C132 H110 Ni11 O5 S22' _chemical_formula_weight 3127.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 18.888(2) _cell_length_b 29.401(4) _cell_length_c 28.354(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.995(3) _cell_angle_gamma 90.00 _cell_volume 15552(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8121 _cell_measurement_theta_min 1.29 _cell_measurement_theta_max 28.33 _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6408 _exptl_absorpt_coefficient_mu 1.639 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.510 _exptl_absorpt_correction_T_max 0.697 _exptl_absorpt_process_details ; Empirical with SADABS (Blessing, 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'N/A' _diffrn_standards_interval_count 'N/A' _diffrn_standards_interval_time 'N/A' _diffrn_standards_decay_% <1 _diffrn_reflns_number 60554 _diffrn_reflns_av_R_equivalents 0.0544 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 28.33 _reflns_number_total 18453 _reflns_number_gt 12887 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1119P)^2^+2.6232P] 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 18453 _refine_ls_number_parameters 915 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1816 _refine_ls_wR_factor_gt 0.1608 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.02721(3) 0.334919(17) 0.706250(17) 0.02879(13) Uani 1 1 d . . . Ni2 Ni 0.08366(3) 0.288733(17) 0.616107(18) 0.02864(13) Uani 1 1 d . . . Ni3 Ni 0.10822(3) 0.214759(17) 0.554744(18) 0.03201(14) Uani 1 1 d . A . Ni4 Ni 0.07949(3) 0.126455(16) 0.590638(18) 0.02924(13) Uani 1 1 d . A . Ni5 Ni 0.04452(3) 0.050795(16) 0.665402(17) 0.02606(13) Uani 1 1 d . A . Ni6 Ni 0.0000 0.00671(2) 0.7500 0.02462(15) Uani 1 2 d S . . S1 S -0.06930(5) 0.36797(4) 0.72548(3) 0.0323(2) Uani 1 1 d . . . S2 S -0.02065(5) 0.30357(3) 0.63865(3) 0.0299(2) Uani 1 1 d . . . S3 S 0.12449(5) 0.30015(4) 0.69220(4) 0.0322(2) Uani 1 1 d . . . S4 S 0.03599(6) 0.27412(3) 0.54116(4) 0.0327(2) Uani 1 1 d . . . S5 S 0.18256(6) 0.26596(3) 0.59101(4) 0.0352(2) Uani 1 1 d . . . S6 S 0.02931(6) 0.16277(3) 0.52584(4) 0.0344(2) Uani 1 1 d . . . S7 S 0.17834(6) 0.15455(4) 0.56962(4) 0.0381(3) Uani 1 1 d . . . S8 S -0.01549(5) 0.10117(3) 0.61758(3) 0.0288(2) Uani 1 1 d . . . S9 S 0.13332(5) 0.09724(3) 0.65850(3) 0.0286(2) Uani 1 1 d . . . S10 S -0.04713(5) 0.00578(3) 0.67307(3) 0.0290(2) Uani 1 1 d . . . S11 S 0.10181(5) 0.00713(4) 0.72192(4) 0.0338(2) Uani 1 1 d . . . C10 C -0.15231(13) 0.34725(11) 0.69572(11) 0.0395(10) Uani 1 1 d G . . C11 C -0.20360(18) 0.37984(10) 0.67932(13) 0.0608(15) Uani 1 1 d G . . H11 H -0.1931 0.4106 0.6840 0.073 Uiso 1 1 calc R . . C12 C -0.27055(16) 0.36651(15) 0.65587(14) 0.087(2) Uani 1 1 d G . . H12 H -0.3049 0.3883 0.6449 0.105 Uiso 1 1 calc R . . C13 C -0.28622(14) 0.32058(17) 0.64882(14) 0.085(2) Uani 1 1 d G . . H13 H -0.3310 0.3117 0.6331 0.102 Uiso 1 1 calc R . . C14 C -0.23493(19) 0.28799(12) 0.66522(13) 0.0681(18) Uani 1 1 d G . . H14 H -0.2454 0.2573 0.6605 0.082 Uiso 1 1 calc R . . C15 C -0.16797(16) 0.30132(10) 0.68867(12) 0.0487(12) Uani 1 1 d G . . H15 H -0.1337 0.2795 0.6996 0.058 Uiso 1 1 calc R . . C20 C -0.06022(15) 0.34863(8) 0.60130(9) 0.0339(9) Uani 1 1 d G . . C21 C -0.03905(14) 0.39359(9) 0.60949(9) 0.0349(9) Uani 1 1 d G . . H21 H -0.0037 0.4008 0.6350 0.042 Uiso 1 1 calc R . . C22 C -0.07080(16) 0.42776(7) 0.57952(11) 0.0418(10) Uani 1 1 d G . . H22 H -0.0566 0.4578 0.5850 0.050 Uiso 1 1 calc R . . C23 C -0.12372(18) 0.41698(9) 0.54135(11) 0.0590(15) Uani 1 1 d G . . H23 H -0.1450 0.4398 0.5213 0.071 Uiso 1 1 calc R . . C24 C -0.14488(18) 0.37202(10) 0.53316(11) 0.0672(18) Uani 1 1 d G . . H24 H -0.1803 0.3648 0.5076 0.081 Uiso 1 1 calc R . . C25 C -0.11313(17) 0.33784(7) 0.56314(11) 0.0503(13) Uani 1 1 d G . . H25 H -0.1273 0.3078 0.5577 0.060 Uiso 1 1 calc R . . C30 C 0.19313(13) 0.34185(9) 0.69542(11) 0.0373(9) Uani 1 1 d G . . C31 C 0.26143(16) 0.33063(10) 0.71830(13) 0.0556(14) Uani 1 1 d G . . H31 H 0.2711 0.3012 0.7296 0.067 Uiso 1 1 calc R . . C32 C 0.31523(13) 0.36334(13) 0.72423(14) 0.0730(18) Uani 1 1 d G . . H32 H 0.3609 0.3558 0.7395 0.088 Uiso 1 1 calc R . . C33 C 0.30073(17) 0.40726(12) 0.70729(15) 0.0714(18) Uani 1 1 d G . . H33 H 0.3367 0.4291 0.7113 0.086 Uiso 1 1 calc R . . C34 C 0.2324(2) 0.41847(9) 0.68442(14) 0.0631(15) Uani 1 1 d G . . H34 H 0.2227 0.4479 0.6731 0.076 Uiso 1 1 calc R . . C35 C 0.17863(14) 0.38577(10) 0.67848(12) 0.0495(12) Uani 1 1 d G . . H35 H 0.1329 0.3933 0.6632 0.059 Uiso 1 1 calc R . . C40 C 0.07884(18) 0.31410(9) 0.50718(10) 0.0398(10) Uani 1 1 d G . . C41 C 0.0763(2) 0.36007(10) 0.51824(11) 0.0645(17) Uani 1 1 d G . . H41 H 0.0556 0.3694 0.5443 0.077 Uiso 1 1 calc R . . C42 C 0.1046(2) 0.39210(8) 0.49032(15) 0.082(2) Uani 1 1 d G . . H42 H 0.1029 0.4229 0.4977 0.098 Uiso 1 1 calc R . . C43 C 0.1355(2) 0.37816(12) 0.45133(13) 0.076(2) Uani 1 1 d G . . H43 H 0.1544 0.3996 0.4326 0.091 Uiso 1 1 calc R . . C44 C 0.13805(19) 0.33220(13) 0.44027(10) 0.0626(16) Uani 1 1 d G . . H44 H 0.1587 0.3229 0.4142 0.075 Uiso 1 1 calc R . . C45 C 0.10973(18) 0.30017(9) 0.46819(11) 0.0482(12) Uani 1 1 d G . . H45 H 0.1115 0.2694 0.4608 0.058 Uiso 1 1 calc R . . C50 C 0.24474(16) 0.24217(12) 0.63830(11) 0.0446(11) Uani 1 1 d G . . C51 C 0.31597(18) 0.25550(14) 0.64168(16) 0.0714(18) Uani 1 1 d G . . H51 H 0.3298 0.2750 0.6189 0.086 Uiso 1 1 calc R . . C52 C 0.36647(14) 0.23976(17) 0.67907(19) 0.100(3) Uani 1 1 d G . . H52 H 0.4141 0.2487 0.6813 0.120 Uiso 1 1 calc R . . C53 C 0.3457(2) 0.21068(17) 0.71309(15) 0.105(3) Uani 1 1 d G . . H53 H 0.3795 0.2001 0.7381 0.126 Uiso 1 1 calc R . . C54 C 0.2745(3) 0.19735(14) 0.70971(12) 0.081(2) Uani 1 1 d G . . H54 H 0.2607 0.1779 0.7325 0.098 Uiso 1 1 calc R . . C55 C 0.22402(17) 0.21310(12) 0.67232(13) 0.0536(13) Uani 1 1 d G . . H55 H 0.1764 0.2042 0.6701 0.064 Uiso 1 1 calc R . . C60 C -0.05993(12) 0.18000(9) 0.52975(9) 0.0347(9) Uani 1 1 d G . . C61 C -0.11195(17) 0.17347(10) 0.48990(8) 0.0461(12) Uani 1 1 d G . . H61 H -0.0995 0.1609 0.4623 0.055 Uiso 1 1 calc R . . C62 C -0.18263(15) 0.18578(12) 0.49136(10) 0.0577(15) Uani 1 1 d G . . H62 H -0.2174 0.1814 0.4647 0.069 Uiso 1 1 calc R . . C63 C -0.20129(11) 0.20462(11) 0.53267(12) 0.0545(14) Uani 1 1 d G . . H63 H -0.2486 0.2129 0.5336 0.065 Uiso 1 1 calc R . . C64 C -0.14927(15) 0.21116(10) 0.57252(9) 0.0444(11) Uani 1 1 d G . . H64 H -0.1617 0.2238 0.6002 0.053 Uiso 1 1 calc R . . C65 C -0.07859(13) 0.19885(9) 0.57106(8) 0.0352(9) Uani 1 1 d G . . H65 H -0.0438 0.2032 0.5977 0.042 Uiso 1 1 calc R . . C70 C 0.1790(5) 0.1282(2) 0.5092(3) 0.034(2) Uani 0.64(2) 1 d PG A 1 C71 C 0.2030(6) 0.1532(2) 0.4732(4) 0.039(3) Uani 0.64(2) 1 d PG A 1 H71 H 0.2159 0.1835 0.4784 0.046 Uiso 0.64(2) 1 calc PR A 1 C72 C 0.2075(5) 0.1329(3) 0.4296(3) 0.045(3) Uani 0.64(2) 1 d PG A 1 H72 H 0.2236 0.1496 0.4055 0.054 Uiso 0.64(2) 1 calc PR A 1 C73 C 0.1881(5) 0.0876(3) 0.4219(3) 0.042(2) Uani 0.64(2) 1 d PG A 1 H73 H 0.1911 0.0740 0.3927 0.050 Uiso 0.64(2) 1 calc PR A 1 C74 C 0.1641(6) 0.06259(17) 0.4579(3) 0.047(3) Uani 0.64(2) 1 d PG A 1 H74 H 0.1511 0.0323 0.4528 0.056 Uiso 0.64(2) 1 calc PR A 1 C75 C 0.1596(5) 0.0829(2) 0.5016(3) 0.036(2) Uani 0.64(2) 1 d PG A 1 H75 H 0.1435 0.0662 0.5257 0.043 Uiso 0.64(2) 1 calc PR A 1 C70 C 0.1947(14) 0.1306(4) 0.5208(7) 0.050(6) Uani 0.36(2) 1 d PG A 2 C71 C 0.2095(16) 0.1560(3) 0.4821(7) 0.059(8) Uani 0.36(2) 1 d PG A 2 H71A H 0.2090 0.1876 0.4835 0.071 Uiso 0.36(2) 1 calc PR A 2 C72 C 0.2250(16) 0.1341(5) 0.4415(7) 0.061(8) Uani 0.36(2) 1 d PG A 2 H72A H 0.2348 0.1511 0.4156 0.073 Uiso 0.36(2) 1 calc PR A 2 C73 C 0.2257(19) 0.0869(5) 0.4395(7) 0.080(10) Uani 0.36(2) 1 d PG A 2 H73A H 0.2360 0.0722 0.4123 0.095 Uiso 0.36(2) 1 calc PR A 2 C74 C 0.211(2) 0.0615(3) 0.4782(8) 0.087(11) Uani 0.36(2) 1 d PG A 2 H74A H 0.2114 0.0299 0.4769 0.104 Uiso 0.36(2) 1 calc PR A 2 C75 C 0.1954(16) 0.0834(4) 0.5189(7) 0.056(7) Uani 0.36(2) 1 d PG A 2 H75A H 0.1855 0.0664 0.5447 0.067 Uiso 0.36(2) 1 calc PR A 2 C80 C -0.07621(13) 0.07660(10) 0.57030(9) 0.0346(9) Uani 1 1 d G A . C81 C -0.05426(15) 0.05716(11) 0.53030(10) 0.0470(12) Uani 1 1 d G . . H81 H -0.0057 0.0542 0.5287 0.056 Uiso 1 1 calc R A . C82 C -0.1050(2) 0.04214(12) 0.49264(9) 0.0670(17) Uani 1 1 d G A . H82 H -0.0903 0.0291 0.4659 0.080 Uiso 1 1 calc R . . C83 C -0.17759(19) 0.04655(13) 0.49499(11) 0.0725(19) Uani 1 1 d G . . H83 H -0.2115 0.0365 0.4698 0.087 Uiso 1 1 calc R A . C84 C -0.19954(13) 0.06598(13) 0.53500(13) 0.0621(16) Uani 1 1 d G A . H84 H -0.2481 0.0689 0.5366 0.075 Uiso 1 1 calc R . . C85 C -0.14885(15) 0.08101(11) 0.57265(10) 0.0445(11) Uani 1 1 d G . . H85 H -0.1635 0.0940 0.5994 0.053 Uiso 1 1 calc R A . C90 C 0.20810(13) 0.06440(9) 0.64775(11) 0.0380(10) Uani 1 1 d G A . C91 C 0.27570(16) 0.08382(10) 0.65923(12) 0.0526(13) Uani 1 1 d G . . H91 H 0.2803 0.1137 0.6702 0.063 Uiso 1 1 calc R A . C92 C 0.33643(13) 0.05865(14) 0.65435(14) 0.0719(19) Uani 1 1 d G A . H92 H 0.3817 0.0716 0.6620 0.086 Uiso 1 1 calc R . . C93 C 0.32955(17) 0.01406(14) 0.63799(14) 0.081(2) Uani 1 1 d G . . H93 H 0.3702 -0.0028 0.6347 0.097 Uiso 1 1 calc R A . C94 C 0.2620(2) -0.00536(9) 0.62651(12) 0.0655(17) Uani 1 1 d G A . H94 H 0.2574 -0.0352 0.6156 0.079 Uiso 1 1 calc R . . C95 C 0.20123(16) 0.01981(10) 0.63139(11) 0.0459(11) Uani 1 1 d G . . H95 H 0.1560 0.0068 0.6237 0.055 Uiso 1 1 calc R A . C100 C -0.0239(7) -0.0482(4) 0.6535(4) 0.048(8) Uani 0.50 1 d PG A 1 C101 C -0.0041(7) -0.0855(5) 0.6828(4) 0.060(5) Uani 0.50 1 d PG A 1 H101 H 0.0031 -0.0821 0.7158 0.073 Uiso 0.50 1 calc PR A 1 C102 C 0.0050(9) -0.1278(4) 0.6627(5) 0.062(5) Uani 0.50 1 d PG A 1 H102 H 0.0182 -0.1527 0.6824 0.074 Uiso 0.50 1 calc PR A 1 C103 C -0.0058(9) -0.1329(3) 0.6134(6) 0.095(9) Uani 0.50 1 d PG A 1 H103 H 0.0003 -0.1613 0.6000 0.114 Uiso 0.50 1 calc PR A 1 C104 C -0.0256(9) -0.0957(5) 0.5841(4) 0.123(9) Uani 0.50 1 d PG A 1 H104 H -0.0328 -0.0991 0.5511 0.148 Uiso 0.50 1 calc PR A 1 C105 C -0.0346(8) -0.0533(4) 0.6041(4) 0.122(10) Uani 0.50 1 d PG A 1 H105 H -0.0479 -0.0284 0.5845 0.146 Uiso 0.50 1 calc PR A 1 C100 C -0.0207(5) -0.0488(3) 0.6526(4) 0.025(6) Uani 0.50 1 d PG A 2 C101 C -0.0301(6) -0.0873(4) 0.6794(3) 0.039(3) Uani 0.50 1 d PG A 2 H10A H -0.0459 -0.0844 0.7088 0.047 Uiso 0.50 1 calc PR A 2 C102 C -0.0160(7) -0.1301(3) 0.6624(4) 0.063(5) Uani 0.50 1 d PG A 2 H10B H -0.0222 -0.1559 0.6804 0.076 Uiso 0.50 1 calc PR A 2 C103 C 0.0076(6) -0.1345(2) 0.6186(4) 0.037(3) Uani 0.50 1 d PG A 2 H10C H 0.0171 -0.1632 0.6072 0.044 Uiso 0.50 1 calc PR A 2 C104 C 0.0170(4) -0.0960(3) 0.5918(3) 0.037(2) Uani 0.50 1 d PG A 2 H10D H 0.0328 -0.0990 0.5624 0.044 Uiso 0.50 1 calc PR A 2 C105 C 0.0028(4) -0.0532(2) 0.6088(4) 0.036(2) Uani 0.50 1 d PG A 2 H10E H 0.0091 -0.0274 0.5908 0.043 Uiso 0.50 1 calc PR A 2 C110 C 0.1603(5) 0.0484(4) 0.7615(6) 0.043(4) Uani 0.50 1 d PG A 1 C111 C 0.2335(6) 0.0396(4) 0.7676(5) 0.057(4) Uani 0.50 1 d PG A 1 H111 H 0.2506 0.0142 0.7535 0.069 Uiso 0.50 1 calc PR A 1 C112 C 0.2812(4) 0.0689(5) 0.7949(5) 0.092(8) Uani 0.50 1 d PG A 1 H112 H 0.3301 0.0630 0.7990 0.110 Uiso 0.50 1 calc PR A 1 C113 C 0.2556(6) 0.1069(5) 0.8160(5) 0.099(8) Uani 0.50 1 d PG A 1 H113 H 0.2875 0.1265 0.8343 0.119 Uiso 0.50 1 calc PR A 1 C114 C 0.1825(7) 0.1157(4) 0.8099(5) 0.069(5) Uani 0.50 1 d PG A 1 H114 H 0.1654 0.1411 0.8241 0.082 Uiso 0.50 1 calc PR A 1 C115 C 0.1348(5) 0.0864(5) 0.7826(5) 0.038(3) Uani 0.50 1 d PG A 1 H115 H 0.0858 0.0922 0.7785 0.046 Uiso 0.50 1 calc PR A 1 C110 C 0.1711(5) 0.0363(4) 0.7555(6) 0.034(3) Uani 0.50 1 d PG A 2 C111 C 0.2407(6) 0.0198(4) 0.7597(5) 0.043(3) Uani 0.50 1 d PG A 2 H11A H 0.2499 -0.0073 0.7448 0.052 Uiso 0.50 1 calc PR A 2 C112 C 0.2967(4) 0.0438(4) 0.7862(5) 0.078(5) Uani 0.50 1 d PG A 2 H11B H 0.3434 0.0328 0.7890 0.094 Uiso 0.50 1 calc PR A 2 C113 C 0.2831(5) 0.0843(4) 0.8084(5) 0.076(6) Uani 0.50 1 d PG A 2 H11C H 0.3206 0.1003 0.8262 0.091 Uiso 0.50 1 calc PR A 2 C114 C 0.2134(6) 0.1008(3) 0.8042(5) 0.058(4) Uani 0.50 1 d PG A 2 H11D H 0.2043 0.1278 0.8191 0.070 Uiso 0.50 1 calc PR A 2 C115 C 0.1574(4) 0.0768(4) 0.7777(5) 0.035(3) Uani 0.50 1 d PG A 2 H11E H 0.1108 0.0878 0.7749 0.042 Uiso 0.50 1 calc PR A 2 C1S C 0.1471(6) 0.5639(3) 0.5778(3) 0.168(5) Uani 0.386(14) 1 d PD B 1 H1S1 H 0.1739 0.5663 0.6098 0.201 Uiso 0.386(14) 1 calc PR B 1 H1S2 H 0.1692 0.5826 0.5559 0.201 Uiso 0.386(14) 1 calc PR B 1 C2S C 0.0437(11) 0.5363(6) 0.6070(10) 0.063(5) Uani 0.193(7) 1 d PD B 1 H2S1 H -0.0057 0.5277 0.5958 0.076 Uiso 0.193(7) 1 calc PR B 1 H2S2 H 0.0476 0.5464 0.6398 0.076 Uiso 0.193(7) 1 calc PR B 1 C3S C 0.1352(12) 0.5112(6) 0.5597(8) 0.047(3) Uani 0.193(7) 1 d PD B 1 H3S1 H 0.1047 0.5087 0.5289 0.057 Uiso 0.193(7) 1 calc PR B 1 H3S2 H 0.1800 0.4953 0.5590 0.057 Uiso 0.193(7) 1 calc PR B 1 C4S C 0.0956(6) 0.4947(3) 0.6030(5) 0.212(8) Uani 0.386(14) 1 d PD B 1 H4S1 H 0.1293 0.4905 0.6322 0.254 Uiso 0.386(14) 1 calc PR B 1 H4S2 H 0.0691 0.4667 0.5952 0.254 Uiso 0.386(14) 1 calc PR B 1 C5S C 0.0669(7) 0.5741(5) 0.5757(7) 0.79(5) Uani 0.386(14) 1 d PD B 1 H5S1 H 0.0594 0.6039 0.5887 0.951 Uiso 0.386(14) 1 calc PR B 1 H5S2 H 0.0415 0.5723 0.5433 0.951 Uiso 0.386(14) 1 calc PR B 1 C1P C 0.1471(6) 0.5639(3) 0.5778(3) 0.168(5) Uani 0.681(14) 1 d PD B 2 H1P1 H 0.1615 0.5719 0.5475 0.201 Uiso 0.681(14) 1 calc PR B 2 H1P2 H 0.1746 0.5825 0.6024 0.201 Uiso 0.681(14) 1 calc PR B 2 C2P C 0.0350(6) 0.5291(4) 0.5745(8) 0.063(5) Uani 0.340(7) 1 d PD B 2 H2P1 H 0.0213 0.5191 0.5417 0.076 Uiso 0.340(7) 1 calc PR B 2 H2P2 H -0.0074 0.5295 0.5898 0.076 Uiso 0.340(7) 1 calc PR B 2 C3P C 0.1635(6) 0.5141(4) 0.5883(5) 0.047(3) Uani 0.340(7) 1 d PD B 2 H3P1 H 0.2037 0.5109 0.6140 0.057 Uiso 0.340(7) 1 calc PR B 2 H3P2 H 0.1749 0.4987 0.5602 0.057 Uiso 0.340(7) 1 calc PR B 2 C4P C 0.0956(6) 0.4947(3) 0.6030(5) 0.212(8) Uani 0.681(14) 1 d PD B 2 H4P1 H 0.0967 0.4963 0.6372 0.254 Uiso 0.681(14) 1 calc PR B 2 H4P2 H 0.0876 0.4635 0.5924 0.254 Uiso 0.681(14) 1 calc PR B 2 C5P C 0.0669(7) 0.5741(5) 0.5757(7) 0.79(5) Uani 0.681(14) 1 d PD B 2 H5P1 H 0.0582 0.5909 0.6037 0.951 Uiso 0.681(14) 1 calc PR B 2 H5P2 H 0.0483 0.5914 0.5474 0.951 Uiso 0.681(14) 1 calc PR B 2 C10S C -0.0423(7) 0.2029(6) 0.7366(4) 0.195(15) Uani 0.53 1 d PD . . H10C' H -0.0406 0.2358 0.7354 0.234 Uiso 0.53 1 calc PR . . H10F H 0.0038 0.1905 0.7507 0.234 Uiso 0.53 1 calc PR . . C11S C 0.0632(5) 0.1881(4) 0.7958(3) 0.066(3) Uani 0.53 1 d PD . . H11E' H 0.0827 0.2138 0.8150 0.079 Uiso 0.53 1 calc PR . . H11F H 0.0803 0.1604 0.8124 0.079 Uiso 0.53 1 calc PR . . C12S C 0.0197(4) 0.1895(3) 0.7113(2) 0.044(2) Uani 0.53 1 d PD . . H12A H -0.0056 0.1611 0.7038 0.053 Uiso 0.53 1 calc PR . . H12B H 0.0125 0.2131 0.6871 0.053 Uiso 0.53 1 calc PR . . C13S C 0.0872(5) 0.1897(5) 0.7475(4) 0.112(8) Uani 0.53 1 d PD . . H13A H 0.1148 0.2171 0.7444 0.135 Uiso 0.53 1 calc PR . . H13B H 0.1167 0.1635 0.7431 0.135 Uiso 0.53 1 calc PR . . C20S C 0.0161(6) 0.5311(4) 0.6960(4) 0.088(4) Uani 0.53 1 d PD . . H20A H 0.0609 0.5230 0.6854 0.106 Uiso 0.53 1 calc PR . . H20B H -0.0195 0.5385 0.6687 0.106 Uiso 0.53 1 calc PR . . C21S C -0.0102(10) 0.4929(4) 0.7270(6) 0.205(18) Uani 0.53 1 d PD . . H21A H -0.0497 0.4990 0.7442 0.247 Uiso 0.53 1 calc PR . . H21B H -0.0012 0.4614 0.7199 0.247 Uiso 0.53 1 calc PR . . C22S C 0.0259(9) 0.5689(5) 0.7320(5) 0.183(13) Uani 0.53 1 d PD . . H22A H 0.0212 0.5976 0.7150 0.219 Uiso 0.53 1 calc PR . . H22B H 0.0743 0.5673 0.7494 0.219 Uiso 0.53 1 calc PR . . C23S C -0.0298(12) 0.5159(6) 0.7719(6) 0.69(8) Uani 0.53 1 d PD . . H23A H -0.0299 0.5373 0.7458 0.832 Uiso 0.53 1 calc PR . . H23B H -0.0763 0.5013 0.7691 0.832 Uiso 0.53 1 calc PR . . C30S C 0.0576(6) 0.7395(4) 0.6023(6) 0.214(8) Uani 0.344(18) 1 d PD C 1 H30A H 0.0104 0.7463 0.5849 0.257 Uiso 0.344(18) 1 calc PR C 1 H30B H 0.0821 0.7678 0.6118 0.257 Uiso 0.344(18) 1 calc PR C 1 C31S C 0.1007(6) 0.7108(5) 0.5720(4) 0.176(6) Uani 0.344(18) 1 d PD C 1 H31A H 0.0800 0.7130 0.5385 0.211 Uiso 0.344(18) 1 calc PR C 1 H31B H 0.1498 0.7214 0.5757 0.211 Uiso 0.344(18) 1 calc PR C 1 C32S C 0.0521(8) 0.7098(8) 0.6460(5) 0.36(2) Uani 0.344(18) 1 d PD C 1 H32A H 0.0747 0.7251 0.6748 0.427 Uiso 0.344(18) 1 calc PR C 1 H32B H 0.0021 0.7048 0.6486 0.427 Uiso 0.344(18) 1 calc PR C 1 C33S C 0.088(3) 0.6651(8) 0.6409(9) 0.087(7) Uani 0.172(9) 1 d PD C 1 H33A H 0.0589 0.6401 0.6489 0.104 Uiso 0.172(9) 1 calc PR C 1 H33B H 0.1343 0.6639 0.6616 0.104 Uiso 0.172(9) 1 calc PR C 1 C34S C 0.098(2) 0.6625(6) 0.5887(9) 0.076(5) Uani 0.172(9) 1 d PD C 1 H34A H 0.1425 0.6469 0.5855 0.091 Uiso 0.172(9) 1 calc PR C 1 H34B H 0.0586 0.6463 0.5701 0.091 Uiso 0.172(9) 1 calc PR C 1 C30P C 0.0576(6) 0.7395(4) 0.6023(6) 0.214(8) Uani 0.723(18) 1 d PD C 2 H30C H 0.0104 0.7463 0.5849 0.257 Uiso 0.723(18) 1 calc PR C 2 H30D H 0.0821 0.7678 0.6118 0.257 Uiso 0.723(18) 1 calc PR C 2 C31P C 0.1007(6) 0.7108(5) 0.5720(4) 0.176(6) Uani 0.723(18) 1 d PD C 2 H31C H 0.0690 0.6916 0.5502 0.211 Uiso 0.723(18) 1 calc PR C 2 H31D H 0.1276 0.7301 0.5535 0.211 Uiso 0.723(18) 1 calc PR C 2 C32P C 0.0521(8) 0.7098(8) 0.6460(5) 0.36(2) Uani 0.723(18) 1 d PD C 2 H32C H 0.0516 0.7283 0.6743 0.427 Uiso 0.723(18) 1 calc PR C 2 H32D H 0.0091 0.6912 0.6408 0.427 Uiso 0.723(18) 1 calc PR C 2 C33P C 0.1187(10) 0.6807(7) 0.6506(5) 0.087(7) Uani 0.361(9) 1 d PD C 2 H33C H 0.1534 0.6915 0.6771 0.104 Uiso 0.361(9) 1 calc PR C 2 H33D H 0.1067 0.6495 0.6572 0.104 Uiso 0.361(9) 1 calc PR C 2 C34P C 0.1502(8) 0.6825(6) 0.6064(6) 0.076(5) Uani 0.361(9) 1 d PD C 2 H34C H 0.1543 0.6521 0.5938 0.091 Uiso 0.361(9) 1 calc PR C 2 H34D H 0.1975 0.6961 0.6124 0.091 Uiso 0.361(9) 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 0.0282(3) 0.0340(3) 0.0242(2) -0.0006(2) 0.0041(2) -0.0018(2) Ni2 0.0318(3) 0.0281(3) 0.0269(3) -0.00001(19) 0.0071(2) -0.0010(2) Ni3 0.0445(3) 0.0257(3) 0.0274(3) 0.00316(19) 0.0107(2) 0.0037(2) Ni4 0.0367(3) 0.0254(2) 0.0270(3) 0.00431(19) 0.0089(2) 0.0034(2) Ni5 0.0259(3) 0.0282(3) 0.0239(2) 0.00483(18) 0.00338(19) 0.00073(19) Ni6 0.0229(3) 0.0257(3) 0.0250(3) 0.000 0.0028(3) 0.000 S1 0.0304(5) 0.0388(6) 0.0278(5) 0.0044(4) 0.0046(4) 0.0017(4) S2 0.0315(5) 0.0320(5) 0.0260(5) -0.0004(4) 0.0037(4) -0.0018(4) S3 0.0301(5) 0.0356(5) 0.0308(5) -0.0035(4) 0.0048(4) -0.0026(4) S4 0.0445(6) 0.0277(5) 0.0267(5) 0.0020(4) 0.0083(4) 0.0020(4) S5 0.0380(6) 0.0303(5) 0.0397(6) 0.0035(4) 0.0135(5) 0.0020(4) S6 0.0541(7) 0.0250(5) 0.0246(5) 0.0011(4) 0.0077(4) 0.0034(4) S7 0.0452(6) 0.0314(5) 0.0424(6) 0.0082(4) 0.0210(5) 0.0066(4) S8 0.0314(5) 0.0286(5) 0.0252(4) 0.0030(4) 0.0007(4) 0.0014(4) S9 0.0281(5) 0.0296(5) 0.0293(5) 0.0038(4) 0.0081(4) 0.0021(4) S10 0.0267(5) 0.0330(5) 0.0270(5) 0.0012(4) 0.0034(4) 0.0011(4) S11 0.0253(5) 0.0409(6) 0.0352(5) 0.0143(4) 0.0051(4) 0.0018(4) C10 0.026(2) 0.064(3) 0.028(2) 0.008(2) 0.0034(17) -0.0037(19) C11 0.043(3) 0.082(4) 0.053(3) 0.031(3) -0.009(2) 0.000(3) C12 0.045(3) 0.130(7) 0.080(5) 0.046(5) -0.015(3) -0.002(4) C13 0.041(3) 0.157(8) 0.052(4) 0.010(4) -0.010(3) -0.019(4) C14 0.055(3) 0.102(5) 0.049(3) -0.022(3) 0.015(3) -0.032(3) C15 0.043(3) 0.066(3) 0.039(3) -0.010(2) 0.013(2) -0.011(2) C20 0.034(2) 0.039(2) 0.029(2) 0.0024(17) 0.0043(17) 0.0015(17) C21 0.034(2) 0.037(2) 0.033(2) 0.0003(17) 0.0042(17) -0.0032(17) C22 0.043(3) 0.035(2) 0.046(3) 0.0016(19) 0.005(2) 0.0013(19) C23 0.057(3) 0.048(3) 0.062(3) 0.009(3) -0.019(3) 0.009(2) C24 0.070(4) 0.050(3) 0.067(4) 0.014(3) -0.035(3) -0.007(3) C25 0.052(3) 0.040(3) 0.051(3) 0.002(2) -0.018(2) -0.004(2) C30 0.035(2) 0.044(2) 0.035(2) -0.0079(18) 0.0103(18) -0.0061(18) C31 0.036(3) 0.071(4) 0.058(3) -0.010(3) 0.001(2) -0.007(2) C32 0.038(3) 0.091(5) 0.084(4) -0.011(4) -0.007(3) -0.024(3) C33 0.057(4) 0.074(4) 0.083(4) -0.018(3) 0.010(3) -0.033(3) C34 0.071(4) 0.048(3) 0.074(4) -0.012(3) 0.023(3) -0.018(3) C35 0.048(3) 0.049(3) 0.055(3) -0.008(2) 0.018(2) -0.006(2) C40 0.049(3) 0.036(2) 0.038(2) 0.0151(18) 0.019(2) 0.0111(19) C41 0.093(4) 0.040(3) 0.074(4) 0.016(3) 0.058(3) 0.016(3) C42 0.094(5) 0.050(3) 0.118(6) 0.034(4) 0.068(4) 0.016(3) C43 0.072(4) 0.080(4) 0.085(4) 0.053(4) 0.043(4) 0.019(3) C44 0.049(3) 0.099(5) 0.045(3) 0.020(3) 0.025(2) 0.018(3) C45 0.051(3) 0.059(3) 0.037(2) 0.006(2) 0.018(2) 0.016(2) C50 0.041(3) 0.041(3) 0.049(3) -0.001(2) 0.003(2) 0.010(2) C51 0.040(3) 0.070(4) 0.101(5) -0.012(4) 0.002(3) 0.013(3) C52 0.043(4) 0.103(6) 0.144(8) -0.023(6) -0.018(4) 0.019(4) C53 0.086(6) 0.101(6) 0.109(7) -0.023(5) -0.046(5) 0.038(5) C54 0.114(6) 0.061(4) 0.060(4) 0.000(3) -0.016(4) 0.027(4) C55 0.064(3) 0.044(3) 0.049(3) -0.005(2) -0.001(3) 0.011(2) C60 0.051(3) 0.0201(18) 0.030(2) 0.0052(15) -0.0025(18) 0.0010(17) C61 0.064(3) 0.037(2) 0.033(2) 0.0075(19) -0.005(2) -0.007(2) C62 0.055(3) 0.058(3) 0.051(3) 0.015(3) -0.020(3) -0.005(3) C63 0.041(3) 0.047(3) 0.070(4) 0.010(3) -0.009(2) 0.000(2) C64 0.048(3) 0.034(2) 0.051(3) -0.001(2) 0.005(2) 0.004(2) C65 0.039(2) 0.027(2) 0.037(2) -0.0025(17) -0.0022(18) 0.0002(17) C70 0.042(5) 0.039(5) 0.027(4) -0.003(3) 0.020(4) 0.005(3) C71 0.049(6) 0.030(5) 0.042(5) 0.007(4) 0.022(4) -0.010(4) C72 0.055(6) 0.048(6) 0.034(5) 0.001(4) 0.016(5) -0.005(4) C73 0.049(5) 0.050(4) 0.029(4) -0.010(3) 0.013(4) -0.003(4) C74 0.065(7) 0.034(4) 0.044(5) -0.010(3) 0.018(5) 0.001(4) C75 0.045(5) 0.032(4) 0.033(4) -0.002(3) 0.014(4) -0.002(3) C70 0.098(17) 0.020(8) 0.038(9) 0.003(6) 0.034(11) -0.003(8) C71 0.11(2) 0.037(12) 0.038(10) -0.015(8) 0.037(12) 0.007(12) C72 0.12(2) 0.037(10) 0.033(10) -0.002(7) 0.036(13) -0.021(11) C73 0.14(3) 0.059(11) 0.047(12) -0.020(9) 0.055(16) -0.020(14) C74 0.17(3) 0.036(9) 0.063(14) -0.007(8) 0.045(18) -0.031(12) C75 0.098(19) 0.028(7) 0.052(11) -0.003(7) 0.045(13) -0.006(9) C80 0.047(2) 0.0257(19) 0.0279(19) 0.0048(15) -0.0063(18) -0.0034(17) C81 0.071(3) 0.034(2) 0.034(2) -0.0013(18) 0.002(2) -0.001(2) C82 0.116(5) 0.041(3) 0.040(3) -0.008(2) -0.002(3) -0.007(3) C83 0.095(5) 0.051(3) 0.056(4) 0.001(3) -0.034(3) -0.002(3) C84 0.057(3) 0.062(3) 0.058(3) 0.003(3) -0.023(3) -0.006(3) C85 0.047(3) 0.038(2) 0.043(3) 0.006(2) -0.008(2) -0.003(2) C90 0.038(2) 0.045(2) 0.034(2) 0.0125(19) 0.0142(18) 0.0106(19) C91 0.035(2) 0.064(3) 0.062(3) 0.022(3) 0.015(2) 0.006(2) C92 0.046(3) 0.099(5) 0.077(4) 0.033(4) 0.027(3) 0.023(3) C93 0.076(4) 0.108(6) 0.070(4) 0.035(4) 0.045(4) 0.054(4) C94 0.102(5) 0.063(3) 0.034(3) 0.005(2) 0.019(3) 0.045(3) C95 0.065(3) 0.046(3) 0.028(2) 0.0067(19) 0.013(2) 0.020(2) C100 0.029(12) 0.084(16) 0.029(14) -0.013(10) 0.002(10) -0.010(10) C101 0.087(14) 0.045(8) 0.042(7) -0.012(6) -0.015(7) 0.022(8) C102 0.076(10) 0.026(7) 0.081(13) -0.007(7) 0.000(7) 0.020(5) C103 0.114(18) 0.079(17) 0.103(19) -0.048(14) 0.047(15) -0.016(12) C104 0.26(3) 0.056(9) 0.068(11) -0.026(8) 0.072(15) -0.006(15) C105 0.30(3) 0.035(7) 0.040(8) -0.003(6) 0.058(14) -0.011(12) C100 0.035(12) 0.006(5) 0.035(13) 0.000(6) 0.013(9) -0.003(6) C101 0.034(7) 0.040(6) 0.047(7) 0.007(5) 0.016(5) -0.004(5) C102 0.091(13) 0.048(9) 0.056(10) 0.005(7) 0.027(8) -0.016(8) C103 0.050(7) 0.022(6) 0.041(7) -0.009(5) 0.018(5) -0.002(5) C104 0.035(5) 0.039(5) 0.038(5) -0.006(4) 0.011(4) 0.001(4) C105 0.035(5) 0.035(5) 0.039(6) -0.006(4) 0.008(4) -0.005(4) C110 0.020(5) 0.076(12) 0.032(7) 0.021(8) -0.001(5) -0.015(7) C111 0.033(7) 0.084(12) 0.053(8) 0.019(8) 0.003(6) 0.002(7) C112 0.014(7) 0.19(3) 0.062(10) 0.029(14) -0.010(6) -0.022(10) C113 0.060(11) 0.17(2) 0.060(10) 0.023(12) -0.019(8) -0.081(13) C114 0.094(13) 0.072(11) 0.041(7) -0.006(7) 0.012(8) -0.041(9) C115 0.038(7) 0.045(7) 0.031(5) 0.006(5) 0.007(6) -0.015(6) C110 0.030(7) 0.047(6) 0.022(5) 0.011(4) -0.004(5) -0.006(5) C111 0.022(5) 0.064(9) 0.043(6) 0.008(6) 0.000(4) 0.004(5) C112 0.034(7) 0.121(15) 0.077(11) 0.028(10) 0.004(7) 0.005(8) C113 0.064(12) 0.090(12) 0.065(11) 0.026(10) -0.015(9) -0.030(9) C114 0.083(12) 0.053(8) 0.037(7) -0.004(5) 0.002(7) -0.022(7) C115 0.032(6) 0.040(7) 0.032(6) 0.002(5) -0.001(6) -0.002(6) C1S 0.298(16) 0.098(7) 0.086(6) 0.001(5) -0.035(8) 0.001(8) C2S 0.042(7) 0.040(7) 0.102(14) -0.026(8) -0.004(9) -0.009(6) C3S 0.043(8) 0.054(7) 0.049(8) -0.020(7) 0.017(6) -0.010(6) C4S 0.186(12) 0.113(8) 0.288(18) 0.043(10) -0.115(12) -0.060(8) C5S 0.100(11) 1.80(14) 0.48(4) 0.76(7) 0.061(17) 0.01(3) C1P 0.298(16) 0.098(7) 0.086(6) 0.001(5) -0.035(8) 0.001(8) C2P 0.042(7) 0.040(7) 0.102(14) -0.026(8) -0.004(9) -0.009(6) C3P 0.043(8) 0.054(7) 0.049(8) -0.020(7) 0.017(6) -0.010(6) C4P 0.186(12) 0.113(8) 0.288(18) 0.043(10) -0.115(12) -0.060(8) C5P 0.100(11) 1.80(14) 0.48(4) 0.76(7) 0.061(17) 0.01(3) C10S 0.36(4) 0.078(12) 0.114(17) 0.012(12) -0.07(2) 0.11(2) C11S 0.127(11) 0.049(6) 0.026(4) 0.010(4) 0.026(6) -0.004(6) C12S 0.082(7) 0.037(5) 0.016(3) -0.004(3) 0.016(4) -0.006(4) C13S 0.22(2) 0.045(7) 0.102(12) 0.017(7) 0.125(14) 0.030(9) C20S 0.049(7) 0.144(14) 0.074(9) 0.007(9) 0.016(6) 0.031(8) C21S 0.20(2) 0.046(8) 0.32(4) 0.073(14) -0.12(2) -0.049(12) C22S 0.103(15) 0.33(4) 0.140(19) -0.08(2) 0.092(13) -0.067(19) C23S 0.10(2) 1.8(2) 0.17(3) -0.41(7) -0.08(2) 0.29(6) C30S 0.106(9) 0.163(12) 0.34(2) -0.049(15) -0.060(13) -0.006(8) C31S 0.101(8) 0.245(17) 0.172(12) -0.027(11) -0.011(8) 0.014(9) C32S 0.153(14) 0.76(6) 0.146(15) -0.04(2) 0.007(11) 0.10(2) C33S 0.086(15) 0.104(16) 0.057(10) 0.006(10) -0.032(10) 0.018(12) C34S 0.079(12) 0.071(11) 0.071(11) -0.003(8) -0.006(9) -0.012(8) C30P 0.106(9) 0.163(12) 0.34(2) -0.049(15) -0.060(13) -0.006(8) C31P 0.101(8) 0.245(17) 0.172(12) -0.027(11) -0.011(8) 0.014(9) C32P 0.153(14) 0.76(6) 0.146(15) -0.04(2) 0.007(11) 0.10(2) C33P 0.086(15) 0.104(16) 0.057(10) 0.006(10) -0.032(10) 0.018(12) C34P 0.079(12) 0.071(11) 0.071(11) -0.003(8) -0.006(9) -0.012(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 S2 2.1907(11) . ? Ni1 S3 2.1929(12) . ? Ni1 S1 2.2004(11) 2_556 ? Ni1 S1 2.2079(12) . ? Ni1 Ni1 2.8301(10) 2_556 ? Ni2 S3 2.2005(11) . ? Ni2 S5 2.2046(12) . ? Ni2 S2 2.2077(11) . ? Ni2 S4 2.2166(11) . ? Ni2 Ni3 2.8680(8) . ? Ni3 S5 2.2008(12) . ? Ni3 S6 2.2016(12) . ? Ni3 S4 2.2116(12) . ? Ni3 S7 2.2116(12) . ? Ni3 Ni4 2.8711(8) . ? Ni4 S8 2.1871(12) . ? Ni4 S9 2.2050(11) . ? Ni4 S6 2.2067(11) . ? Ni4 S7 2.2071(12) . ? Ni5 S9 2.1952(11) . ? Ni5 S8 2.1991(10) . ? Ni5 S11 2.2010(11) . ? Ni5 S10 2.2166(11) . ? Ni5 Ni6 2.9617(6) . ? Ni6 S11 2.1933(10) . ? Ni6 S11 2.1933(10) 2_556 ? Ni6 S10 2.2234(10) . ? Ni6 S10 2.2234(10) 2_556 ? Ni6 Ni5 2.9617(6) 2_556 ? S1 C10 1.769(2) . ? S1 Ni1 2.2004(11) 2_556 ? S2 C20 1.785(2) . ? S3 C30 1.776(2) . ? S4 C40 1.792(2) . ? S5 C50 1.782(3) . ? S6 C60 1.780(2) . ? S7 C70 1.625(12) . ? S7 C70 1.880(8) . ? S8 C80 1.776(2) . ? S9 C90 1.776(2) . ? S10 C100 1.761(9) . ? S10 C100 1.803(7) . ? S11 C110 1.721(8) . ? S11 C110 1.887(9) . ? C10 C11 1.3900 . ? C10 C15 1.3900 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C20 C21 1.3900 . ? C20 C25 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C30 C31 1.3900 . ? C30 C35 1.3900 . ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C40 C41 1.3900 . ? C40 C45 1.3900 . ? C41 C42 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C50 C51 1.3900 . ? C50 C55 1.3900 . ? C51 C52 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C60 C61 1.3900 . ? C60 C65 1.3900 . ? C61 C62 1.3900 . ? C62 C63 1.3900 . ? C63 C64 1.3900 . ? C64 C65 1.3900 . ? C70 C71 1.3900 . ? C70 C75 1.3900 . ? C71 C72 1.3900 . ? C72 C73 1.3900 . ? C73 C74 1.3900 . ? C74 C75 1.3900 . ? C70 C71 1.3900 . ? C70 C75 1.3900 . ? C71 C72 1.3900 . ? C72 C73 1.3900 . ? C73 C74 1.3900 . ? C74 C75 1.3900 . ? C80 C81 1.3900 . ? C80 C85 1.3900 . ? C81 C82 1.3900 . ? C82 C83 1.3900 . ? C83 C84 1.3900 . ? C84 C85 1.3900 . ? C90 C91 1.3900 . ? C90 C95 1.3900 . ? C91 C92 1.3900 . ? C92 C93 1.3900 . ? C93 C94 1.3900 . ? C94 C95 1.3900 . ? C100 C101 1.3900 . ? C100 C105 1.3900 . ? C101 C102 1.3900 . ? C102 C103 1.3900 . ? C103 C104 1.3900 . ? C104 C105 1.3900 . ? C100 C101 1.3900 . ? C100 C105 1.3900 . ? C101 C102 1.3900 . ? C102 C103 1.3900 . ? C103 C104 1.3900 . ? C104 C105 1.3900 . ? C110 C111 1.3900 . ? C110 C115 1.3900 . ? C111 C112 1.3900 . ? C112 C113 1.3900 . ? C113 C114 1.3900 . ? C114 C115 1.3900 . ? C110 C111 1.3900 . ? C110 C115 1.3900 . ? C111 C112 1.3900 . ? C112 C113 1.3900 . ? C113 C114 1.3900 . ? C114 C115 1.3900 . ? C1S C5S 1.536(11) . ? C1S C3S 1.638(15) . ? C2S C5S 1.526(16) . ? C2S C4S 1.584(15) . ? C3S C4S 1.607(16) . ? C10S C11S 1.038(16) 2_556 ? C10S C13S 1.093(18) 2_556 ? C10S C12S 1.524(9) 2_556 ? C10S C10S 1.66(2) 2_556 ? C11S C13S 1.511(8) . ? C11S C12S 1.547(9) 2_556 ? C12S C13S 1.507(9) . ? C12S C10S 1.524(9) 2_556 ? C20S C22S 1.501(9) . ? C20S C21S 1.553(9) . ? C21S C23S 1.01(3) 2_556 ? C22S C22S 1.518(10) 2_556 ? C23S C20S 1.01(3) 2_556 ? C23S C21S 1.01(3) 2_556 ? C23S C22S 1.564(10) 2_556 ? C23S C23S 1.80(3) 2_556 ? C30S C31S 1.528(11) . ? C30S C32S 1.532(12) . ? C31S C34S 1.499(16) . ? C32S C33S 1.499(17) . ? C33S C34S 1.524(18) . ? C33P C34P 1.471(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Ni1 S3 83.55(4) . . ? S2 Ni1 S1 176.77(5) . 2_556 ? S3 Ni1 S1 99.67(4) . 2_556 ? S2 Ni1 S1 99.07(4) . . ? S3 Ni1 S1 176.01(4) . . ? S1 Ni1 S1 77.71(5) 2_556 . ? S2 Ni1 Ni1 127.61(4) . 2_556 ? S3 Ni1 Ni1 126.07(4) . 2_556 ? S1 Ni1 Ni1 50.18(3) 2_556 2_556 ? S1 Ni1 Ni1 49.94(3) . 2_556 ? S3 Ni2 S5 100.26(4) . . ? S3 Ni2 S2 82.98(4) . . ? S5 Ni2 S2 173.23(5) . . ? S3 Ni2 S4 175.69(5) . . ? S5 Ni2 S4 82.49(4) . . ? S2 Ni2 S4 93.94(4) . . ? S3 Ni2 Ni3 130.19(4) . . ? S5 Ni2 Ni3 49.33(3) . . ? S2 Ni2 Ni3 124.18(3) . . ? S4 Ni2 Ni3 49.56(3) . . ? S5 Ni3 S6 173.78(5) . . ? S5 Ni3 S4 82.69(4) . . ? S6 Ni3 S4 96.88(5) . . ? S5 Ni3 S7 97.99(5) . . ? S6 Ni3 S7 82.28(4) . . ? S4 Ni3 S7 178.36(5) . . ? S5 Ni3 Ni2 49.44(3) . . ? S6 Ni3 Ni2 126.02(4) . . ? S4 Ni3 Ni2 49.71(3) . . ? S7 Ni3 Ni2 129.80(4) . . ? S5 Ni3 Ni4 126.52(4) . . ? S6 Ni3 Ni4 49.44(3) . . ? S4 Ni3 Ni4 129.03(4) . . ? S7 Ni3 Ni4 49.41(3) . . ? Ni2 Ni3 Ni4 114.41(2) . . ? S8 Ni4 S9 81.62(4) . . ? S8 Ni4 S6 100.74(4) . . ? S9 Ni4 S6 173.96(4) . . ? S8 Ni4 S7 175.04(5) . . ? S9 Ni4 S7 95.01(4) . . ? S6 Ni4 S7 82.27(5) . . ? S8 Ni4 Ni3 129.94(3) . . ? S9 Ni4 Ni3 125.08(3) . . ? S6 Ni4 Ni3 49.28(3) . . ? S7 Ni4 Ni3 49.55(3) . . ? S9 Ni5 S8 81.57(4) . . ? S9 Ni5 S11 97.60(4) . . ? S8 Ni5 S11 171.50(5) . . ? S9 Ni5 S10 178.15(5) . . ? S8 Ni5 S10 97.33(4) . . ? S11 Ni5 S10 83.27(4) . . ? S9 Ni5 Ni6 131.46(3) . . ? S8 Ni5 Ni6 127.58(3) . . ? S11 Ni5 Ni6 47.51(3) . . ? S10 Ni5 Ni6 48.26(3) . . ? S11 Ni6 S11 179.35(7) . 2_556 ? S11 Ni6 S10 83.29(4) . . ? S11 Ni6 S10 96.72(4) 2_556 . ? S11 Ni6 S10 96.72(4) . 2_556 ? S11 Ni6 S10 83.29(4) 2_556 2_556 ? S10 Ni6 S10 178.59(6) . 2_556 ? S11 Ni6 Ni5 47.74(3) . . ? S11 Ni6 Ni5 131.88(3) 2_556 . ? S10 Ni6 Ni5 48.06(3) . . ? S10 Ni6 Ni5 132.77(3) 2_556 . ? S11 Ni6 Ni5 131.88(3) . 2_556 ? S11 Ni6 Ni5 47.73(3) 2_556 2_556 ? S10 Ni6 Ni5 132.77(3) . 2_556 ? S10 Ni6 Ni5 48.06(3) 2_556 2_556 ? Ni5 Ni6 Ni5 128.09(3) . 2_556 ? C10 S1 Ni1 116.04(11) . 2_556 ? C10 S1 Ni1 115.79(12) . . ? Ni1 S1 Ni1 79.88(4) 2_556 . ? C20 S2 Ni1 106.50(10) . . ? C20 S2 Ni2 106.54(11) . . ? Ni1 S2 Ni2 94.11(4) . . ? C30 S3 Ni1 107.13(11) . . ? C30 S3 Ni2 107.27(12) . . ? Ni1 S3 Ni2 94.25(4) . . ? C40 S4 Ni3 107.05(11) . . ? C40 S4 Ni2 103.79(12) . . ? Ni3 S4 Ni2 80.73(4) . . ? C50 S5 Ni3 112.37(12) . . ? C50 S5 Ni2 111.61(13) . . ? Ni3 S5 Ni2 81.23(4) . . ? C60 S6 Ni3 111.82(10) . . ? C60 S6 Ni4 111.93(10) . . ? Ni3 S6 Ni4 81.28(4) . . ? C70 S7 C70 10.6(11) . . ? C70 S7 Ni4 110.5(8) . . ? C70 S7 Ni4 102.6(3) . . ? C70 S7 Ni3 111.9(8) . . ? C70 S7 Ni3 104.2(3) . . ? Ni4 S7 Ni3 81.05(4) . . ? C80 S8 Ni4 110.04(11) . . ? C80 S8 Ni5 113.66(11) . . ? Ni4 S8 Ni5 94.16(4) . . ? C90 S9 Ni5 108.44(11) . . ? C90 S9 Ni4 109.42(11) . . ? Ni5 S9 Ni4 93.77(4) . . ? C100 S10 C100 1.8(7) . . ? C100 S10 Ni5 105.7(4) . . ? C100 S10 Ni5 103.9(3) . . ? C100 S10 Ni6 103.9(4) . . ? C100 S10 Ni6 103.8(4) . . ? Ni5 S10 Ni6 83.68(4) . . ? C110 S11 C110 13.5(6) . . ? C110 S11 Ni6 115.8(5) . . ? C110 S11 Ni6 104.7(4) . . ? C110 S11 Ni5 110.9(5) . . ? C110 S11 Ni5 103.5(5) . . ? Ni6 S11 Ni5 84.75(4) . . ? C11 C10 C15 120.0 . . ? C11 C10 S1 116.21(18) . . ? C15 C10 S1 123.79(18) . . ? C10 C11 C12 120.0 . . ? C11 C12 C13 120.0 . . ? C14 C13 C12 120.0 . . ? C15 C14 C13 120.0 . . ? C14 C15 C10 120.0 . . ? C21 C20 C25 120.0 . . ? C21 C20 S2 121.59(15) . . ? C25 C20 S2 118.41(15) . . ? C20 C21 C22 120.0 . . ? C21 C22 C23 120.0 . . ? C22 C23 C24 120.0 . . ? C25 C24 C23 120.0 . . ? C24 C25 C20 120.0 . . ? C31 C30 C35 120.0 . . ? C31 C30 S3 118.49(18) . . ? C35 C30 S3 121.37(18) . . ? C32 C31 C30 120.0 . . ? C31 C32 C33 120.0 . . ? C34 C33 C32 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C30 120.0 . . ? C41 C40 C45 120.0 . . ? C41 C40 S4 118.81(17) . . ? C45 C40 S4 121.02(18) . . ? C40 C41 C42 120.0 . . ? C43 C42 C41 120.0 . . ? C42 C43 C44 120.0 . . ? C45 C44 C43 120.0 . . ? C44 C45 C40 120.0 . . ? C51 C50 C55 120.0 . . ? C51 C50 S5 117.3(2) . . ? C55 C50 S5 122.7(2) . . ? C50 C51 C52 120.0 . . ? C51 C52 C53 120.0 . . ? C54 C53 C52 120.0 . . ? C53 C54 C55 120.0 . . ? C54 C55 C50 120.0 . . ? C61 C60 C65 120.0 . . ? C61 C60 S6 117.77(16) . . ? C65 C60 S6 122.23(16) . . ? C60 C61 C62 120.0 . . ? C63 C62 C61 120.0 . . ? C62 C63 C64 120.0 . . ? C65 C64 C63 120.0 . . ? C64 C65 C60 120.0 . . ? C71 C70 C75 120.0 . . ? C71 C70 S7 120.0(4) . . ? C75 C70 S7 119.9(4) . . ? C72 C71 C70 120.0 . . ? C71 C72 C73 120.0 . . ? C72 C73 C74 120.0 . . ? C75 C74 C73 120.0 . . ? C74 C75 C70 120.0 . . ? C71 C70 C75 120.0 . . ? C71 C70 S7 121.9(9) . . ? C75 C70 S7 118.1(9) . . ? C72 C71 C70 120.0 . . ? C71 C72 C73 120.0 . . ? C72 C73 C74 120.0 . . ? C75 C74 C73 120.0 . . ? C74 C75 C70 120.0 . . ? C81 C80 C85 120.0 . . ? C81 C80 S8 122.92(17) . . ? C85 C80 S8 116.85(17) . . ? C82 C81 C80 120.0 . . ? C81 C82 C83 120.0 . . ? C84 C83 C82 120.0 . . ? C83 C84 C85 120.0 . . ? C84 C85 C80 120.0 . . ? C91 C90 C95 120.0 . . ? C91 C90 S9 117.55(18) . . ? C95 C90 S9 122.32(18) . . ? C90 C91 C92 120.0 . . ? C93 C92 C91 120.0 . . ? C92 C93 C94 120.0 . . ? C95 C94 C93 120.0 . . ? C94 C95 C90 120.0 . . ? C101 C100 C105 120.0 . . ? C101 C100 S10 125.3(7) . . ? C105 C100 S10 114.3(7) . . ? C102 C101 C100 120.0 . . ? C101 C102 C103 120.0 . . ? C104 C103 C102 120.0 . . ? C103 C104 C105 120.0 . . ? C104 C105 C100 120.0 . . ? C101 C100 C105 120.0 . . ? C101 C100 S10 118.9(6) . . ? C105 C100 S10 120.9(6) . . ? C100 C101 C102 120.0 . . ? C103 C102 C101 120.0 . . ? C102 C103 C104 120.0 . . ? C105 C104 C103 120.0 . . ? C104 C105 C100 120.0 . . ? C111 C110 C115 120.0 . . ? C111 C110 S11 115.7(6) . . ? C115 C110 S11 124.2(6) . . ? C110 C111 C112 120.0 . . ? C113 C112 C111 120.0 . . ? C112 C113 C114 120.0 . . ? C113 C114 C115 120.0 . . ? C114 C115 C110 120.0 . . ? C111 C110 C115 120.0 . . ? C111 C110 S11 120.1(6) . . ? C115 C110 S11 119.9(6) . . ? C112 C111 C110 120.0 . . ? C111 C112 C113 120.0 . . ? C112 C113 C114 120.0 . . ? C115 C114 C113 120.0 . . ? C114 C115 C110 120.0 . . ? C5S C1S C3S 94.9(9) . . ? C5S C2S C4S 106.5(9) . . ? C4S C3S C1S 96.0(9) . . ? C3S C4S C2S 100.9(9) . . ? C2S C5S C1S 102.0(9) . . ? C11S C10S C13S 90.3(16) 2_556 2_556 ? C11S C10S C12S 139.5(17) 2_556 2_556 ? C13S C10S C12S 68.0(7) 2_556 2_556 ? C11S C10S C10S 127.7(11) 2_556 2_556 ? C13S C10S C10S 124.4(10) 2_556 2_556 ? C12S C10S C10S 56.7(6) 2_556 2_556 ? C13S C11S C12S 108.7(6) . 2_556 ? C13S C12S C10S 42.3(7) . 2_556 ? C12S C13S C11S 106.0(7) . . ? C22S C20S C21S 99.6(7) . . ? C23S C21S C20S 39.7(15) 2_556 . ? C20S C22S C22S 115.6(11) . 2_556 ? C20S C23S C21S 100(2) 2_556 2_556 ? C20S C23S C22S 67.5(9) 2_556 2_556 ? C21S C23S C22S 129(2) 2_556 2_556 ? C20S C23S C23S 121(2) 2_556 2_556 ? C21S C23S C23S 58.4(15) 2_556 2_556 ? C22S C23S C23S 84.8(6) 2_556 2_556 ? C31S C30S C32S 104.5(7) . . ? C34S C31S C30S 107.4(9) . . ? C33S C32S C30S 109.3(9) . . ? C32S C33S C34S 105.4(11) . . ? C31S C34S C33S 105.9(12) . . ? 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 S3 Ni2 Ni3 S5 -65.25(6) . . . . ? S2 Ni2 Ni3 S5 -177.61(6) . . . . ? S4 Ni2 Ni3 S5 120.40(6) . . . . ? S3 Ni2 Ni3 S6 109.32(6) . . . . ? S5 Ni2 Ni3 S6 174.57(6) . . . . ? S2 Ni2 Ni3 S6 -3.04(6) . . . . ? S4 Ni2 Ni3 S6 -65.03(5) . . . . ? S3 Ni2 Ni3 S4 174.35(6) . . . . ? S5 Ni2 Ni3 S4 -120.40(6) . . . . ? S2 Ni2 Ni3 S4 61.99(5) . . . . ? S3 Ni2 Ni3 S7 -3.61(7) . . . . ? S5 Ni2 Ni3 S7 61.64(6) . . . . ? S2 Ni2 Ni3 S7 -115.97(6) . . . . ? S4 Ni2 Ni3 S7 -177.96(6) . . . . ? S3 Ni2 Ni3 Ni4 52.89(5) . . . . ? S5 Ni2 Ni3 Ni4 118.14(4) . . . . ? S2 Ni2 Ni3 Ni4 -59.47(5) . . . . ? S4 Ni2 Ni3 Ni4 -121.46(5) . . . . ? S5 Ni3 Ni4 S8 107.53(6) . . . . ? S6 Ni3 Ni4 S8 -66.42(6) . . . . ? S4 Ni3 Ni4 S8 -5.83(7) . . . . ? S7 Ni3 Ni4 S8 173.54(6) . . . . ? Ni2 Ni3 Ni4 S8 51.07(5) . . . . ? S5 Ni3 Ni4 S9 -3.30(6) . . . . ? S6 Ni3 Ni4 S9 -177.25(6) . . . . ? S4 Ni3 Ni4 S9 -116.65(6) . . . . ? S7 Ni3 Ni4 S9 62.71(6) . . . . ? Ni2 Ni3 Ni4 S9 -59.76(5) . . . . ? S5 Ni3 Ni4 S6 173.95(6) . . . . ? S4 Ni3 Ni4 S6 60.60(6) . . . . ? S7 Ni3 Ni4 S6 -120.04(6) . . . . ? Ni2 Ni3 Ni4 S6 117.49(5) . . . . ? S5 Ni3 Ni4 S7 -66.01(6) . . . . ? S6 Ni3 Ni4 S7 120.04(6) . . . . ? S4 Ni3 Ni4 S7 -179.36(6) . . . . ? Ni2 Ni3 Ni4 S7 -122.47(5) . . . . ? S9 Ni5 Ni6 S11 -55.26(6) . . . . ? S8 Ni5 Ni6 S11 -170.92(6) . . . . ? S10 Ni5 Ni6 S11 127.18(6) . . . . ? S9 Ni5 Ni6 S11 124.03(6) . . . 2_556 ? S8 Ni5 Ni6 S11 8.37(7) . . . 2_556 ? S11 Ni5 Ni6 S11 179.29(7) . . . 2_556 ? S10 Ni5 Ni6 S11 -53.53(5) . . . 2_556 ? S9 Ni5 Ni6 S10 177.56(6) . . . . ? S8 Ni5 Ni6 S10 61.90(5) . . . . ? S11 Ni5 Ni6 S10 -127.18(6) . . . . ? S9 Ni5 Ni6 S10 -3.98(7) . . . 2_556 ? S8 Ni5 Ni6 S10 -119.63(6) . . . 2_556 ? S11 Ni5 Ni6 S10 51.29(6) . . . 2_556 ? S10 Ni5 Ni6 S10 178.47(7) . . . 2_556 ? S9 Ni5 Ni6 Ni5 60.45(4) . . . 2_556 ? S8 Ni5 Ni6 Ni5 -55.21(4) . . . 2_556 ? S11 Ni5 Ni6 Ni5 115.71(4) . . . 2_556 ? S10 Ni5 Ni6 Ni5 -117.11(4) . . . 2_556 ? S2 Ni1 S1 C10 18.18(13) . . . . ? S3 Ni1 S1 C10 -112.7(7) . . . . ? S1 Ni1 S1 C10 -161.84(12) 2_556 . . . ? Ni1 Ni1 S1 C10 -114.15(13) 2_556 . . . ? S2 Ni1 S1 Ni1 132.32(4) . . . 2_556 ? S3 Ni1 S1 Ni1 1.5(7) . . . 2_556 ? S1 Ni1 S1 Ni1 -47.69(5) 2_556 . . 2_556 ? S3 Ni1 S2 C20 -125.63(12) . . . . ? S1 Ni1 S2 C20 57.2(9) 2_556 . . . ? S1 Ni1 S2 C20 57.41(12) . . . . ? Ni1 Ni1 S2 C20 103.00(11) 2_556 . . . ? S3 Ni1 S2 Ni2 -17.03(4) . . . . ? S1 Ni1 S2 Ni2 165.8(8) 2_556 . . . ? S1 Ni1 S2 Ni2 166.01(4) . . . . ? Ni1 Ni1 S2 Ni2 -148.40(3) 2_556 . . . ? S3 Ni2 S2 C20 125.55(10) . . . . ? S5 Ni2 S2 C20 -115.4(4) . . . . ? S4 Ni2 S2 C20 -57.49(10) . . . . ? Ni3 Ni2 S2 C20 -99.82(10) . . . . ? S3 Ni2 S2 Ni1 16.99(4) . . . . ? S5 Ni2 S2 Ni1 136.1(4) . . . . ? S4 Ni2 S2 Ni1 -166.05(4) . . . . ? Ni3 Ni2 S2 Ni1 151.61(3) . . . . ? S2 Ni1 S3 C30 126.62(12) . . . . ? S1 Ni1 S3 C30 -53.54(12) 2_556 . . . ? S1 Ni1 S3 C30 -102.1(7) . . . . ? Ni1 Ni1 S3 C30 -100.72(12) 2_556 . . . ? S2 Ni1 S3 Ni2 17.09(4) . . . . ? S1 Ni1 S3 Ni2 -163.07(4) 2_556 . . . ? S1 Ni1 S3 Ni2 148.4(6) . . . . ? Ni1 Ni1 S3 Ni2 149.74(3) 2_556 . . . ? S5 Ni2 S3 C30 59.63(12) . . . . ? S2 Ni2 S3 C30 -126.38(12) . . . . ? S4 Ni2 S3 C30 -171.1(6) . . . . ? Ni3 Ni2 S3 C30 104.05(12) . . . . ? S5 Ni2 S3 Ni1 169.03(4) . . . . ? S2 Ni2 S3 Ni1 -16.97(4) . . . . ? S4 Ni2 S3 Ni1 -61.7(6) . . . . ? Ni3 Ni2 S3 Ni1 -146.54(3) . . . . ? S5 Ni3 S4 C40 60.34(12) . . . . ? S6 Ni3 S4 C40 -125.92(12) . . . . ? S7 Ni3 S4 C40 175(69) . . . . ? Ni2 Ni3 S4 C40 101.69(13) . . . . ? Ni4 Ni3 S4 C40 -167.72(12) . . . . ? S5 Ni3 S4 Ni2 -41.35(4) . . . . ? S6 Ni3 S4 Ni2 132.39(4) . . . . ? S7 Ni3 S4 Ni2 73.4(19) . . . . ? Ni4 Ni3 S4 Ni2 90.59(4) . . . . ? S3 Ni2 S4 C40 166.0(6) . . . . ? S5 Ni2 S4 C40 -64.13(11) . . . . ? S2 Ni2 S4 C40 121.64(11) . . . . ? Ni3 Ni2 S4 C40 -105.42(11) . . . . ? S3 Ni2 S4 Ni3 -88.5(6) . . . . ? S5 Ni2 S4 Ni3 41.29(4) . . . . ? S2 Ni2 S4 Ni3 -132.94(4) . . . . ? S6 Ni3 S5 C50 65.0(5) . . . . ? S4 Ni3 S5 C50 151.40(14) . . . . ? S7 Ni3 S5 C50 -27.10(14) . . . . ? Ni2 Ni3 S5 C50 109.85(14) . . . . ? Ni4 Ni3 S5 C50 17.38(14) . . . . ? S6 Ni3 S5 Ni2 -44.9(4) . . . . ? S4 Ni3 S5 Ni2 41.55(4) . . . . ? S7 Ni3 S5 Ni2 -136.94(4) . . . . ? Ni4 Ni3 S5 Ni2 -92.47(4) . . . . ? S3 Ni2 S5 C50 24.50(14) . . . . ? S2 Ni2 S5 C50 -93.7(4) . . . . ? S4 Ni2 S5 C50 -152.13(13) . . . . ? Ni3 Ni2 S5 C50 -110.67(14) . . . . ? S3 Ni2 S5 Ni3 135.17(4) . . . . ? S2 Ni2 S5 Ni3 17.0(4) . . . . ? S4 Ni2 S5 Ni3 -41.46(4) . . . . ? S5 Ni3 S6 C60 58.8(5) . . . . ? S4 Ni3 S6 C60 -26.81(11) . . . . ? S7 Ni3 S6 C60 151.77(11) . . . . ? Ni2 Ni3 S6 C60 17.34(11) . . . . ? Ni4 Ni3 S6 C60 110.22(11) . . . . ? S5 Ni3 S6 Ni4 -51.4(4) . . . . ? S4 Ni3 S6 Ni4 -137.03(4) . . . . ? S7 Ni3 S6 Ni4 41.56(4) . . . . ? Ni2 Ni3 S6 Ni4 -92.88(4) . . . . ? S8 Ni4 S6 C60 24.24(11) . . . . ? S9 Ni4 S6 C60 -88.2(5) . . . . ? S7 Ni4 S6 C60 -151.76(11) . . . . ? Ni3 Ni4 S6 C60 -110.10(11) . . . . ? S8 Ni4 S6 Ni3 134.34(4) . . . . ? S9 Ni4 S6 Ni3 21.9(5) . . . . ? S7 Ni4 S6 Ni3 -41.66(4) . . . . ? S8 Ni4 S7 C70 163.8(10) . . . . ? S9 Ni4 S7 C70 116.8(9) . . . . ? S6 Ni4 S7 C70 -68.6(9) . . . . ? Ni3 Ni4 S7 C70 -110.1(9) . . . . ? S8 Ni4 S7 C70 171.2(6) . . . . ? S9 Ni4 S7 C70 124.3(3) . . . . ? S6 Ni4 S7 C70 -61.2(3) . . . . ? Ni3 Ni4 S7 C70 -102.6(3) . . . . ? S8 Ni4 S7 Ni3 -86.1(5) . . . . ? S9 Ni4 S7 Ni3 -133.11(4) . . . . ? S6 Ni4 S7 Ni3 41.46(4) . . . . ? S5 Ni3 S7 C70 -119.3(8) . . . . ? S6 Ni3 S7 C70 67.0(8) . . . . ? S4 Ni3 S7 C70 126(2) . . . . ? Ni2 Ni3 S7 C70 -161.8(8) . . . . ? Ni4 Ni3 S7 C70 108.5(8) . . . . ? S5 Ni3 S7 C70 -127.0(3) . . . . ? S6 Ni3 S7 C70 59.2(3) . . . . ? S4 Ni3 S7 C70 118.4(19) . . . . ? Ni2 Ni3 S7 C70 -169.5(3) . . . . ? Ni4 Ni3 S7 C70 100.8(3) . . . . ? S5 Ni3 S7 Ni4 132.14(4) . . . . ? S6 Ni3 S7 Ni4 -41.58(4) . . . . ? S4 Ni3 S7 Ni4 17.6(19) . . . . ? Ni2 Ni3 S7 Ni4 89.68(5) . . . . ? S9 Ni4 S8 C80 -139.39(11) . . . . ? S6 Ni4 S8 C80 46.26(11) . . . . ? S7 Ni4 S8 C80 173.2(5) . . . . ? Ni3 Ni4 S8 C80 91.25(11) . . . . ? S9 Ni4 S8 Ni5 -22.34(4) . . . . ? S6 Ni4 S8 Ni5 163.30(4) . . . . ? S7 Ni4 S8 Ni5 -69.7(5) . . . . ? Ni3 Ni4 S8 Ni5 -151.70(3) . . . . ? S9 Ni5 S8 C80 136.46(12) . . . . ? S11 Ni5 S8 C80 -138.5(3) . . . . ? S10 Ni5 S8 C80 -45.03(12) . . . . ? Ni6 Ni5 S8 C80 -86.61(12) . . . . ? S9 Ni5 S8 Ni4 22.45(4) . . . . ? S11 Ni5 S8 Ni4 107.5(3) . . . . ? S10 Ni5 S8 Ni4 -159.05(4) . . . . ? Ni6 Ni5 S8 Ni4 159.38(3) . . . . ? S8 Ni5 S9 C90 -134.16(12) . . . . ? S11 Ni5 S9 C90 54.39(12) . . . . ? S10 Ni5 S9 C90 173(24) . . . . ? Ni6 Ni5 S9 C90 92.07(12) . . . . ? S8 Ni5 S9 Ni4 -22.24(4) . . . . ? S11 Ni5 S9 Ni4 166.30(4) . . . . ? S10 Ni5 S9 Ni4 -75.6(14) . . . . ? Ni6 Ni5 S9 Ni4 -156.01(3) . . . . ? S8 Ni4 S9 C90 133.43(11) . . . . ? S6 Ni4 S9 C90 -113.2(4) . . . . ? S7 Ni4 S9 C90 -50.24(12) . . . . ? Ni3 Ni4 S9 C90 -92.99(11) . . . . ? S8 Ni4 S9 Ni5 22.37(4) . . . . ? S6 Ni4 S9 Ni5 135.7(4) . . . . ? S7 Ni4 S9 Ni5 -161.30(4) . . . . ? Ni3 Ni4 S9 Ni5 155.95(3) . . . . ? S9 Ni5 S10 C100 175(56) . . . . ? S8 Ni5 S10 C100 122.1(4) . . . . ? S11 Ni5 S10 C100 -66.4(4) . . . . ? Ni6 Ni5 S10 C100 -102.7(4) . . . . ? S9 Ni5 S10 C100 175(56) . . . . ? S8 Ni5 S10 C100 122.1(4) . . . . ? S11 Ni5 S10 C100 -66.4(4) . . . . ? Ni6 Ni5 S10 C100 -102.7(4) . . . . ? S9 Ni5 S10 Ni6 -82.1(14) . . . . ? S8 Ni5 S10 Ni6 -135.18(4) . . . . ? S11 Ni5 S10 Ni6 36.27(4) . . . . ? S11 Ni6 S10 C100 68.2(5) . . . . ? S11 Ni6 S10 C100 -112.4(5) 2_556 . . . ? S10 Ni6 S10 C100 -22.2(5) 2_556 . . . ? Ni5 Ni6 S10 C100 104.6(5) . . . . ? Ni5 Ni6 S10 C100 -148.0(5) 2_556 . . . ? S11 Ni6 S10 C100 66.4(3) . . . . ? S11 Ni6 S10 C100 -114.3(3) 2_556 . . . ? S10 Ni6 S10 C100 -24.0(3) 2_556 . . . ? Ni5 Ni6 S10 C100 102.8(3) . . . . ? Ni5 Ni6 S10 C100 -149.8(3) 2_556 . . . ? S11 Ni6 S10 Ni5 -36.42(4) . . . . ? S11 Ni6 S10 Ni5 142.93(4) 2_556 . . . ? S10 Ni6 S10 Ni5 -126.83(3) 2_556 . . . ? Ni5 Ni6 S10 Ni5 107.37(5) 2_556 . . . ? S11 Ni6 S11 C110 56.6(6) 2_556 . . . ? S10 Ni6 S11 C110 147.3(6) . . . . ? S10 Ni6 S11 C110 -34.1(6) 2_556 . . . ? Ni5 Ni6 S11 C110 110.7(6) . . . . ? Ni5 Ni6 S11 C110 2.9(6) 2_556 . . . ? S11 Ni6 S11 C110 48.5(5) 2_556 . . . ? S10 Ni6 S11 C110 139.3(5) . . . . ? S10 Ni6 S11 C110 -42.2(5) 2_556 . . . ? Ni5 Ni6 S11 C110 102.6(5) . . . . ? Ni5 Ni6 S11 C110 -5.1(5) 2_556 . . . ? S11 Ni6 S11 Ni5 -54.11(9) 2_556 . . . ? S10 Ni6 S11 Ni5 36.64(4) . . . . ? S10 Ni6 S11 Ni5 -144.78(4) 2_556 . . . ? Ni5 Ni6 S11 Ni5 -107.74(5) 2_556 . . . ? S9 Ni5 S11 C110 25.9(5) . . . . ? S8 Ni5 S11 C110 -57.9(6) . . . . ? S10 Ni5 S11 C110 -152.4(5) . . . . ? Ni6 Ni5 S11 C110 -115.7(5) . . . . ? S9 Ni5 S11 C110 37.7(4) . . . . ? S8 Ni5 S11 C110 -46.1(5) . . . . ? S10 Ni5 S11 C110 -140.6(4) . . . . ? Ni6 Ni5 S11 C110 -103.8(4) . . . . ? S9 Ni5 S11 Ni6 141.59(4) . . . . ? S8 Ni5 S11 Ni6 57.8(3) . . . . ? S10 Ni5 S11 Ni6 -36.77(4) . . . . ? Ni1 S1 C10 C11 132.23(16) 2_556 . . . ? Ni1 S1 C10 C11 -136.68(16) . . . . ? Ni1 S1 C10 C15 -47.2(2) 2_556 . . . ? Ni1 S1 C10 C15 43.9(2) . . . . ? C15 C10 C11 C12 0.0 . . . . ? S1 C10 C11 C12 -179.5(2) . . . . ? C10 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 C10 0.0 . . . . ? C11 C10 C15 C14 0.0 . . . . ? S1 C10 C15 C14 179.4(3) . . . . ? Ni1 S2 C20 C21 20.8(2) . . . . ? Ni2 S2 C20 C21 -78.76(19) . . . . ? Ni1 S2 C20 C25 -159.54(16) . . . . ? Ni2 S2 C20 C25 100.92(17) . . . . ? C25 C20 C21 C22 0.0 . . . . ? S2 C20 C21 C22 179.7(2) . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C20 0.0 . . . . ? C21 C20 C25 C24 0.0 . . . . ? S2 C20 C25 C24 -179.7(2) . . . . ? Ni1 S3 C30 C31 138.41(17) . . . . ? Ni2 S3 C30 C31 -121.39(17) . . . . ? Ni1 S3 C30 C35 -37.3(2) . . . . ? Ni2 S3 C30 C35 62.9(2) . . . . ? C35 C30 C31 C32 0.0 . . . . ? S3 C30 C31 C32 -175.8(3) . . . . ? C30 C31 C32 C33 0.0 . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C30 0.0 . . . . ? C31 C30 C35 C34 0.0 . . . . ? S3 C30 C35 C34 175.7(3) . . . . ? Ni3 S4 C40 C41 -138.67(17) . . . . ? Ni2 S4 C40 C41 -54.30(19) . . . . ? Ni3 S4 C40 C45 46.0(2) . . . . ? Ni2 S4 C40 C45 130.33(18) . . . . ? C45 C40 C41 C42 0.0 . . . . ? S4 C40 C41 C42 -175.4(3) . . . . ? C40 C41 C42 C43 0.0 . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 C40 0.0 . . . . ? C41 C40 C45 C44 0.0 . . . . ? S4 C40 C45 C44 175.3(3) . . . . ? Ni3 S5 C50 C51 135.93(18) . . . . ? Ni2 S5 C50 C51 -134.88(18) . . . . ? Ni3 S5 C50 C55 -47.1(3) . . . . ? Ni2 S5 C50 C55 42.1(3) . . . . ? C55 C50 C51 C52 0.0 . . . . ? S5 C50 C51 C52 177.1(3) . . . . ? C50 C51 C52 C53 0.0 . . . . ? C51 C52 C53 C54 0.0 . . . . ? C52 C53 C54 C55 0.0 . . . . ? C53 C54 C55 C50 0.0 . . . . ? C51 C50 C55 C54 0.0 . . . . ? S5 C50 C55 C54 -176.9(3) . . . . ? Ni3 S6 C60 C61 134.60(13) . . . . ? Ni4 S6 C60 C61 -136.25(14) . . . . ? Ni3 S6 C60 C65 -46.30(18) . . . . ? Ni4 S6 C60 C65 42.84(18) . . . . ? C65 C60 C61 C62 0.0 . . . . ? S6 C60 C61 C62 179.1(2) . . . . ? C60 C61 C62 C63 0.0 . . . . ? C61 C62 C63 C64 0.0 . . . . ? C62 C63 C64 C65 0.0 . . . . ? C63 C64 C65 C60 0.0 . . . . ? C61 C60 C65 C64 0.0 . . . . ? S6 C60 C65 C64 -179.1(2) . . . . ? C70 S7 C70 C71 -78(4) . . . . ? Ni4 S7 C70 C71 142.9(3) . . . . ? Ni3 S7 C70 C71 59.1(4) . . . . ? C70 S7 C70 C75 98(4) . . . . ? Ni4 S7 C70 C75 -41.0(6) . . . . ? Ni3 S7 C70 C75 -124.8(5) . . . . ? C75 C70 C71 C72 0.0 . . . . ? S7 C70 C71 C72 176.1(6) . . . . ? C70 C71 C72 C73 0.0 . . . . ? C71 C72 C73 C74 0.0 . . . . ? C72 C73 C74 C75 0.0 . . . . ? C73 C74 C75 C70 0.0 . . . . ? C71 C70 C75 C74 0.0 . . . . ? S7 C70 C75 C74 -176.1(6) . . . . ? C70 S7 C70 C71 87(4) . . . . ? Ni4 S7 C70 C71 130.0(8) . . . . ? Ni3 S7 C70 C71 41.7(11) . . . . ? C70 S7 C70 C75 -95(4) . . . . ? Ni4 S7 C70 C75 -51.5(13) . . . . ? Ni3 S7 C70 C75 -139.9(11) . . . . ? C75 C70 C71 C72 0.0 . . . . ? S7 C70 C71 C72 178.4(15) . . . . ? C70 C71 C72 C73 0.0 . . . . ? C71 C72 C73 C74 0.0 . . . . ? C72 C73 C74 C75 0.0 . . . . ? C73 C74 C75 C70 0.0 . . . . ? C71 C70 C75 C74 0.0 . . . . ? S7 C70 C75 C74 -178.5(15) . . . . ? Ni4 S8 C80 C81 27.9(2) . . . . ? Ni5 S8 C80 C81 -76.27(19) . . . . ? Ni4 S8 C80 C85 -146.62(14) . . . . ? Ni5 S8 C80 C85 109.25(16) . . . . ? C85 C80 C81 C82 0.0 . . . . ? S8 C80 C81 C82 -174.3(2) . . . . ? C80 C81 C82 C83 0.0 . . . . ? C81 C82 C83 C84 0.0 . . . . ? C82 C83 C84 C85 0.0 . . . . ? C83 C84 C85 C80 0.0 . . . . ? C81 C80 C85 C84 0.0 . . . . ? S8 C80 C85 C84 174.6(2) . . . . ? Ni5 S9 C90 C91 -157.13(14) . . . . ? Ni4 S9 C90 C91 101.86(16) . . . . ? Ni5 S9 C90 C95 18.8(2) . . . . ? Ni4 S9 C90 C95 -82.22(18) . . . . ? C95 C90 C91 C92 0.0 . . . . ? S9 C90 C91 C92 176.0(2) . . . . ? C90 C91 C92 C93 0.0 . . . . ? C91 C92 C93 C94 0.0 . . . . ? C92 C93 C94 C95 0.0 . . . . ? C93 C94 C95 C90 0.0 . . . . ? C91 C90 C95 C94 0.0 . . . . ? S9 C90 C95 C94 -175.8(2) . . . . ? C100 S10 C100 C101 108(25) . . . . ? Ni5 S10 C100 C101 107.1(8) . . . . ? Ni6 S10 C100 C101 19.9(9) . . . . ? C100 S10 C100 C105 -79(25) . . . . ? Ni5 S10 C100 C105 -80.0(6) . . . . ? Ni6 S10 C100 C105 -167.3(6) . . . . ? C105 C100 C101 C102 0.0 . . . . ? S10 C100 C101 C102 172.4(11) . . . . ? C100 C101 C102 C103 0.0 . . . . ? C101 C102 C103 C104 0.0 . . . . ? C102 C103 C104 C105 0.0 . . . . ? C103 C104 C105 C100 0.0 . . . . ? C101 C100 C105 C104 0.0 . . . . ? S10 C100 C105 C104 -173.2(10) . . . . ? C100 S10 C100 C101 -45(24) . . . . ? Ni5 S10 C100 C101 134.1(5) . . . . ? Ni6 S10 C100 C101 47.3(5) . . . . ? C100 S10 C100 C105 129(25) . . . . ? Ni5 S10 C100 C105 -51.4(5) . . . . ? Ni6 S10 C100 C105 -138.2(5) . . . . ? C105 C100 C101 C102 0.0 . . . . ? S10 C100 C101 C102 174.5(8) . . . . ? C100 C101 C102 C103 0.0 . . . . ? C101 C102 C103 C104 0.0 . . . . ? C102 C103 C104 C105 0.0 . . . . ? C103 C104 C105 C100 0.0 . . . . ? C101 C100 C105 C104 0.0 . . . . ? S10 C100 C105 C104 -174.4(8) . . . . ? C110 S11 C110 C111 3(4) . . . . ? Ni6 S11 C110 C111 150.0(7) . . . . ? Ni5 S11 C110 C111 -122.0(7) . . . . ? C110 S11 C110 C115 -179(100) . . . . ? Ni6 S11 C110 C115 -32.1(9) . . . . ? Ni5 S11 C110 C115 55.9(9) . . . . ? C115 C110 C111 C112 0.0 . . . . ? S11 C110 C111 C112 178.0(12) . . . . ? C110 C111 C112 C113 0.0 . . . . ? C111 C112 C113 C114 0.0 . . . . ? C112 C113 C114 C115 0.0 . . . . ? C113 C114 C115 C110 0.0 . . . . ? C111 C110 C115 C114 0.0 . . . . ? S11 C110 C115 C114 -177.8(13) . . . . ? C110 S11 C110 C111 178(5) . . . . ? Ni6 S11 C110 C111 142.8(7) . . . . ? Ni5 S11 C110 C111 -122.8(8) . . . . ? C110 S11 C110 C115 -3(4) . . . . ? Ni6 S11 C110 C115 -38.2(10) . . . . ? Ni5 S11 C110 C115 56.1(9) . . . . ? C115 C110 C111 C112 0.0 . . . . ? S11 C110 C111 C112 179.0(13) . . . . ? C110 C111 C112 C113 0.0 . . . . ? C111 C112 C113 C114 0.0 . . . . ? C112 C113 C114 C115 0.0 . . . . ? C113 C114 C115 C110 0.0 . . . . ? C111 C110 C115 C114 0.0 . . . . ? S11 C110 C115 C114 -179.0(13) . . . . ? C5S C1S C3S C4S -60.0(12) . . . . ? C1S C3S C4S C2S 42.7(16) . . . . ? C5S C2S C4S C3S -11(2) . . . . ? C4S C2S C5S C1S -28(2) . . . . ? C3S C1S C5S C2S 54.7(16) . . . . ? C10S C12S C13S C11S 24.3(10) 2_556 . . . ? C12S C11S C13S C12S -3.1(11) 2_556 . . . ? C22S C20S C21S C23S -50.6(18) . . . 2_556 ? C21S C20S C22S C22S -33(2) . . . 2_556 ? C32S C30S C31S C34S 18(2) . . . . ? C31S C30S C32S C33S -2(3) . . . . ? C30S C32S C33S C34S -15(4) . . . . ? C30S C31S C34S C33S -27(3) . . . . ? C32S C33S C34S C31S 26(4) . . . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 1.272 _refine_diff_density_min -0.872 _refine_diff_density_rms 0.228 data_n99080 _database_code_CSD 167795 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C152 H150 Ni11 O5 S22' _chemical_formula_weight 3407.85 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 '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 17.5354(18) _cell_length_b 19.518(2) _cell_length_c 24.994(3) _cell_angle_alpha 82.095(2) _cell_angle_beta 75.406(2) _cell_angle_gamma 72.380(2) _cell_volume 7872.5(15) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 7432 _cell_measurement_theta_min 1.66 _cell_measurement_theta_max 22.50 _exptl_crystal_description 'rhombic' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3524 _exptl_absorpt_coefficient_mu 1.625 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.8288 _exptl_absorpt_correction_T_max 0.9088 _exptl_absorpt_process_details ; Empirical with SADABS (Blessing, 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'N/A' _diffrn_standards_interval_count 'N/A' _diffrn_standards_interval_time 'N/A' _diffrn_standards_decay_% <1 _diffrn_reflns_number 34311 _diffrn_reflns_av_R_equivalents 0.1408 _diffrn_reflns_av_sigmaI/netI 0.3494 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 22.50 _reflns_number_total 20483 _reflns_number_gt 7053 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1183P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00445(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 20483 _refine_ls_number_parameters 1366 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.2398 _refine_ls_R_factor_gt 0.0911 _refine_ls_wR_factor_ref 0.2679 _refine_ls_wR_factor_gt 0.2019 _refine_ls_goodness_of_fit_ref 0.842 _refine_ls_restrained_S_all 0.841 _refine_ls_shift/su_max 1.297 _refine_ls_shift/su_mean 0.038 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 0.92541(13) 0.65722(12) 0.34990(9) 0.0421(7) Uani 1 1 d . A . Ni2 Ni 0.91896(13) 0.52300(12) 0.31673(9) 0.0394(7) Uani 1 1 d . . . Ni3 Ni 0.84994(13) 0.41300(13) 0.27300(9) 0.0416(7) Uani 1 1 d . . . Ni4 Ni 0.76211(13) 0.34860(12) 0.21838(9) 0.0404(7) Uani 1 1 d . . . Ni5 Ni 0.62601(13) 0.44273(12) 0.17436(9) 0.0369(6) Uani 1 1 d . . . Ni6 Ni 0.49092(13) 0.59206(12) 0.15148(9) 0.0372(6) Uani 1 1 d . . . Ni7 Ni 0.41745(13) 0.74356(12) 0.16206(9) 0.0409(7) Uani 1 1 d . A . Ni8 Ni 0.42305(14) 0.89176(12) 0.20655(9) 0.0448(7) Uani 1 1 d . A . Ni9 Ni 0.50511(13) 0.97246(12) 0.25278(9) 0.0418(7) Uani 1 1 d . A . Ni10 Ni 0.65537(13) 0.90899(12) 0.29495(9) 0.0424(7) Uani 1 1 d . A . Ni11 Ni 0.80726(14) 0.79501(13) 0.33596(10) 0.0497(7) Uani 1 1 d . A . S1 S 1.0141(3) 0.5802(2) 0.29073(18) 0.0407(13) Uani 1 1 d . . . S2 S 0.9108(3) 0.5571(3) 0.39897(18) 0.0440(14) Uani 1 1 d . . . S3 S 0.9177(3) 0.4925(3) 0.23523(19) 0.0444(14) Uani 1 1 d . . . S4 S 0.8097(3) 0.4831(3) 0.3428(2) 0.0534(15) Uani 1 1 d . . . S5 S 0.8934(3) 0.3460(3) 0.20063(19) 0.0432(13) Uani 1 1 d . . . S6 S 0.7733(3) 0.3369(2) 0.30537(19) 0.0432(13) Uani 1 1 d . . . S7 S 0.6301(3) 0.3513(2) 0.23741(19) 0.0400(12) Uani 1 1 d . . . S8 S 0.7462(3) 0.3727(2) 0.13221(19) 0.0428(13) Uani 1 1 d . . . S9 S 0.6206(3) 0.5378(2) 0.11498(18) 0.0386(12) Uani 1 1 d . . . S10 S 0.5129(3) 0.5143(2) 0.22168(18) 0.0409(13) Uani 1 1 d . . . S11 S 0.4668(3) 0.6809(2) 0.08755(18) 0.0399(13) Uani 1 1 d . . . S12 S 0.3624(3) 0.6529(3) 0.18602(19) 0.0461(13) Uani 1 1 d . . . S13 S 0.4841(3) 0.8246(3) 0.13564(19) 0.0494(14) Uani 1 1 d . . . S14 S 0.3621(3) 0.8046(3) 0.2377(2) 0.0560(15) Uani 1 1 d . . . S15 S 0.4779(3) 0.9812(3) 0.1698(2) 0.0513(15) Uani 1 1 d . . . S16 S 0.3833(3) 0.9527(3) 0.2821(2) 0.0540(15) Uani 1 1 d . . . S17 S 0.6303(3) 0.9837(2) 0.22329(19) 0.0442(13) Uani 1 1 d . . . S18 S 0.5301(3) 0.9722(3) 0.3359(2) 0.0486(14) Uani 1 1 d . . . S19 S 0.7756(3) 0.8398(3) 0.2557(2) 0.0532(15) Uani 1 1 d . . . S20 S 0.6723(3) 0.8280(3) 0.3651(2) 0.0532(15) Uani 1 1 d . . . S21 S 0.9410(3) 0.7580(3) 0.3007(2) 0.0525(15) Uani 1 1 d . . . S22 S 0.8424(3) 0.7346(3) 0.4110(2) 0.0535(15) Uani 1 1 d . . . C10 C 1.0210(9) 0.6124(7) 0.2207(4) 0.048(5) Uani 1 1 d G . . C11 C 0.9529(7) 0.6532(8) 0.2005(6) 0.062(6) Uani 1 1 d G . . H11A H 0.9000 0.6641 0.2246 0.074 Uiso 1 1 calc R . . C12 C 0.9623(11) 0.6782(7) 0.1451(6) 0.099(9) Uani 1 1 d G . . H12A H 0.9157 0.7061 0.1312 0.118 Uiso 1 1 calc R . . C13 C 1.0397(14) 0.6624(9) 0.1098(4) 0.124(13) Uani 1 1 d G . . H13A H 1.0461 0.6795 0.0719 0.149 Uiso 1 1 calc R . . C14 C 1.1078(10) 0.6216(9) 0.1300(6) 0.098(9) Uani 1 1 d G . . H14A H 1.1607 0.6108 0.1059 0.118 Uiso 1 1 calc R . . C15 C 1.0984(7) 0.5966(7) 0.1855(7) 0.089(8) Uani 1 1 d G . . H15A H 1.1450 0.5687 0.1993 0.107 Uiso 1 1 calc R . . C20 C 1.0105(5) 0.5227(7) 0.4153(5) 0.037(5) Uani 1 1 d G . . C21 C 1.0602(8) 0.4541(6) 0.4020(5) 0.057(6) Uani 1 1 d G . . H21A H 1.0445 0.4264 0.3805 0.068 Uiso 1 1 calc R . . C22 C 1.1328(7) 0.4261(5) 0.4202(5) 0.074(8) Uani 1 1 d G . . H22A H 1.1668 0.3792 0.4111 0.089 Uiso 1 1 calc R . . C23 C 1.1558(6) 0.4666(8) 0.4517(5) 0.053(6) Uani 1 1 d G . . H23A H 1.2055 0.4474 0.4642 0.064 Uiso 1 1 calc R . . C24 C 1.1061(8) 0.5352(7) 0.4650(4) 0.052(5) Uani 1 1 d G . . H24A H 1.1218 0.5629 0.4865 0.063 Uiso 1 1 calc R . . C25 C 1.0335(7) 0.5632(5) 0.4468(5) 0.047(5) Uani 1 1 d G . . H25A H 0.9995 0.6101 0.4559 0.057 Uiso 1 1 calc R . . C30 C 1.0205(5) 0.4452(6) 0.2046(5) 0.037(5) Uani 1 1 d G . . C31 C 1.0459(6) 0.4483(6) 0.1471(4) 0.041(5) Uani 1 1 d G . . H31A H 1.0086 0.4747 0.1250 0.049 Uiso 1 1 calc R . . C32 C 1.1261(7) 0.4127(6) 0.1222(3) 0.054(6) Uani 1 1 d G . . H32A H 1.1434 0.4148 0.0829 0.065 Uiso 1 1 calc R . . C33 C 1.1807(5) 0.3740(6) 0.1546(5) 0.053(6) Uani 1 1 d G . . H33A H 1.2355 0.3497 0.1376 0.063 Uiso 1 1 calc R . . C34 C 1.1553(6) 0.3710(6) 0.2121(5) 0.050(5) Uani 1 1 d G . . H34A H 1.1926 0.3446 0.2342 0.059 Uiso 1 1 calc R . . C35 C 1.0752(7) 0.4066(6) 0.2370(3) 0.049(5) Uani 1 1 d G . . H35A H 1.0578 0.4045 0.2763 0.058 Uiso 1 1 calc R . . C40 C 0.8793(11) 0.3630(12) 0.4069(7) 0.107(10) Uani 1 1 d G . . C41 C 0.8120(13) 0.4224(10) 0.4041(6) 0.080(8) Uani 1 1 d G . . H41A H 0.8133 0.4558 0.3726 0.096 Uiso 1 1 calc R . . C42 C 0.7429(10) 0.4331(11) 0.4474(8) 0.145(14) Uani 1 1 d G . . H42A H 0.6970 0.4738 0.4455 0.174 Uiso 1 1 calc R . . C43 C 0.7410(13) 0.3844(15) 0.4935(6) 0.20(3) Uani 1 1 d G . . H43A H 0.6938 0.3917 0.5231 0.244 Uiso 1 1 calc R . . C44 C 0.8083(18) 0.3249(12) 0.4963(7) 0.20(3) Uani 1 1 d G . . H44A H 0.8070 0.2916 0.5278 0.243 Uiso 1 1 calc R . . C45 C 0.8774(15) 0.3142(9) 0.4529(10) 0.21(2) Uani 1 1 d G . . H45A H 0.9233 0.2736 0.4548 0.249 Uiso 1 1 calc R . . C50 C 0.9445(8) 0.2606(7) 0.2259(6) 0.044(5) Uani 1 1 d G . . C51 C 0.9417(10) 0.1991(11) 0.2051(6) 0.105(10) Uani 1 1 d G . . H51A H 0.9086 0.2032 0.1794 0.126 Uiso 1 1 calc R . . C52 C 0.9875(12) 0.1317(8) 0.2218(9) 0.131(13) Uani 1 1 d G . . H52A H 0.9856 0.0896 0.2076 0.157 Uiso 1 1 calc R . . C53 C 1.0360(10) 0.1256(8) 0.2594(9) 0.126(12) Uani 1 1 d G . . H53A H 1.0673 0.0795 0.2709 0.151 Uiso 1 1 calc R . . C54 C 1.0388(9) 0.1871(12) 0.2803(7) 0.133(12) Uani 1 1 d G . . H54A H 1.0719 0.1830 0.3059 0.160 Uiso 1 1 calc R . . C55 C 0.9930(10) 0.2546(9) 0.2635(7) 0.094(8) Uani 1 1 d G . . H55A H 0.9949 0.2966 0.2777 0.112 Uiso 1 1 calc R . . C60 C 0.6778(6) 0.3803(7) 0.3485(5) 0.050(6) Uani 1 1 d G . . C61 C 0.6469(9) 0.3426(6) 0.3963(6) 0.065(7) Uani 1 1 d G . . H61A H 0.6764 0.2946 0.4051 0.078 Uiso 1 1 calc R . . C62 C 0.5729(10) 0.3753(9) 0.4312(4) 0.094(9) Uani 1 1 d G . . H62A H 0.5518 0.3496 0.4638 0.112 Uiso 1 1 calc R . . C63 C 0.5298(6) 0.4456(10) 0.4183(6) 0.078(8) Uani 1 1 d G . . H63A H 0.4792 0.4679 0.4421 0.093 Uiso 1 1 calc R . . C64 C 0.5606(8) 0.4832(6) 0.3705(7) 0.063(6) Uani 1 1 d G . . H64A H 0.5312 0.5313 0.3617 0.076 Uiso 1 1 calc R . . C65 C 0.6346(8) 0.4506(7) 0.3356(5) 0.051(6) Uani 1 1 d G . . H65A H 0.6557 0.4763 0.3030 0.061 Uiso 1 1 calc R . . C70 C 0.6260(9) 0.2814(7) 0.2008(5) 0.044(5) Uani 1 1 d G . . C71 C 0.6831(7) 0.2143(8) 0.2021(6) 0.073(7) Uani 1 1 d G . . H71A H 0.7274 0.2072 0.2196 0.087 Uiso 1 1 calc R . . C72 C 0.6753(9) 0.1574(6) 0.1780(7) 0.108(9) Uani 1 1 d G . . H72A H 0.7143 0.1115 0.1789 0.130 Uiso 1 1 calc R . . C73 C 0.6105(10) 0.1677(7) 0.1525(6) 0.077(7) Uani 1 1 d G . . H73A H 0.6051 0.1289 0.1359 0.092 Uiso 1 1 calc R . . C74 C 0.5534(8) 0.2349(8) 0.1511(6) 0.070(7) Uani 1 1 d G . . H74A H 0.5090 0.2419 0.1337 0.084 Uiso 1 1 calc R . . C75 C 0.5611(8) 0.2917(6) 0.1753(6) 0.058(6) Uani 1 1 d G . . H75A H 0.5221 0.3377 0.1744 0.069 Uiso 1 1 calc R . . C80 C 0.8068(6) 0.4311(6) 0.0955(4) 0.042(5) Uani 1 1 d G . . C81 C 0.8423(7) 0.4199(6) 0.0399(5) 0.050(6) Uani 1 1 d G . . H81A H 0.8367 0.3810 0.0236 0.060 Uiso 1 1 calc R . . C82 C 0.8858(7) 0.4658(8) 0.0080(4) 0.081(8) Uani 1 1 d G . . H82A H 0.9101 0.4582 -0.0300 0.097 Uiso 1 1 calc R . . C83 C 0.8940(6) 0.5229(7) 0.0317(5) 0.062(6) Uani 1 1 d G . . H83A H 0.9237 0.5542 0.0099 0.074 Uiso 1 1 calc R . . C84 C 0.8585(7) 0.5340(5) 0.0873(6) 0.047(5) Uani 1 1 d G . . H84A H 0.8640 0.5730 0.1036 0.057 Uiso 1 1 calc R . . C85 C 0.8149(7) 0.4881(6) 0.1192(4) 0.051(6) Uani 1 1 d G . . H85A H 0.7907 0.4958 0.1572 0.061 Uiso 1 1 calc R . . C90 C 0.6254(7) 0.5043(6) 0.0502(4) 0.045(5) Uani 1 1 d G . . C91 C 0.6702(7) 0.5301(6) 0.0017(5) 0.054(6) Uani 1 1 d G . . H91A H 0.6969 0.5654 0.0030 0.065 Uiso 1 1 calc R . . C92 C 0.6759(7) 0.5043(7) -0.0487(4) 0.057(6) Uani 1 1 d G . . H92A H 0.7065 0.5220 -0.0819 0.069 Uiso 1 1 calc R . . C93 C 0.6368(8) 0.4527(7) -0.0506(4) 0.059(6) Uani 1 1 d G . . H93A H 0.6407 0.4351 -0.0851 0.071 Uiso 1 1 calc R . . C94 C 0.5920(8) 0.4270(7) -0.0021(6) 0.097(9) Uani 1 1 d G . . H94A H 0.5653 0.3917 -0.0034 0.117 Uiso 1 1 calc R . . C95 C 0.5863(8) 0.4527(7) 0.0483(5) 0.068(6) Uani 1 1 d G . . H95A H 0.5557 0.4351 0.0815 0.081 Uiso 1 1 calc R . . C100 C 0.4370(6) 0.4666(6) 0.2415(5) 0.051(6) Uani 1 1 d G . . C101 C 0.3933(7) 0.4596(6) 0.2043(4) 0.043(5) Uani 1 1 d G . . H10A H 0.4047 0.4793 0.1672 0.052 Uiso 1 1 calc R . . C102 C 0.3328(7) 0.4239(7) 0.2214(5) 0.083(8) Uani 1 1 d G . . H10B H 0.3028 0.4191 0.1959 0.100 Uiso 1 1 calc R . . C103 C 0.3161(7) 0.3951(6) 0.2756(6) 0.055(6) Uani 1 1 d G . . H10C H 0.2747 0.3707 0.2873 0.066 Uiso 1 1 calc R . . C104 C 0.3599(8) 0.4021(6) 0.3129(4) 0.064(6) Uani 1 1 d G . . H10D H 0.3484 0.3824 0.3500 0.076 Uiso 1 1 calc R . . C105 C 0.4203(7) 0.4378(6) 0.2958(5) 0.042(5) Uani 1 1 d G . . H10E H 0.4503 0.4426 0.3213 0.050 Uiso 1 1 calc R . . C110 C 0.5534(6) 0.7008(5) 0.0422(5) 0.032(4) Uani 1 1 d G . . C111 C 0.5484(7) 0.7187(6) -0.0128(5) 0.053(6) Uani 1 1 d G . . H11B H 0.4996 0.7209 -0.0239 0.064 Uiso 1 1 calc R . . C112 C 0.6147(9) 0.7333(6) -0.0517(4) 0.067(7) Uani 1 1 d G . . H11C H 0.6113 0.7455 -0.0893 0.081 Uiso 1 1 calc R . . C113 C 0.6860(7) 0.7300(6) -0.0355(5) 0.063(6) Uani 1 1 d G . . H11D H 0.7314 0.7399 -0.0620 0.076 Uiso 1 1 calc R . . C114 C 0.6911(6) 0.7121(6) 0.0196(6) 0.062(6) Uani 1 1 d G . . H11E H 0.7398 0.7098 0.0306 0.074 Uiso 1 1 calc R . . C115 C 0.6247(7) 0.6975(5) 0.0584(4) 0.037(5) Uani 1 1 d G . . H11F H 0.6282 0.6852 0.0960 0.045 Uiso 1 1 calc R . . C120 C 0.3291(8) 0.6317(6) 0.2582(4) 0.046(5) Uani 1 1 d G . . C121 C 0.2604(7) 0.6060(7) 0.2749(6) 0.067(7) Uani 1 1 d G . . H12B H 0.2314 0.6026 0.2484 0.081 Uiso 1 1 calc R . . C122 C 0.2341(7) 0.5852(7) 0.3303(7) 0.069(7) Uani 1 1 d G . . H12C H 0.1872 0.5677 0.3417 0.083 Uiso 1 1 calc R . . C123 C 0.2766(9) 0.5902(7) 0.3690(4) 0.077(7) Uani 1 1 d G . . H12D H 0.2586 0.5760 0.4069 0.093 Uiso 1 1 calc R . . C124 C 0.3453(8) 0.6159(7) 0.3523(4) 0.064(6) Uani 1 1 d G . . H12E H 0.3743 0.6193 0.3788 0.077 Uiso 1 1 calc R . . C125 C 0.3715(6) 0.6366(6) 0.2969(5) 0.043(5) Uani 1 1 d G . . H12F H 0.4185 0.6542 0.2855 0.052 Uiso 1 1 calc R . . C130 C 0.4589(9) 0.8700(6) 0.0724(5) 0.044(5) Uani 1 1 d G . . C131 C 0.3805(8) 0.8851(8) 0.0630(7) 0.098(9) Uani 1 1 d G . . H13B H 0.3382 0.8722 0.0908 0.118 Uiso 1 1 calc R . . C132 C 0.3639(10) 0.9190(9) 0.0129(8) 0.141(14) Uani 1 1 d G . . H13C H 0.3103 0.9293 0.0064 0.169 Uiso 1 1 calc R . . C133 C 0.4258(14) 0.9379(8) -0.0279(6) 0.134(14) Uani 1 1 d G . . H13D H 0.4145 0.9611 -0.0622 0.160 Uiso 1 1 calc R . . C134 C 0.5043(11) 0.9228(8) -0.0185(5) 0.096(9) Uani 1 1 d G . . H13E H 0.5466 0.9357 -0.0464 0.115 Uiso 1 1 calc R . . C135 C 0.5208(7) 0.8889(7) 0.0316(7) 0.076(7) Uani 1 1 d G . . H13F H 0.5744 0.8786 0.0380 0.091 Uiso 1 1 calc R . . C140 C 0.2613(13) 0.8462(16) 0.2379(16) 0.068(16) Uani 0.65(2) 1 d PG A 1 C145 C 0.2246(18) 0.8255(19) 0.2020(14) 0.15(3) Uani 0.65(2) 1 d PG A 1 H14B H 0.2573 0.7944 0.1736 0.180 Uiso 0.65(2) 1 calc PR A 1 C144 C 0.1400(19) 0.850(2) 0.2076(14) 0.27(6) Uani 0.65(2) 1 d PG A 1 H14C H 0.1149 0.8361 0.1830 0.324 Uiso 0.65(2) 1 calc PR A 1 C143 C 0.0922(13) 0.8957(18) 0.2491(15) 0.126(19) Uani 0.65(2) 1 d PG A 1 H14D H 0.0344 0.9126 0.2529 0.151 Uiso 0.65(2) 1 calc PR A 1 C142 C 0.1289(19) 0.9164(17) 0.2850(15) 0.15(2) Uani 0.65(2) 1 d PG A 1 H14E H 0.0962 0.9475 0.3134 0.175 Uiso 0.65(2) 1 calc PR A 1 C141 C 0.214(2) 0.8916(19) 0.2794(16) 0.24(4) Uani 0.65(2) 1 d PG A 1 H14F H 0.2386 0.9058 0.3039 0.285 Uiso 0.65(2) 1 calc PR A 1 C240 C 0.2582(18) 0.851(2) 0.2214(19) 0.12(6) Uani 0.35(2) 1 d PG A 2 C241 C 0.202(2) 0.8137(15) 0.2208(19) 0.12(5) Uani 0.35(2) 1 d PG A 2 H24B H 0.2146 0.7633 0.2299 0.146 Uiso 0.35(2) 1 calc PR A 2 C242 C 0.128(2) 0.851(2) 0.2068(17) 0.03(3) Uani 0.35(2) 1 d PG A 2 H24C H 0.0894 0.8252 0.2064 0.033 Uiso 0.35(2) 1 calc PR A 2 C243 C 0.109(2) 0.924(2) 0.194(2) 0.10(4) Uani 0.35(2) 1 d PG A 2 H24D H 0.0585 0.9495 0.1840 0.124 Uiso 0.35(2) 1 calc PR A 2 C244 C 0.165(3) 0.9614(15) 0.194(2) 0.13(4) Uani 0.35(2) 1 d PG A 2 H24E H 0.1529 1.0119 0.1851 0.154 Uiso 0.35(2) 1 calc PR A 2 C245 C 0.240(3) 0.925(2) 0.2081(18) 0.08(3) Uani 0.35(2) 1 d PG A 2 H24F H 0.2782 0.9500 0.2085 0.093 Uiso 0.35(2) 1 calc PR A 2 C150 C 0.3902(8) 1.0569(7) 0.1733(6) 0.058(6) Uani 1 1 d G A . C151 C 0.3902(8) 1.1206(8) 0.1923(6) 0.072(8) Uani 1 1 d G . . H15B H 0.4370 1.1235 0.2035 0.087 Uiso 1 1 calc R A . C152 C 0.3217(11) 1.1801(7) 0.1948(6) 0.087(8) Uani 1 1 d G A . H15C H 0.3217 1.2236 0.2078 0.104 Uiso 1 1 calc R . . C153 C 0.2533(9) 1.1759(9) 0.1784(8) 0.126(12) Uani 1 1 d G . . H15D H 0.2065 1.2166 0.1801 0.151 Uiso 1 1 calc R A . C154 C 0.2533(9) 1.1122(11) 0.1595(10) 0.25(3) Uani 1 1 d G A . H15E H 0.2065 1.1093 0.1482 0.304 Uiso 1 1 calc R . . C155 C 0.3218(11) 1.0527(8) 0.1569(8) 0.152(14) Uani 1 1 d G . . H15F H 0.3218 1.0091 0.1440 0.182 Uiso 1 1 calc R A . C160 C 0.3809(11) 0.8913(9) 0.3426(6) 0.067(7) Uani 1 1 d G A . C161 C 0.4462(9) 0.8314(10) 0.3488(7) 0.095(9) Uani 1 1 d G . . H16A H 0.4946 0.8212 0.3201 0.115 Uiso 1 1 calc R A . C162 C 0.4409(12) 0.7865(8) 0.3971(9) 0.104(9) Uani 1 1 d G A . H16B H 0.4855 0.7456 0.4013 0.124 Uiso 1 1 calc R . . C163 C 0.3702(16) 0.8015(12) 0.4390(7) 0.156(14) Uani 1 1 d G . . H16C H 0.3665 0.7708 0.4720 0.187 Uiso 1 1 calc R A . C164 C 0.3048(11) 0.8613(14) 0.4327(7) 0.22(2) Uani 1 1 d G A . H16D H 0.2565 0.8715 0.4614 0.263 Uiso 1 1 calc R . . C165 C 0.3102(9) 0.9062(10) 0.3845(8) 0.173(17) Uani 1 1 d G . . H16E H 0.2655 0.9471 0.3802 0.208 Uiso 1 1 calc R A . C170 C 0.6777(7) 0.9382(6) 0.1608(4) 0.033(4) Uani 1 1 d G A . C171 C 0.7286(8) 0.9695(6) 0.1193(6) 0.070(7) Uani 1 1 d G . . H17A H 0.7361 1.0142 0.1242 0.084 Uiso 1 1 calc R A . C172 C 0.7685(8) 0.9353(8) 0.0705(5) 0.084(8) Uani 1 1 d G A . H17B H 0.8032 0.9566 0.0421 0.101 Uiso 1 1 calc R . . C173 C 0.7575(8) 0.8698(8) 0.0632(4) 0.089(9) Uani 1 1 d G . . H17C H 0.7848 0.8465 0.0299 0.107 Uiso 1 1 calc R A . C174 C 0.7067(9) 0.8386(6) 0.1047(6) 0.088(8) Uani 1 1 d G A . H17D H 0.6992 0.7938 0.0997 0.106 Uiso 1 1 calc R . . C175 C 0.6668(7) 0.8727(7) 0.1535(5) 0.050(6) Uani 1 1 d G . . H17E H 0.6320 0.8514 0.1818 0.060 Uiso 1 1 calc R A . C180 C 0.5328(10) 1.0635(7) 0.3334(5) 0.054(6) Uani 1 1 d G A . C181 C 0.5962(8) 1.0768(7) 0.3506(6) 0.071(7) Uani 1 1 d G . . H18A H 0.6378 1.0377 0.3620 0.085 Uiso 1 1 calc R A . C182 C 0.5987(9) 1.1472(10) 0.3511(6) 0.093(8) Uani 1 1 d G A . H18B H 0.6421 1.1563 0.3628 0.112 Uiso 1 1 calc R . . C183 C 0.5379(13) 1.2043(6) 0.3344(6) 0.095(10) Uani 1 1 d G . . H18C H 0.5396 1.2525 0.3348 0.114 Uiso 1 1 calc R A . C184 C 0.4745(10) 1.1911(8) 0.3173(5) 0.106(11) Uani 1 1 d G A . H18D H 0.4329 1.2301 0.3059 0.127 Uiso 1 1 calc R . . C185 C 0.4720(8) 1.1207(11) 0.3167(5) 0.077(8) Uani 1 1 d G . . H18E H 0.4286 1.1116 0.3050 0.093 Uiso 1 1 calc R A . C190 C 0.8934(12) 0.8706(9) 0.1716(8) 0.120(12) Uani 1 1 d G . . C191 C 0.9401(9) 0.9139(14) 0.1394(6) 0.168(18) Uani 1 1 d G A . H19A H 0.9786 0.8969 0.1065 0.202 Uiso 1 1 calc R . . C192 C 0.9305(12) 0.9820(14) 0.1554(10) 0.18(2) Uani 1 1 d G A . H19B H 0.9625 1.0116 0.1334 0.211 Uiso 1 1 calc R . . C193 C 0.8742(14) 1.0069(9) 0.2036(10) 0.151(14) Uani 1 1 d G A . H19C H 0.8676 1.0534 0.2145 0.182 Uiso 1 1 calc R . . C194 C 0.8275(10) 0.9636(11) 0.2358(6) 0.081(8) Uani 1 1 d G A . H19D H 0.7890 0.9806 0.2687 0.098 Uiso 1 1 calc R . . C195 C 0.8371(8) 0.8955(10) 0.2198(7) 0.065(6) Uani 1 1 d G A . H19E H 0.8051 0.8659 0.2418 0.078 Uiso 1 1 calc R . . C200 C 0.6492(9) 0.8741(7) 0.4275(5) 0.079(8) Uani 1 1 d G A . C201 C 0.5770(8) 0.8739(8) 0.4664(7) 0.095(9) Uani 1 1 d G . . H20A H 0.5413 0.8492 0.4601 0.114 Uiso 1 1 calc R A . C202 C 0.5569(9) 0.9100(9) 0.5145(5) 0.114(12) Uani 1 1 d G A . H20B H 0.5075 0.9099 0.5410 0.136 Uiso 1 1 calc R . . C203 C 0.6091(13) 0.9462(8) 0.5236(5) 0.132(15) Uani 1 1 d G . . H20C H 0.5954 0.9708 0.5565 0.159 Uiso 1 1 calc R A . C204 C 0.6814(11) 0.9464(8) 0.4847(8) 0.129(13) Uani 1 1 d G A . H20D H 0.7171 0.9711 0.4910 0.155 Uiso 1 1 calc R . . C205 C 0.7015(8) 0.9103(8) 0.4366(6) 0.081(8) Uani 1 1 d G . . H20E H 0.7508 0.9105 0.4100 0.098 Uiso 1 1 calc R A . C210 C 0.9910(10) 0.7894(10) 0.3418(8) 0.088(8) Uani 1 1 d G A . C211 C 0.9579(10) 0.8557(10) 0.3651(11) 0.20(2) Uani 1 1 d G . . H21B H 0.9047 0.8844 0.3618 0.241 Uiso 1 1 calc R A . C212 C 1.0027(16) 0.8799(11) 0.3933(13) 0.46(6) Uani 1 1 d G A . H21C H 0.9801 0.9252 0.4092 0.551 Uiso 1 1 calc R . . C213 C 1.0807(16) 0.8379(14) 0.3981(12) 0.27(3) Uani 1 1 d G . . H21D H 1.1113 0.8545 0.4174 0.321 Uiso 1 1 calc R A . C214 C 1.1138(11) 0.7717(13) 0.3748(10) 0.19(2) Uani 1 1 d G A . H21E H 1.1670 0.7429 0.3781 0.228 Uiso 1 1 calc R . . C215 C 1.0690(11) 0.7474(8) 0.3466(8) 0.106(10) Uani 1 1 d G . . H21F H 1.0916 0.7021 0.3307 0.127 Uiso 1 1 calc R A . C220 C 0.7592(7) 0.7063(7) 0.4554(6) 0.046(5) Uani 1 1 d G A . C221 C 0.7197(10) 0.6633(7) 0.4393(5) 0.066(7) Uani 1 1 d G . . H22B H 0.7381 0.6461 0.4032 0.079 Uiso 1 1 calc R A . C222 C 0.6534(10) 0.6455(8) 0.4759(9) 0.094(9) Uani 1 1 d G A . H22C H 0.6265 0.6161 0.4649 0.113 Uiso 1 1 calc R . . C223 C 0.6266(7) 0.6707(10) 0.5288(8) 0.101(10) Uani 1 1 d G . . H22D H 0.5813 0.6586 0.5538 0.121 Uiso 1 1 calc R A . C224 C 0.6660(11) 0.7137(9) 0.5449(5) 0.093(9) Uani 1 1 d G A . H22E H 0.6477 0.7310 0.5810 0.112 Uiso 1 1 calc R . . C225 C 0.7323(10) 0.7315(7) 0.5082(7) 0.078(8) Uani 1 1 d G . . H22F H 0.7593 0.7609 0.5193 0.094 Uiso 1 1 calc R A . O1A O 0.5727(14) 0.6558(14) 0.2864(11) 0.214(11) Uiso 1 1 d D . . O1B O 0.178(4) 0.861(3) 0.045(3) 0.60(5) Uiso 1 1 d D . . O1C O 0.910(3) 0.850(2) 0.934(2) 0.47(3) Uiso 1 1 d D . . O1D O 0.831(3) 0.052(2) 0.381(2) 0.42(3) Uiso 1 1 d D . . O1E O 0.849(2) 0.7432(13) 0.6377(14) 0.269(14) Uiso 1 1 d D . . C1A C 0.6404(15) 0.6660(18) 0.3053(9) 0.173(14) Uiso 1 1 d D . . H1AA H 0.6494 0.6320 0.3379 0.207 Uiso 1 1 calc R . . H1AB H 0.6236 0.7154 0.3179 0.207 Uiso 1 1 calc R . . C2A C 0.7216(11) 0.6557(18) 0.2632(11) 0.160(13) Uiso 1 1 d D . . H2AA H 0.7598 0.6076 0.2690 0.192 Uiso 1 1 calc R . . H2AB H 0.7482 0.6934 0.2645 0.192 Uiso 1 1 calc R . . C3A C 0.6942(14) 0.6628(17) 0.2090(8) 0.153(12) Uiso 1 1 d D . . H3AA H 0.7110 0.7018 0.1835 0.183 Uiso 1 1 calc R . . H3AB H 0.7162 0.6171 0.1903 0.183 Uiso 1 1 calc R . . C4A C 0.6016(13) 0.6812(17) 0.2294(10) 0.153(12) Uiso 1 1 d D . . H4AA H 0.5789 0.7343 0.2260 0.183 Uiso 1 1 calc R . . H4AB H 0.5792 0.6606 0.2048 0.183 Uiso 1 1 calc R . . C1B C 0.155(4) 0.861(3) -0.007(3) 0.48(5) Uiso 1 1 d D . . H1BA H 0.1633 0.9040 -0.0309 0.575 Uiso 1 1 calc R . . H1BB H 0.0965 0.8629 0.0006 0.575 Uiso 1 1 calc R . . C2B C 0.206(4) 0.794(3) -0.0371(13) 0.33(3) Uiso 1 1 d D . . H2BA H 0.2449 0.8051 -0.0711 0.394 Uiso 1 1 calc R . . H2BB H 0.1712 0.7681 -0.0468 0.394 Uiso 1 1 calc R . . C3B C 0.252(3) 0.750(2) 0.007(2) 0.30(3) Uiso 1 1 d D . . H3BA H 0.2559 0.6979 0.0084 0.365 Uiso 1 1 calc R . . H3BB H 0.3073 0.7561 0.0012 0.365 Uiso 1 1 calc R . . C4B C 0.195(4) 0.784(4) 0.0593(14) 0.42(4) Uiso 1 1 d D . . H4BA H 0.1441 0.7691 0.0691 0.501 Uiso 1 1 calc R . . H4BB H 0.2226 0.7701 0.0909 0.501 Uiso 1 1 calc R . . C1C C 0.988(3) 0.826(2) 0.952(2) 0.35(3) Uiso 1 1 d D . . H1CA H 0.9952 0.8648 0.9709 0.423 Uiso 1 1 calc R . . H1CB H 1.0350 0.8117 0.9208 0.423 Uiso 1 1 calc R . . C2C C 0.976(3) 0.763(3) 0.9926(14) 0.37(3) Uiso 1 1 d D . . H2CA H 0.9335 0.7781 1.0264 0.439 Uiso 1 1 calc R . . H2CB H 1.0281 0.7344 1.0031 0.439 Uiso 1 1 calc R . . C3C C 0.949(3) 0.7201(14) 0.9570(18) 0.24(2) Uiso 1 1 d D . . H3CA H 0.9960 0.6889 0.9324 0.290 Uiso 1 1 calc R . . H3CB H 0.9140 0.6905 0.9802 0.290 Uiso 1 1 calc R . . C4C C 0.899(2) 0.782(2) 0.9244(15) 0.226(18) Uiso 1 1 d D . . H4CA H 0.9182 0.7737 0.8843 0.271 Uiso 1 1 calc R . . H4CB H 0.8406 0.7835 0.9358 0.271 Uiso 1 1 calc R . . C1D C 0.831(3) 0.125(3) 0.3561(13) 0.35(3) Uiso 1 1 d D . . H1DA H 0.7812 0.1458 0.3407 0.424 Uiso 1 1 calc R . . H1DB H 0.8794 0.1218 0.3251 0.424 Uiso 1 1 calc R . . C2D C 0.832(2) 0.1739(13) 0.3980(19) 0.25(2) Uiso 1 1 d D . . H2DA H 0.7754 0.1978 0.4182 0.305 Uiso 1 1 calc R . . H2DB H 0.8598 0.2108 0.3802 0.305 Uiso 1 1 calc R . . C3D C 0.880(3) 0.119(3) 0.4362(17) 0.43(4) Uiso 1 1 d D . . H3DA H 0.9404 0.1103 0.4220 0.516 Uiso 1 1 calc R . . H3DB H 0.8650 0.1345 0.4745 0.516 Uiso 1 1 calc R . . C4D C 0.853(3) 0.0530(18) 0.4331(17) 0.26(2) Uiso 1 1 d D . . H4DA H 0.8982 0.0091 0.4379 0.316 Uiso 1 1 calc R . . H4DB H 0.8053 0.0518 0.4639 0.316 Uiso 1 1 calc R . . C1E C 0.878(4) 0.780(2) 0.5848(13) 0.46(5) Uiso 1 1 d D . . H1EA H 0.8491 0.7728 0.5575 0.546 Uiso 1 1 calc R . . H1EB H 0.9371 0.7565 0.5715 0.546 Uiso 1 1 calc R . . C2E C 0.866(3) 0.860(2) 0.5861(17) 0.27(2) Uiso 1 1 d D . . H2EA H 0.8710 0.8857 0.5489 0.325 Uiso 1 1 calc R . . H2EB H 0.9005 0.8714 0.6072 0.325 Uiso 1 1 calc R . . C3E C 0.776(2) 0.8711(17) 0.618(2) 0.28(2) Uiso 1 1 d D . . H3EA H 0.7615 0.9058 0.6471 0.339 Uiso 1 1 calc R . . H3EB H 0.7379 0.8898 0.5928 0.339 Uiso 1 1 calc R . . C4E C 0.7695(18) 0.797(2) 0.645(2) 0.31(3) Uiso 1 1 d D . . H4EA H 0.7443 0.8015 0.6846 0.370 Uiso 1 1 calc R . . H4EB H 0.7328 0.7815 0.6277 0.370 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 0.0357(14) 0.0499(16) 0.0340(15) -0.0146(12) -0.0106(12) 0.0053(12) Ni2 0.0327(13) 0.0493(16) 0.0329(14) -0.0152(12) -0.0071(12) -0.0013(12) Ni3 0.0376(14) 0.0549(17) 0.0349(15) -0.0122(13) -0.0146(12) -0.0075(13) Ni4 0.0385(14) 0.0475(16) 0.0372(15) -0.0130(12) -0.0132(12) -0.0067(12) Ni5 0.0335(13) 0.0425(15) 0.0363(14) -0.0111(12) -0.0098(12) -0.0076(12) Ni6 0.0353(13) 0.0441(16) 0.0313(14) -0.0124(12) -0.0080(12) -0.0049(12) Ni7 0.0381(14) 0.0425(16) 0.0343(15) -0.0101(12) -0.0088(12) 0.0041(12) Ni8 0.0486(15) 0.0424(16) 0.0344(15) -0.0125(12) -0.0103(13) 0.0055(13) Ni9 0.0421(14) 0.0371(15) 0.0372(15) -0.0106(12) -0.0069(12) 0.0041(12) Ni10 0.0393(14) 0.0450(16) 0.0355(15) -0.0093(12) -0.0087(12) 0.0025(12) Ni11 0.0441(15) 0.0522(17) 0.0373(15) -0.0122(13) -0.0045(13) 0.0097(13) S1 0.035(3) 0.049(3) 0.035(3) -0.014(2) -0.006(2) -0.003(2) S2 0.037(3) 0.053(3) 0.033(3) -0.014(2) -0.010(2) 0.008(2) S3 0.032(3) 0.057(3) 0.041(3) -0.017(3) -0.013(2) 0.002(2) S4 0.042(3) 0.074(4) 0.040(3) -0.024(3) -0.003(3) -0.007(3) S5 0.044(3) 0.054(3) 0.035(3) -0.012(2) -0.009(2) -0.014(3) S6 0.043(3) 0.047(3) 0.040(3) -0.007(2) -0.015(3) -0.007(2) S7 0.044(3) 0.037(3) 0.043(3) -0.003(2) -0.017(3) -0.011(2) S8 0.048(3) 0.040(3) 0.041(3) -0.011(2) -0.015(3) -0.006(2) S9 0.041(3) 0.044(3) 0.033(3) -0.010(2) -0.013(2) -0.008(2) S10 0.034(3) 0.054(3) 0.036(3) -0.011(2) -0.006(2) -0.010(2) S11 0.037(3) 0.051(3) 0.028(3) -0.013(2) -0.009(2) -0.003(2) S12 0.035(3) 0.058(4) 0.042(3) -0.008(3) -0.010(2) -0.005(3) S13 0.058(3) 0.048(3) 0.036(3) -0.009(3) -0.019(3) 0.003(3) S14 0.069(4) 0.040(3) 0.043(3) -0.012(3) -0.004(3) 0.006(3) S15 0.055(3) 0.040(3) 0.049(3) -0.011(3) -0.021(3) 0.012(3) S16 0.048(3) 0.056(4) 0.046(3) -0.021(3) -0.010(3) 0.010(3) S17 0.053(3) 0.044(3) 0.032(3) -0.014(2) -0.009(3) -0.003(3) S18 0.052(3) 0.045(3) 0.041(3) -0.013(3) -0.011(3) 0.003(3) S19 0.058(3) 0.047(3) 0.039(3) -0.006(3) -0.011(3) 0.010(3) S20 0.050(3) 0.053(4) 0.040(3) -0.011(3) -0.004(3) 0.008(3) S21 0.046(3) 0.047(3) 0.053(3) -0.012(3) -0.011(3) 0.008(3) S22 0.051(3) 0.057(4) 0.038(3) -0.015(3) -0.007(3) 0.009(3) C10 0.062(13) 0.064(15) 0.026(11) -0.021(10) -0.011(11) -0.020(12) C11 0.080(16) 0.098(18) 0.015(11) 0.005(11) -0.016(11) -0.033(14) C12 0.13(3) 0.10(2) 0.066(19) -0.006(17) -0.047(19) -0.022(19) C13 0.24(4) 0.07(2) 0.053(19) -0.022(16) -0.01(2) -0.05(2) C14 0.12(2) 0.11(2) 0.051(18) -0.015(16) 0.042(17) -0.057(19) C15 0.099(19) 0.093(19) 0.049(16) -0.041(14) 0.037(15) -0.019(15) C20 0.020(9) 0.048(13) 0.035(11) -0.010(10) -0.008(9) 0.008(9) C21 0.051(13) 0.076(16) 0.047(13) -0.026(12) -0.011(11) -0.013(12) C22 0.075(16) 0.051(15) 0.055(15) -0.001(12) -0.026(13) 0.050(13) C23 0.045(12) 0.074(17) 0.040(13) 0.029(11) -0.035(11) -0.008(12) C24 0.074(15) 0.053(15) 0.027(11) 0.018(10) 0.003(11) -0.034(12) C25 0.029(11) 0.076(15) 0.025(11) 0.000(10) -0.004(9) 0.000(11) C30 0.025(10) 0.056(13) 0.027(11) -0.022(10) -0.003(9) 0.000(9) C31 0.035(11) 0.030(11) 0.054(14) -0.005(10) -0.013(10) 0.000(9) C32 0.062(14) 0.077(16) 0.009(10) -0.017(10) 0.014(10) -0.011(12) C33 0.030(11) 0.041(13) 0.092(18) -0.035(12) -0.024(12) 0.004(10) C34 0.047(13) 0.062(14) 0.040(13) -0.023(11) -0.005(11) -0.012(11) C35 0.045(12) 0.054(14) 0.041(12) -0.027(11) -0.002(11) 0.000(11) C40 0.19(3) 0.065(19) 0.09(2) 0.018(16) -0.10(2) -0.03(2) C41 0.10(2) 0.13(2) 0.037(15) -0.032(15) 0.002(15) -0.078(19) C42 0.12(3) 0.32(5) 0.039(17) -0.03(2) -0.010(19) -0.13(3) C43 0.30(5) 0.42(7) 0.010(16) 0.00(2) 0.00(2) -0.31(5) C44 0.42(8) 0.18(4) 0.15(4) 0.08(3) -0.18(5) -0.23(5) C45 0.44(8) 0.15(3) 0.09(3) 0.06(3) -0.13(4) -0.14(4) C50 0.036(11) 0.054(14) 0.030(11) 0.006(10) 0.011(10) -0.017(10) C51 0.080(18) 0.063(19) 0.17(3) -0.04(2) -0.023(19) -0.014(16) C52 0.16(3) 0.05(2) 0.18(3) -0.04(2) -0.07(3) 0.01(2) C53 0.10(2) 0.06(2) 0.18(4) 0.03(2) 0.02(2) -0.019(17) C54 0.08(2) 0.08(2) 0.22(4) 0.02(3) -0.05(2) 0.002(19) C55 0.080(18) 0.09(2) 0.10(2) -0.017(17) -0.024(17) 0.002(16) C60 0.024(10) 0.063(15) 0.062(15) -0.036(12) -0.014(11) 0.007(11) C61 0.096(18) 0.091(17) 0.004(10) 0.032(11) 0.008(11) -0.052(14) C62 0.09(2) 0.14(3) 0.026(13) 0.018(15) 0.022(14) -0.047(18) C63 0.059(15) 0.11(2) 0.059(18) -0.038(16) -0.006(14) -0.011(16) C64 0.050(15) 0.069(16) 0.075(17) -0.004(14) -0.021(14) -0.017(13) C65 0.035(12) 0.081(17) 0.032(12) -0.015(12) -0.003(10) -0.011(11) C70 0.059(13) 0.033(13) 0.045(13) 0.009(10) -0.024(11) -0.013(11) C71 0.066(15) 0.076(18) 0.089(18) -0.016(15) -0.021(14) -0.032(15) C72 0.10(2) 0.08(2) 0.15(3) -0.027(19) -0.03(2) -0.008(17) C73 0.077(17) 0.075(19) 0.089(19) -0.019(15) -0.034(15) -0.019(15) C74 0.091(17) 0.051(15) 0.093(18) 0.002(13) -0.064(15) -0.022(14) C75 0.081(15) 0.049(14) 0.063(15) -0.005(11) -0.033(13) -0.033(12) C80 0.038(11) 0.043(13) 0.055(14) 0.004(10) -0.023(11) -0.018(10) C81 0.059(13) 0.084(16) 0.001(9) -0.002(9) 0.019(9) -0.034(12) C82 0.061(15) 0.13(2) 0.061(17) -0.007(16) -0.014(14) -0.040(16) C83 0.023(11) 0.11(2) 0.050(15) 0.012(13) 0.000(11) -0.027(12) C84 0.039(12) 0.043(13) 0.056(14) 0.026(10) 0.004(11) -0.030(10) C85 0.057(13) 0.046(13) 0.052(14) -0.021(11) -0.024(11) -0.003(11) C90 0.056(13) 0.043(13) 0.032(12) -0.020(10) -0.006(11) -0.003(11) C91 0.059(13) 0.067(15) 0.022(11) -0.027(11) 0.011(10) -0.004(11) C92 0.084(16) 0.048(14) 0.035(13) -0.003(10) 0.003(12) -0.025(12) C93 0.065(15) 0.074(17) 0.027(13) -0.015(12) -0.005(12) -0.001(13) C94 0.15(2) 0.11(2) 0.070(18) -0.032(16) -0.056(19) -0.060(19) C95 0.100(17) 0.079(17) 0.038(14) -0.012(12) 0.000(13) -0.055(14) C100 0.013(10) 0.070(15) 0.068(15) -0.017(12) -0.018(11) 0.003(10) C101 0.054(12) 0.040(12) 0.052(13) 0.002(10) -0.028(11) -0.027(10) C102 0.104(19) 0.12(2) 0.057(17) -0.006(15) -0.049(16) -0.059(17) C103 0.040(12) 0.079(16) 0.059(15) -0.002(12) -0.009(12) -0.040(11) C104 0.088(17) 0.063(15) 0.049(14) 0.008(11) -0.021(13) -0.034(13) C105 0.040(12) 0.059(14) 0.034(12) 0.022(10) -0.017(10) -0.030(10) C110 0.030(10) 0.024(10) 0.044(12) -0.026(9) 0.004(9) -0.011(8) C111 0.072(15) 0.058(14) 0.022(11) -0.001(10) 0.020(11) -0.032(12) C112 0.098(18) 0.039(14) 0.047(15) 0.000(11) -0.018(15) 0.007(13) C113 0.082(17) 0.065(15) 0.035(14) -0.039(12) 0.018(12) -0.018(13) C114 0.073(15) 0.063(15) 0.058(16) -0.036(12) -0.005(13) -0.023(12) C115 0.021(10) 0.034(11) 0.048(12) -0.028(9) 0.028(10) -0.015(9) C120 0.056(13) 0.057(14) 0.017(10) 0.004(9) -0.024(10) 0.009(11) C121 0.025(12) 0.095(18) 0.09(2) -0.039(15) 0.000(12) -0.020(12) C122 0.058(15) 0.092(18) 0.045(15) -0.009(13) -0.001(13) -0.010(13) C123 0.084(18) 0.099(19) 0.033(14) -0.003(13) -0.010(14) -0.006(15) C124 0.061(15) 0.084(17) 0.053(16) 0.002(13) -0.021(13) -0.023(13) C125 0.060(13) 0.043(12) 0.020(11) -0.004(9) -0.009(10) -0.004(10) C130 0.050(12) 0.042(13) 0.041(13) -0.014(10) -0.009(11) -0.012(10) C131 0.11(2) 0.11(2) 0.11(2) 0.040(17) -0.072(19) -0.043(17) C132 0.14(3) 0.14(3) 0.18(3) 0.11(3) -0.11(3) -0.09(2) C133 0.26(4) 0.10(2) 0.07(2) 0.004(17) -0.10(3) -0.04(3) C134 0.15(3) 0.058(17) 0.053(18) -0.004(14) -0.018(17) 0.008(18) C135 0.080(17) 0.099(19) 0.021(12) -0.006(12) 0.008(13) 0.001(14) C140 0.00(2) 0.07(3) 0.12(4) -0.07(2) 0.04(2) 0.00(2) C145 0.00(2) 0.29(8) 0.13(5) -0.11(5) 0.02(3) 0.01(3) C144 0.23(8) 0.23(9) 0.21(8) -0.04(7) 0.13(6) 0.00(6) C143 0.06(3) 0.14(5) 0.15(5) -0.03(4) 0.01(3) 0.00(3) C142 0.13(5) 0.13(4) 0.20(6) -0.07(4) 0.00(4) -0.08(4) C141 0.04(3) 0.46(12) 0.22(8) -0.16(8) -0.01(4) -0.03(5) C240 0.12(8) 0.23(15) 0.00(4) -0.03(5) 0.04(4) -0.09(8) C241 0.00(3) 0.00(3) 0.22(10) 0.08(4) 0.14(5) 0.04(2) C242 0.00(3) 0.04(7) 0.03(5) -0.04(5) 0.00(4) 0.02(4) C243 0.04(4) 0.00(3) 0.26(11) 0.03(5) -0.05(6) 0.01(3) C244 0.05(4) 0.17(8) 0.20(10) -0.11(7) 0.00(5) -0.04(5) C245 0.16(7) 0.02(4) 0.10(5) 0.08(3) -0.12(5) -0.06(4) C150 0.028(11) 0.070(16) 0.072(16) -0.005(13) -0.028(11) 0.006(11) C151 0.072(15) 0.058(16) 0.065(16) -0.031(13) -0.031(13) 0.039(13) C152 0.11(2) 0.066(19) 0.052(16) 0.003(13) 0.004(16) 0.008(17) C153 0.08(2) 0.041(18) 0.19(3) 0.039(19) -0.02(2) 0.039(16) C154 0.12(3) 0.10(3) 0.54(8) 0.08(4) -0.20(4) 0.04(2) C155 0.14(3) 0.08(2) 0.28(4) 0.04(2) -0.14(3) -0.04(2) C160 0.064(15) 0.087(18) 0.043(14) -0.002(12) -0.025(13) -0.003(14) C161 0.12(2) 0.10(2) 0.040(15) 0.004(14) -0.034(15) 0.027(17) C162 0.10(2) 0.10(2) 0.09(2) 0.007(19) -0.03(2) -0.009(18) C163 0.13(3) 0.19(4) 0.09(3) 0.06(2) 0.01(2) -0.02(3) C164 0.14(3) 0.33(6) 0.09(3) 0.05(3) 0.06(3) -0.01(4) C165 0.08(2) 0.24(4) 0.09(2) 0.06(3) 0.041(19) 0.03(2) C170 0.025(10) 0.041(12) 0.023(11) -0.008(9) -0.003(9) 0.004(9) C171 0.090(17) 0.036(13) 0.047(14) -0.006(11) 0.012(13) 0.017(12) C172 0.13(2) 0.060(17) 0.047(15) -0.003(13) 0.000(15) -0.023(16) C173 0.13(2) 0.10(2) 0.013(12) -0.022(13) 0.044(13) -0.042(18) C174 0.13(2) 0.074(18) 0.072(18) -0.037(15) -0.032(17) -0.023(17) C175 0.049(12) 0.056(14) 0.037(12) -0.030(11) 0.013(10) -0.009(11) C180 0.057(14) 0.079(17) 0.019(11) -0.024(11) 0.005(10) -0.013(13) C181 0.091(18) 0.025(14) 0.090(18) -0.025(12) -0.005(15) -0.008(12) C182 0.11(2) 0.065(18) 0.12(2) -0.014(17) -0.028(19) -0.049(17) C183 0.19(3) 0.032(16) 0.041(15) 0.010(12) 0.029(17) -0.045(19) C184 0.18(3) 0.048(19) 0.062(17) -0.037(14) -0.052(19) 0.037(18) C185 0.078(17) 0.09(2) 0.056(16) -0.045(15) -0.023(13) 0.017(15) C190 0.063(18) 0.15(3) 0.055(17) 0.034(17) 0.047(14) 0.029(18) C191 0.06(2) 0.21(4) 0.15(4) -0.01(3) 0.01(2) 0.04(3) C192 0.10(3) 0.28(6) 0.13(4) 0.02(3) 0.02(2) -0.08(3) C193 0.12(3) 0.18(3) 0.21(4) -0.01(3) -0.08(3) -0.09(3) C194 0.048(15) 0.10(2) 0.084(19) 0.016(17) -0.017(14) -0.013(15) C195 0.025(12) 0.066(17) 0.089(19) 0.009(14) -0.003(12) -0.006(11) C200 0.058(15) 0.11(2) 0.036(14) -0.029(13) -0.008(13) 0.042(14) C201 0.062(15) 0.12(2) 0.043(15) -0.012(15) 0.018(13) 0.040(15) C202 0.10(2) 0.13(3) 0.038(17) -0.015(16) 0.032(16) 0.028(19) C203 0.16(3) 0.12(3) 0.06(2) -0.052(19) -0.02(2) 0.05(2) C204 0.16(3) 0.08(2) 0.11(2) -0.070(19) -0.08(2) 0.07(2) C205 0.107(19) 0.075(18) 0.062(17) -0.033(14) -0.036(15) 0.001(15) C210 0.061(16) 0.066(18) 0.13(2) -0.023(16) -0.028(16) 0.006(14) C211 0.09(2) 0.08(2) 0.45(6) -0.15(3) -0.04(3) -0.015(18) C212 0.21(5) 0.28(6) 1.03(17) -0.34(8) -0.33(8) 0.00(4) C213 0.23(5) 0.21(5) 0.46(8) -0.09(5) -0.22(6) -0.07(4) C214 0.18(3) 0.11(3) 0.32(5) -0.11(3) -0.16(4) 0.03(2) C215 0.12(2) 0.09(2) 0.13(2) -0.008(18) -0.08(2) -0.019(19) C220 0.045(12) 0.006(10) 0.082(17) 0.010(10) -0.025(12) 0.004(9) C221 0.041(13) 0.078(18) 0.058(15) -0.010(13) -0.002(13) 0.008(13) C222 0.070(19) 0.12(2) 0.10(2) -0.026(19) -0.038(17) -0.006(17) C223 0.054(16) 0.13(3) 0.10(3) 0.021(19) -0.011(17) -0.012(17) C224 0.075(19) 0.11(2) 0.045(16) 0.021(15) 0.017(15) 0.012(17) C225 0.11(2) 0.080(18) 0.029(13) -0.007(13) -0.011(14) -0.006(15) _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 2.207(6) . ? Ni1 S1 2.214(5) . ? Ni1 S22 2.217(5) . ? Ni1 S21 2.224(6) . ? Ni1 Ni11 2.895(3) . ? Ni1 Ni2 2.896(3) . ? Ni2 S1 2.199(5) . ? Ni2 S4 2.200(6) . ? Ni2 S2 2.204(5) . ? Ni2 S3 2.207(5) . ? Ni3 S4 2.206(5) . ? Ni3 S3 2.205(6) . ? Ni3 S5 2.217(5) . ? Ni3 S6 2.236(6) . ? Ni3 Ni4 2.919(3) . ? Ni4 S6 2.207(5) . ? Ni4 S8 2.210(5) . ? Ni4 S5 2.217(5) . ? Ni4 S7 2.228(5) . ? Ni4 Ni5 2.897(3) . ? Ni5 S9 2.205(5) . ? Ni5 S10 2.208(5) . ? Ni5 S7 2.209(5) . ? Ni5 S8 2.225(5) . ? Ni6 S10 2.188(5) . ? Ni6 S11 2.207(5) . ? Ni6 S9 2.210(5) . ? Ni6 S12 2.217(5) . ? Ni6 Ni7 2.865(3) . ? Ni7 S13 2.179(6) . ? Ni7 S12 2.207(6) . ? Ni7 S11 2.211(5) . ? Ni7 S14 2.221(5) . ? Ni8 S13 2.200(5) . ? Ni8 S16 2.217(5) . ? Ni8 S15 2.224(6) . ? Ni8 S14 2.228(6) . ? Ni8 Ni9 2.932(3) . ? Ni9 S17 2.200(5) . ? Ni9 S16 2.209(6) . ? Ni9 S15 2.217(5) . ? Ni9 S18 2.227(5) . ? Ni9 Ni10 2.942(3) . ? Ni10 S17 2.195(5) . ? Ni10 S19 2.198(5) . ? Ni10 S20 2.209(6) . ? Ni10 S18 2.229(5) . ? Ni11 S22 2.195(5) . ? Ni11 S20 2.210(5) . ? Ni11 S19 2.210(5) . ? Ni11 S21 2.215(5) . ? S1 C10 1.764(10) . ? S2 C20 1.801(8) . ? S3 C30 1.783(8) . ? S4 C41 1.804(14) . ? S5 C50 1.752(12) . ? S6 C60 1.780(9) . ? S7 C70 1.771(9) . ? S8 C80 1.796(9) . ? S9 C90 1.801(8) . ? S10 C100 1.781(9) . ? S11 C110 1.763(9) . ? S12 C120 1.782(9) . ? S13 C130 1.791(11) . ? S14 C140 1.71(2) . ? S14 C240 1.89(3) . ? S15 C150 1.774(10) . ? S16 C160 1.795(13) . ? S17 C170 1.790(8) . ? S18 C180 1.791(11) . ? S19 C195 1.761(15) . ? S20 C200 1.803(10) . ? S21 C210 1.777(13) . ? S22 C220 1.781(12) . ? C10 C11 1.3900 . ? C10 C15 1.3900 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C20 C21 1.3900 . ? C20 C25 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C30 C31 1.3900 . ? C30 C35 1.3900 . ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C40 C41 1.3900 . ? C40 C45 1.3900 . ? C41 C42 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C50 C51 1.3900 . ? C50 C55 1.3900 . ? C51 C52 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C60 C61 1.3900 . ? C60 C65 1.3900 . ? C61 C62 1.3900 . ? C62 C63 1.3900 . ? C63 C64 1.3900 . ? C64 C65 1.3900 . ? C70 C71 1.3900 . ? C70 C75 1.3900 . ? C71 C72 1.3900 . ? C72 C73 1.3900 . ? C73 C74 1.3900 . ? C74 C75 1.3900 . ? C80 C81 1.3900 . ? C80 C85 1.3900 . ? C81 C82 1.3900 . ? C82 C83 1.3900 . ? C83 C84 1.3900 . ? C84 C85 1.3900 . ? C90 C91 1.3900 . ? C90 C95 1.3900 . ? C91 C92 1.3900 . ? C92 C93 1.3900 . ? C93 C94 1.3900 . ? C94 C95 1.3900 . ? C100 C101 1.3900 . ? C100 C105 1.3900 . ? C101 C102 1.3900 . ? C102 C103 1.3900 . ? C103 C104 1.3900 . ? C104 C105 1.3900 . ? C110 C111 1.3900 . ? C110 C115 1.3900 . ? C111 C112 1.3900 . ? C112 C113 1.3900 . ? C113 C114 1.3900 . ? C114 C115 1.3900 . ? C120 C121 1.3900 . ? C120 C125 1.3900 . ? C121 C122 1.3900 . ? C122 C123 1.3900 . ? C123 C124 1.3900 . ? C124 C125 1.3900 . ? C130 C131 1.3900 . ? C130 C135 1.3900 . ? C131 C132 1.3900 . ? C132 C133 1.3900 . ? C133 C134 1.3900 . ? C134 C135 1.3900 . ? C140 C145 1.3900 . ? C140 C141 1.3900 . ? C145 C144 1.3900 . ? C144 C143 1.3900 . ? C143 C142 1.3900 . ? C142 C141 1.3900 . ? C240 C241 1.3900 . ? C240 C245 1.3900 . ? C241 C242 1.3900 . ? C242 C243 1.3900 . ? C243 C244 1.3900 . ? C244 C245 1.3900 . ? C150 C151 1.3900 . ? C150 C155 1.3900 . ? C151 C152 1.3900 . ? C152 C153 1.3900 . ? C153 C154 1.3900 . ? C154 C155 1.3900 . ? C160 C161 1.3900 . ? C160 C165 1.3900 . ? C161 C162 1.3900 . ? C162 C163 1.3900 . ? C163 C164 1.3900 . ? C164 C165 1.3900 . ? C170 C171 1.3900 . ? C170 C175 1.3900 . ? C171 C172 1.3900 . ? C172 C173 1.3900 . ? C173 C174 1.3900 . ? C174 C175 1.3900 . ? C180 C181 1.3900 . ? C180 C185 1.3900 . ? C181 C182 1.3900 . ? C182 C183 1.3900 . ? C183 C184 1.3900 . ? C184 C185 1.3900 . ? C190 C191 1.3900 . ? C190 C195 1.3900 . ? C191 C192 1.3900 . ? C192 C193 1.3900 . ? C193 C194 1.3900 . ? C194 C195 1.3900 . ? C200 C201 1.3900 . ? C200 C205 1.3900 . ? C201 C202 1.3900 . ? C202 C203 1.3900 . ? C203 C204 1.3900 . ? C204 C205 1.3900 . ? C210 C211 1.3900 . ? C210 C215 1.3900 . ? C211 C212 1.3900 . ? C212 C213 1.3900 . ? C213 C214 1.3900 . ? C214 C215 1.3900 . ? C220 C221 1.3900 . ? C220 C225 1.3900 . ? C221 C222 1.3900 . ? C222 C223 1.3900 . ? C223 C224 1.3900 . ? C224 C225 1.3900 . ? O1A C1A 1.459(4) . ? O1A C4A 1.459(4) . ? O1B C4B 1.460(4) . ? O1B C1B 1.460(4) . ? O1C C1C 1.461(4) . ? O1C C4C 1.461(4) . ? O1D C1D 1.460(4) . ? O1D C4D 1.461(4) . ? O1E C4E 1.460(4) . ? O1E C1E 1.461(4) . ? C1A C2A 1.518(4) . ? C2A C3A 1.524(10) . ? C3A C4A 1.518(4) . ? C1B C2B 1.519(4) . ? C2B C3B 1.538(10) . ? C3B C4B 1.519(4) . ? C1C C2C 1.520(4) . ? C2C C3C 1.542(10) . ? C3C C4C 1.520(4) . ? C1D C2D 1.520(4) . ? C2D C3D 1.540(10) . ? C3D C4D 1.519(4) . ? C1E C2E 1.519(4) . ? C2E C3E 1.542(10) . ? C3E C4E 1.519(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Ni1 S1 82.47(19) . . ? S2 Ni1 S22 97.8(2) . . ? S1 Ni1 S22 176.8(2) . . ? S2 Ni1 S21 179.6(2) . . ? S1 Ni1 S21 97.5(2) . . ? S22 Ni1 S21 82.2(2) . . ? S2 Ni1 Ni11 131.17(15) . . ? S1 Ni1 Ni11 133.10(16) . . ? S22 Ni1 Ni11 48.66(14) . . ? S21 Ni1 Ni11 49.15(13) . . ? S2 Ni1 Ni2 48.93(12) . . ? S1 Ni1 Ni2 48.77(14) . . ? S22 Ni1 Ni2 133.47(18) . . ? S21 Ni1 Ni2 131.29(15) . . ? Ni11 Ni1 Ni2 124.18(10) . . ? S1 Ni2 S4 170.8(2) . . ? S1 Ni2 S2 82.86(19) . . ? S4 Ni2 S2 95.16(19) . . ? S1 Ni2 S3 99.47(19) . . ? S4 Ni2 S3 82.02(19) . . ? S2 Ni2 S3 175.95(18) . . ? S1 Ni2 Ni1 49.20(12) . . ? S4 Ni2 Ni1 123.30(15) . . ? S2 Ni2 Ni1 49.01(15) . . ? S3 Ni2 Ni1 130.53(18) . . ? S4 Ni3 S3 81.9(2) . . ? S4 Ni3 S5 177.4(2) . . ? S3 Ni3 S5 95.52(19) . . ? S4 Ni3 S6 99.9(2) . . ? S3 Ni3 S6 174.36(19) . . ? S5 Ni3 S6 82.60(19) . . ? S4 Ni3 Ni4 132.82(16) . . ? S3 Ni3 Ni4 126.62(15) . . ? S5 Ni3 Ni4 48.84(13) . . ? S6 Ni3 Ni4 48.50(13) . . ? S6 Ni4 S8 174.0(2) . . ? S6 Ni4 S5 83.27(18) . . ? S8 Ni4 S5 97.16(19) . . ? S6 Ni4 S7 95.97(19) . . ? S8 Ni4 S7 83.58(18) . . ? S5 Ni4 S7 179.24(19) . . ? S6 Ni4 Ni5 126.30(15) . . ? S8 Ni4 Ni5 49.44(13) . . ? S5 Ni4 Ni5 131.51(17) . . ? S7 Ni4 Ni5 48.96(14) . . ? S6 Ni4 Ni3 49.38(14) . . ? S8 Ni4 Ni3 127.00(17) . . ? S5 Ni4 Ni3 48.84(12) . . ? S7 Ni4 Ni3 130.53(14) . . ? Ni5 Ni4 Ni3 118.33(10) . . ? S9 Ni5 S10 82.91(19) . . ? S9 Ni5 S7 176.96(18) . . ? S10 Ni5 S7 95.0(2) . . ? S9 Ni5 S8 98.24(19) . . ? S10 Ni5 S8 174.57(19) . . ? S7 Ni5 S8 83.66(19) . . ? S9 Ni5 Ni4 130.39(15) . . ? S10 Ni5 Ni4 126.56(15) . . ? S7 Ni5 Ni4 49.52(13) . . ? S8 Ni5 Ni4 48.98(13) . . ? S10 Ni6 S11 172.94(18) . . ? S10 Ni6 S9 83.27(18) . . ? S11 Ni6 S9 99.59(19) . . ? S10 Ni6 S12 99.4(2) . . ? S11 Ni6 S12 77.52(19) . . ? S9 Ni6 S12 176.5(2) . . ? S10 Ni6 Ni7 123.62(14) . . ? S11 Ni6 Ni7 49.62(12) . . ? S9 Ni6 Ni7 127.04(16) . . ? S12 Ni6 Ni7 49.48(15) . . ? S13 Ni7 S12 173.98(19) . . ? S13 Ni7 S11 98.3(2) . . ? S12 Ni7 S11 77.66(19) . . ? S13 Ni7 S14 84.3(2) . . ? S12 Ni7 S14 99.8(2) . . ? S11 Ni7 S14 177.0(2) . . ? S13 Ni7 Ni6 124.19(15) . . ? S12 Ni7 Ni6 49.79(13) . . ? S11 Ni7 Ni6 49.50(14) . . ? S14 Ni7 Ni6 129.79(17) . . ? S13 Ni8 S16 169.7(2) . . ? S13 Ni8 S15 94.5(2) . . ? S16 Ni8 S15 83.4(2) . . ? S13 Ni8 S14 83.7(2) . . ? S16 Ni8 S14 99.3(2) . . ? S15 Ni8 S14 175.1(2) . . ? S13 Ni8 Ni9 123.46(17) . . ? S16 Ni8 Ni9 48.38(15) . . ? S15 Ni8 Ni9 48.57(13) . . ? S14 Ni8 Ni9 136.02(16) . . ? S17 Ni9 S16 175.9(2) . . ? S17 Ni9 S15 96.3(2) . . ? S16 Ni9 S15 83.7(2) . . ? S17 Ni9 S18 83.14(19) . . ? S16 Ni9 S18 97.1(2) . . ? S15 Ni9 S18 176.0(2) . . ? S17 Ni9 Ni8 128.79(14) . . ? S16 Ni9 Ni8 48.63(13) . . ? S15 Ni9 Ni8 48.78(16) . . ? S18 Ni9 Ni8 134.25(18) . . ? S17 Ni9 Ni10 47.92(14) . . ? S16 Ni9 Ni10 129.64(17) . . ? S15 Ni9 Ni10 133.24(15) . . ? S18 Ni9 Ni10 48.71(13) . . ? Ni8 Ni9 Ni10 125.07(10) . . ? S17 Ni10 S19 98.8(2) . . ? S17 Ni10 S20 174.1(2) . . ? S19 Ni10 S20 82.25(19) . . ? S17 Ni10 S18 83.21(19) . . ? S19 Ni10 S18 175.8(2) . . ? S20 Ni10 S18 95.4(2) . . ? S17 Ni10 Ni9 48.06(14) . . ? S19 Ni10 Ni9 130.56(16) . . ? S20 Ni10 Ni9 127.24(17) . . ? S18 Ni10 Ni9 48.66(13) . . ? S22 Ni11 S20 100.0(2) . . ? S22 Ni11 S19 171.4(2) . . ? S20 Ni11 S19 81.9(2) . . ? S22 Ni11 S21 82.9(2) . . ? S20 Ni11 S21 175.1(2) . . ? S19 Ni11 S21 94.6(2) . . ? S22 Ni11 Ni1 49.33(13) . . ? S20 Ni11 Ni1 130.06(19) . . ? S19 Ni11 Ni1 123.28(15) . . ? S21 Ni11 Ni1 49.43(15) . . ? C10 S1 Ni2 109.9(4) . . ? C10 S1 Ni1 113.8(5) . . ? Ni2 S1 Ni1 82.03(17) . . ? C20 S2 Ni2 108.5(4) . . ? C20 S2 Ni1 99.8(4) . . ? Ni2 S2 Ni1 82.06(18) . . ? C30 S3 Ni3 108.5(4) . . ? C30 S3 Ni2 107.0(4) . . ? Ni3 S3 Ni2 92.5(2) . . ? C41 S4 Ni2 112.4(6) . . ? C41 S4 Ni3 105.2(6) . . ? Ni2 S4 Ni3 92.7(2) . . ? C50 S5 Ni4 105.8(5) . . ? C50 S5 Ni3 104.8(5) . . ? Ni4 S5 Ni3 82.32(17) . . ? C60 S6 Ni4 110.0(4) . . ? C60 S6 Ni3 111.2(4) . . ? Ni4 S6 Ni3 82.13(19) . . ? C70 S7 Ni5 103.0(5) . . ? C70 S7 Ni4 105.4(5) . . ? Ni5 S7 Ni4 81.52(18) . . ? C80 S8 Ni4 110.1(4) . . ? C80 S8 Ni5 107.1(4) . . ? Ni4 S8 Ni5 81.58(17) . . ? C90 S9 Ni5 104.2(4) . . ? C90 S9 Ni6 108.4(4) . . ? Ni5 S9 Ni6 94.3(2) . . ? C100 S10 Ni6 111.1(4) . . ? C100 S10 Ni5 108.1(4) . . ? Ni6 S10 Ni5 94.8(2) . . ? C110 S11 Ni6 116.6(4) . . ? C110 S11 Ni7 114.6(4) . . ? Ni6 S11 Ni7 80.88(17) . . ? C120 S12 Ni7 117.4(4) . . ? C120 S12 Ni6 113.1(4) . . ? Ni7 S12 Ni6 80.73(18) . . ? C130 S13 Ni7 108.2(5) . . ? C130 S13 Ni8 111.9(4) . . ? Ni7 S13 Ni8 96.8(2) . . ? C140 S14 C240 12(2) . . ? C140 S14 Ni7 108.2(13) . . ? C240 S14 Ni7 97.5(17) . . ? C140 S14 Ni8 103.6(11) . . ? C240 S14 Ni8 99.4(12) . . ? Ni7 S14 Ni8 94.8(2) . . ? C150 S15 Ni9 103.0(5) . . ? C150 S15 Ni8 102.4(5) . . ? Ni9 S15 Ni8 82.6(2) . . ? C160 S16 Ni9 111.0(6) . . ? C160 S16 Ni8 109.8(5) . . ? Ni9 S16 Ni8 82.98(19) . . ? C170 S17 Ni10 109.7(4) . . ? C170 S17 Ni9 108.9(4) . . ? Ni10 S17 Ni9 84.0(2) . . ? C180 S18 Ni9 99.3(5) . . ? C180 S18 Ni10 106.7(5) . . ? Ni9 S18 Ni10 82.63(17) . . ? C195 S19 Ni10 108.3(6) . . ? C195 S19 Ni11 111.5(5) . . ? Ni10 S19 Ni11 93.2(2) . . ? C200 S20 Ni10 108.8(5) . . ? C200 S20 Ni11 107.1(5) . . ? Ni10 S20 Ni11 92.9(2) . . ? C210 S21 Ni11 107.6(6) . . ? C210 S21 Ni1 100.6(6) . . ? Ni11 S21 Ni1 81.4(2) . . ? C220 S22 Ni11 111.2(4) . . ? C220 S22 Ni1 115.6(5) . . ? Ni11 S22 Ni1 82.01(18) . . ? C11 C10 C15 120.0 . . ? C11 C10 S1 122.5(9) . . ? C15 C10 S1 117.5(9) . . ? C10 C11 C12 120.0 . . ? C11 C12 C13 120.0 . . ? C14 C13 C12 120.0 . . ? C13 C14 C15 120.0 . . ? C14 C15 C10 120.0 . . ? C21 C20 C25 120.0 . . ? C21 C20 S2 121.3(8) . . ? C25 C20 S2 118.4(8) . . ? C20 C21 C22 120.0 . . ? C23 C22 C21 120.0 . . ? C22 C23 C24 120.0 . . ? C25 C24 C23 120.0 . . ? C24 C25 C20 120.0 . . ? C31 C30 C35 120.0 . . ? C31 C30 S3 118.8(7) . . ? C35 C30 S3 121.2(7) . . ? C30 C31 C32 120.0 . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C33 C34 C35 120.0 . . ? C34 C35 C30 120.0 . . ? C41 C40 C45 120.0 . . ? C40 C41 C42 120.0 . . ? C40 C41 S4 121.0(14) . . ? C42 C41 S4 118.8(14) . . ? C43 C42 C41 120.0 . . ? C42 C43 C44 120.0 . . ? C43 C44 C45 120.0 . . ? C44 C45 C40 120.0 . . ? C51 C50 C55 120.0 . . ? C51 C50 S5 119.9(12) . . ? C55 C50 S5 119.9(12) . . ? C50 C51 C52 120.0 . . ? C51 C52 C53 120.0 . . ? C54 C53 C52 120.0 . . ? C55 C54 C53 120.0 . . ? C54 C55 C50 120.0 . . ? C61 C60 C65 120.0 . . ? C61 C60 S6 118.6(9) . . ? C65 C60 S6 121.4(9) . . ? C62 C61 C60 120.0 . . ? C61 C62 C63 120.0 . . ? C64 C63 C62 120.0 . . ? C65 C64 C63 120.0 . . ? C64 C65 C60 120.0 . . ? C71 C70 C75 120.0 . . ? C71 C70 S7 119.9(9) . . ? C75 C70 S7 119.8(9) . . ? C70 C71 C72 120.0 . . ? C73 C72 C71 120.0 . . ? C74 C73 C72 120.0 . . ? C75 C74 C73 120.0 . . ? C74 C75 C70 120.0 . . ? C81 C80 C85 120.0 . . ? C81 C80 S8 116.8(7) . . ? C85 C80 S8 123.0(7) . . ? C82 C81 C80 120.0 . . ? C81 C82 C83 120.0 . . ? C82 C83 C84 120.0 . . ? C85 C84 C83 120.0 . . ? C84 C85 C80 120.0 . . ? C91 C90 C95 120.0 . . ? C91 C90 S9 118.9(8) . . ? C95 C90 S9 121.1(8) . . ? C90 C91 C92 120.0 . . ? C91 C92 C93 120.0 . . ? C94 C93 C92 120.0 . . ? C95 C94 C93 120.0 . . ? C94 C95 C90 120.0 . . ? C101 C100 C105 120.0 . . ? C101 C100 S10 121.2(8) . . ? C105 C100 S10 118.7(8) . . ? C100 C101 C102 120.0 . . ? C103 C102 C101 120.0 . . ? C102 C103 C104 120.0 . . ? C103 C104 C105 120.0 . . ? C104 C105 C100 120.0 . . ? C111 C110 C115 120.0 . . ? C111 C110 S11 116.2(8) . . ? C115 C110 S11 123.8(8) . . ? C110 C111 C112 120.0 . . ? C111 C112 C113 120.0 . . ? C114 C113 C112 120.0 . . ? C115 C114 C113 120.0 . . ? C114 C115 C110 120.0 . . ? C121 C120 C125 120.0 . . ? C121 C120 S12 117.6(8) . . ? C125 C120 S12 122.4(8) . . ? C120 C121 C122 120.0 . . ? C121 C122 C123 120.0 . . ? C124 C123 C122 120.0 . . ? C123 C124 C125 120.0 . . ? C124 C125 C120 120.0 . . ? C131 C130 C135 120.0 . . ? C131 C130 S13 121.8(10) . . ? C135 C130 S13 118.2(10) . . ? C130 C131 C132 120.0 . . ? C133 C132 C131 120.0 . . ? C132 C133 C134 120.0 . . ? C135 C134 C133 120.0 . . ? C134 C135 C130 120.0 . . ? C145 C140 C141 120.0 . . ? C145 C140 S14 119(2) . . ? C141 C140 S14 120(2) . . ? C140 C145 C144 120.0 . . ? C145 C144 C143 120.0 . . ? C144 C143 C142 120.0 . . ? C141 C142 C143 120.0 . . ? C142 C141 C140 120.0 . . ? C241 C240 C245 120.0 . . ? C241 C240 S14 123(2) . . ? C245 C240 S14 117(2) . . ? C240 C241 C242 120.0 . . ? C243 C242 C241 120.0 . . ? C242 C243 C244 120.0 . . ? C243 C244 C245 120.0 . . ? C244 C245 C240 120.0 . . ? C151 C150 C155 120.0 . . ? C151 C150 S15 119.9(10) . . ? C155 C150 S15 120.1(10) . . ? C150 C151 C152 120.0 . . ? C151 C152 C153 120.0 . . ? C154 C153 C152 120.0 . . ? C153 C154 C155 120.0 . . ? C154 C155 C150 120.0 . . ? C161 C160 C165 120.0 . . ? C161 C160 S16 122.8(12) . . ? C165 C160 S16 117.2(12) . . ? C162 C161 C160 120.0 . . ? C161 C162 C163 120.0 . . ? C164 C163 C162 120.0 . . ? C163 C164 C165 120.0 . . ? C164 C165 C160 120.0 . . ? C171 C170 C175 120.0 . . ? C171 C170 S17 117.8(8) . . ? C175 C170 S17 122.1(8) . . ? C172 C171 C170 120.0 . . ? C171 C172 C173 120.0 . . ? C174 C173 C172 120.0 . . ? C173 C174 C175 120.0 . . ? C174 C175 C170 120.0 . . ? C181 C180 C185 120.0 . . ? C181 C180 S18 118.4(12) . . ? C185 C180 S18 121.6(12) . . ? C180 C181 C182 120.0 . . ? C183 C182 C181 120.0 . . ? C184 C183 C182 120.0 . . ? C183 C184 C185 120.0 . . ? C184 C185 C180 120.0 . . ? C191 C190 C195 120.0 . . ? C190 C191 C192 120.0 . . ? C191 C192 C193 120.0 . . ? C192 C193 C194 120.0 . . ? C195 C194 C193 120.0 . . ? C194 C195 C190 120.0 . . ? C194 C195 S19 122.8(14) . . ? C190 C195 S19 117.0(14) . . ? C201 C200 C205 120.0 . . ? C201 C200 S20 118.7(10) . . ? C205 C200 S20 121.3(10) . . ? C202 C201 C200 120.0 . . ? C201 C202 C203 120.0 . . ? C204 C203 C202 120.0 . . ? C203 C204 C205 120.0 . . ? C204 C205 C200 120.0 . . ? C211 C210 C215 120.0 . . ? C211 C210 S21 122.6(12) . . ? C215 C210 S21 117.3(12) . . ? C212 C211 C210 120.0 . . ? C213 C212 C211 120.0 . . ? C214 C213 C212 120.0 . . ? C213 C214 C215 120.0 . . ? C214 C215 C210 120.0 . . ? C221 C220 C225 120.0 . . ? C221 C220 S22 123.6(12) . . ? C225 C220 S22 116.4(12) . . ? C222 C221 C220 120.0 . . ? C221 C222 C223 120.0 . . ? C224 C223 C222 120.0 . . ? C223 C224 C225 120.0 . . ? C224 C225 C220 120.0 . . ? C1A O1A C4A 93.6(18) . . ? C4B O1B C1B 96(3) . . ? C1C O1C C4C 102(3) . . ? C1D O1D C4D 101.7(11) . . ? C4E O1E C1E 90(3) . . ? O1A C1A C2A 116.3(17) . . ? C1A C2A C3A 101.4(7) . . ? C4A C3A C2A 101.4(7) . . ? O1A C4A C3A 115.3(18) . . ? O1B C1B C2B 112(3) . . ? C1B C2B C3B 100.7(8) . . ? C4B C3B C2B 100.7(8) . . ? O1B C4B C3B 105(4) . . ? O1C C1C C2C 102(4) . . ? C1C C2C C3C 100.5(8) . . ? C4C C3C C2C 100.4(8) . . ? O1C C4C C3C 110(3) . . ? O1D C1D C2D 112.1(12) . . ? C1D C2D C3D 100.6(8) . . ? C4D C3D C2D 100.6(8) . . ? O1D C4D C3D 112.6(12) . . ? O1E C1E C2E 115.5(15) . . ? C1E C2E C3E 91(3) . . ? C4E C3E C2E 106.1(16) . . ? O1E C4E C3E 112.8(14) . . ? 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 S2 Ni1 Ni2 S1 -122.2(2) . . . . ? S22 Ni1 Ni2 S1 -177.0(3) . . . . ? S21 Ni1 Ni2 S1 57.3(2) . . . . ? Ni11 Ni1 Ni2 S1 120.2(2) . . . . ? S2 Ni1 Ni2 S4 64.6(2) . . . . ? S1 Ni1 Ni2 S4 -173.2(3) . . . . ? S22 Ni1 Ni2 S4 9.9(3) . . . . ? S21 Ni1 Ni2 S4 -115.9(3) . . . . ? Ni11 Ni1 Ni2 S4 -53.0(2) . . . . ? S1 Ni1 Ni2 S2 122.2(2) . . . . ? S22 Ni1 Ni2 S2 -54.8(3) . . . . ? S21 Ni1 Ni2 S2 179.5(3) . . . . ? Ni11 Ni1 Ni2 S2 -117.62(19) . . . . ? S2 Ni1 Ni2 S3 174.7(2) . . . . ? S1 Ni1 Ni2 S3 -63.1(2) . . . . ? S22 Ni1 Ni2 S3 119.9(3) . . . . ? S21 Ni1 Ni2 S3 -5.8(3) . . . . ? Ni11 Ni1 Ni2 S3 57.1(2) . . . . ? S4 Ni3 Ni4 S6 -59.6(3) . . . . ? S3 Ni3 Ni4 S6 -176.4(2) . . . . ? S5 Ni3 Ni4 S6 123.0(2) . . . . ? S4 Ni3 Ni4 S8 114.2(3) . . . . ? S3 Ni3 Ni4 S8 -2.5(3) . . . . ? S5 Ni3 Ni4 S8 -63.2(2) . . . . ? S6 Ni3 Ni4 S8 173.8(2) . . . . ? S4 Ni3 Ni4 S5 177.4(3) . . . . ? S3 Ni3 Ni4 S5 60.6(2) . . . . ? S6 Ni3 Ni4 S5 -123.0(2) . . . . ? S4 Ni3 Ni4 S7 -3.2(3) . . . . ? S3 Ni3 Ni4 S7 -119.9(3) . . . . ? S5 Ni3 Ni4 S7 179.4(3) . . . . ? S6 Ni3 Ni4 S7 56.4(2) . . . . ? S4 Ni3 Ni4 Ni5 55.4(3) . . . . ? S3 Ni3 Ni4 Ni5 -61.3(2) . . . . ? S5 Ni3 Ni4 Ni5 -121.9(2) . . . . ? S6 Ni3 Ni4 Ni5 115.06(19) . . . . ? S6 Ni4 Ni5 S9 113.9(3) . . . . ? S8 Ni4 Ni5 S9 -60.6(2) . . . . ? S5 Ni4 Ni5 S9 -3.2(3) . . . . ? S7 Ni4 Ni5 S9 176.0(2) . . . . ? Ni3 Ni4 Ni5 S9 55.4(2) . . . . ? S6 Ni4 Ni5 S10 -1.5(3) . . . . ? S8 Ni4 Ni5 S10 -176.0(3) . . . . ? S5 Ni4 Ni5 S10 -118.6(3) . . . . ? S7 Ni4 Ni5 S10 60.6(2) . . . . ? Ni3 Ni4 Ni5 S10 -60.0(2) . . . . ? S6 Ni4 Ni5 S7 -62.1(2) . . . . ? S8 Ni4 Ni5 S7 123.4(2) . . . . ? S5 Ni4 Ni5 S7 -179.2(2) . . . . ? Ni3 Ni4 Ni5 S7 -120.63(18) . . . . ? S6 Ni4 Ni5 S8 174.6(3) . . . . ? S5 Ni4 Ni5 S8 57.4(2) . . . . ? S7 Ni4 Ni5 S8 -123.4(2) . . . . ? Ni3 Ni4 Ni5 S8 116.0(2) . . . . ? S10 Ni6 Ni7 S13 107.9(2) . . . . ? S11 Ni6 Ni7 S13 -69.5(2) . . . . ? S9 Ni6 Ni7 S13 -1.1(3) . . . . ? S12 Ni6 Ni7 S13 179.7(2) . . . . ? S10 Ni6 Ni7 S12 -71.9(2) . . . . ? S11 Ni6 Ni7 S12 110.7(2) . . . . ? S9 Ni6 Ni7 S12 179.1(2) . . . . ? S10 Ni6 Ni7 S11 177.4(2) . . . . ? S9 Ni6 Ni7 S11 68.4(2) . . . . ? S12 Ni6 Ni7 S11 -110.7(2) . . . . ? S10 Ni6 Ni7 S14 -6.3(3) . . . . ? S11 Ni6 Ni7 S14 176.2(3) . . . . ? S9 Ni6 Ni7 S14 -115.3(3) . . . . ? S12 Ni6 Ni7 S14 65.5(3) . . . . ? S13 Ni8 Ni9 S17 3.8(3) . . . . ? S16 Ni8 Ni9 S17 175.8(3) . . . . ? S15 Ni8 Ni9 S17 -58.9(2) . . . . ? S14 Ni8 Ni9 S17 123.4(3) . . . . ? S13 Ni8 Ni9 S16 -172.0(3) . . . . ? S15 Ni8 Ni9 S16 125.3(2) . . . . ? S14 Ni8 Ni9 S16 -52.3(3) . . . . ? S13 Ni8 Ni9 S15 62.7(2) . . . . ? S16 Ni8 Ni9 S15 -125.3(2) . . . . ? S14 Ni8 Ni9 S15 -177.6(3) . . . . ? S13 Ni8 Ni9 S18 -120.9(3) . . . . ? S16 Ni8 Ni9 S18 51.1(3) . . . . ? S15 Ni8 Ni9 S18 176.4(3) . . . . ? S14 Ni8 Ni9 S18 -1.3(3) . . . . ? S13 Ni8 Ni9 Ni10 -57.1(2) . . . . ? S16 Ni8 Ni9 Ni10 114.9(2) . . . . ? S15 Ni8 Ni9 Ni10 -119.85(19) . . . . ? S14 Ni8 Ni9 Ni10 62.5(2) . . . . ? S16 Ni9 Ni10 S17 175.6(2) . . . . ? S15 Ni9 Ni10 S17 49.8(3) . . . . ? S18 Ni9 Ni10 S17 -125.4(3) . . . . ? Ni8 Ni9 Ni10 S17 113.42(19) . . . . ? S17 Ni9 Ni10 S19 -60.0(3) . . . . ? S16 Ni9 Ni10 S19 115.5(3) . . . . ? S15 Ni9 Ni10 S19 -10.2(4) . . . . ? S18 Ni9 Ni10 S19 174.6(3) . . . . ? Ni8 Ni9 Ni10 S19 53.4(3) . . . . ? S17 Ni9 Ni10 S20 -175.4(2) . . . . ? S16 Ni9 Ni10 S20 0.2(3) . . . . ? S15 Ni9 Ni10 S20 -125.5(3) . . . . ? S18 Ni9 Ni10 S20 59.3(3) . . . . ? Ni8 Ni9 Ni10 S20 -62.0(2) . . . . ? S17 Ni9 Ni10 S18 125.4(3) . . . . ? S16 Ni9 Ni10 S18 -59.0(3) . . . . ? S15 Ni9 Ni10 S18 175.2(3) . . . . ? Ni8 Ni9 Ni10 S18 -121.2(2) . . . . ? S2 Ni1 Ni11 S22 58.1(3) . . . . ? S1 Ni1 Ni11 S22 -176.4(3) . . . . ? S21 Ni1 Ni11 S22 -121.5(3) . . . . ? Ni2 Ni1 Ni11 S22 120.7(2) . . . . ? S2 Ni1 Ni11 S20 -6.8(3) . . . . ? S1 Ni1 Ni11 S20 118.6(3) . . . . ? S22 Ni1 Ni11 S20 -65.0(3) . . . . ? S21 Ni1 Ni11 S20 173.6(3) . . . . ? Ni2 Ni1 Ni11 S20 55.7(2) . . . . ? S2 Ni1 Ni11 S19 -116.3(3) . . . . ? S1 Ni1 Ni11 S19 9.2(3) . . . . ? S22 Ni1 Ni11 S19 -174.4(3) . . . . ? S21 Ni1 Ni11 S19 64.1(3) . . . . ? Ni2 Ni1 Ni11 S19 -53.7(3) . . . . ? S2 Ni1 Ni11 S21 179.6(3) . . . . ? S1 Ni1 Ni11 S21 -55.0(3) . . . . ? S22 Ni1 Ni11 S21 121.5(3) . . . . ? Ni2 Ni1 Ni11 S21 -117.9(2) . . . . ? S4 Ni2 S1 C10 -74.5(13) . . . . ? S2 Ni2 S1 C10 -152.6(5) . . . . ? S3 Ni2 S1 C10 24.0(5) . . . . ? Ni1 Ni2 S1 C10 -112.5(5) . . . . ? S4 Ni2 S1 Ni1 38.1(13) . . . . ? S2 Ni2 S1 Ni1 -40.08(16) . . . . ? S3 Ni2 S1 Ni1 136.57(17) . . . . ? S2 Ni1 S1 C10 148.4(5) . . . . ? S22 Ni1 S1 C10 -116(4) . . . . ? S21 Ni1 S1 C10 -32.1(5) . . . . ? Ni11 Ni1 S1 C10 6.6(6) . . . . ? Ni2 Ni1 S1 C10 108.3(5) . . . . ? S2 Ni1 S1 Ni2 40.07(16) . . . . ? S22 Ni1 S1 Ni2 136(4) . . . . ? S21 Ni1 S1 Ni2 -140.37(18) . . . . ? Ni11 Ni1 S1 Ni2 -101.7(2) . . . . ? S1 Ni2 S2 C20 -57.5(5) . . . . ? S4 Ni2 S2 C20 131.6(5) . . . . ? S3 Ni2 S2 C20 177(100) . . . . ? Ni1 Ni2 S2 C20 -97.7(5) . . . . ? S1 Ni2 S2 Ni1 40.22(16) . . . . ? S4 Ni2 S2 Ni1 -130.69(18) . . . . ? S3 Ni2 S2 Ni1 -85(3) . . . . ? S1 Ni1 S2 C20 67.6(4) . . . . ? S22 Ni1 S2 C20 -109.2(4) . . . . ? S21 Ni1 S2 C20 -13(31) . . . . ? Ni11 Ni1 S2 C20 -149.3(4) . . . . ? Ni2 Ni1 S2 C20 107.5(4) . . . . ? S1 Ni1 S2 Ni2 -39.95(15) . . . . ? S22 Ni1 S2 Ni2 143.24(17) . . . . ? S21 Ni1 S2 Ni2 -121(31) . . . . ? Ni11 Ni1 S2 Ni2 103.18(17) . . . . ? S4 Ni3 S3 C30 133.5(4) . . . . ? S5 Ni3 S3 C30 -46.7(4) . . . . ? S6 Ni3 S3 C30 -116.9(19) . . . . ? Ni4 Ni3 S3 C30 -88.0(4) . . . . ? S4 Ni3 S3 Ni2 24.59(17) . . . . ? S5 Ni3 S3 Ni2 -155.61(17) . . . . ? S6 Ni3 S3 Ni2 134.2(19) . . . . ? Ni4 Ni3 S3 Ni2 163.16(12) . . . . ? S1 Ni2 S3 C30 54.4(5) . . . . ? S4 Ni2 S3 C30 -134.9(5) . . . . ? S2 Ni2 S3 C30 179(100) . . . . ? Ni1 Ni2 S3 C30 97.6(5) . . . . ? S1 Ni2 S3 Ni3 164.57(17) . . . . ? S4 Ni2 S3 Ni3 -24.66(18) . . . . ? S2 Ni2 S3 Ni3 -71(3) . . . . ? Ni1 Ni2 S3 Ni3 -152.22(14) . . . . ? S1 Ni2 S4 C41 -127.8(13) . . . . ? S2 Ni2 S4 C41 -50.6(7) . . . . ? S3 Ni2 S4 C41 132.3(7) . . . . ? Ni1 Ni2 S4 C41 -93.9(7) . . . . ? S1 Ni2 S4 Ni3 124.6(12) . . . . ? S2 Ni2 S4 Ni3 -158.27(19) . . . . ? S3 Ni2 S4 Ni3 24.65(19) . . . . ? Ni1 Ni2 S4 Ni3 158.51(14) . . . . ? S3 Ni3 S4 C41 -138.8(6) . . . . ? S5 Ni3 S4 C41 -143(5) . . . . ? S6 Ni3 S4 C41 46.6(6) . . . . ? Ni4 Ni3 S4 C41 87.6(6) . . . . ? S3 Ni3 S4 Ni2 -24.68(18) . . . . ? S5 Ni3 S4 Ni2 -29(5) . . . . ? S6 Ni3 S4 Ni2 160.72(18) . . . . ? Ni4 Ni3 S4 Ni2 -158.29(16) . . . . ? S6 Ni4 S5 C50 63.4(6) . . . . ? S8 Ni4 S5 C50 -122.6(6) . . . . ? S7 Ni4 S5 C50 69(16) . . . . ? Ni5 Ni4 S5 C50 -162.8(6) . . . . ? Ni3 Ni4 S5 C50 103.3(6) . . . . ? S6 Ni4 S5 Ni3 -39.85(18) . . . . ? S8 Ni4 S5 Ni3 134.09(18) . . . . ? S7 Ni4 S5 Ni3 -34(16) . . . . ? Ni5 Ni4 S5 Ni3 93.90(19) . . . . ? S4 Ni3 S5 C50 125(5) . . . . ? S3 Ni3 S5 C50 120.3(5) . . . . ? S6 Ni3 S5 C50 -65.1(5) . . . . ? Ni4 Ni3 S5 C50 -104.4(5) . . . . ? S4 Ni3 S5 Ni4 -131(5) . . . . ? S3 Ni3 S5 Ni4 -135.36(18) . . . . ? S6 Ni3 S5 Ni4 39.29(17) . . . . ? S8 Ni4 S6 C60 55(2) . . . . ? S5 Ni4 S6 C60 149.3(5) . . . . ? S7 Ni4 S6 C60 -30.7(5) . . . . ? Ni5 Ni4 S6 C60 11.4(5) . . . . ? Ni3 Ni4 S6 C60 109.8(5) . . . . ? S8 Ni4 S6 Ni3 -55(2) . . . . ? S5 Ni4 S6 Ni3 39.47(17) . . . . ? S7 Ni4 S6 Ni3 -140.46(17) . . . . ? Ni5 Ni4 S6 Ni3 -98.38(18) . . . . ? S4 Ni3 S6 C60 31.5(5) . . . . ? S3 Ni3 S6 C60 -77(2) . . . . ? S5 Ni3 S6 C60 -148.0(4) . . . . ? Ni4 Ni3 S6 C60 -108.5(4) . . . . ? S4 Ni3 S6 Ni4 140.02(18) . . . . ? S3 Ni3 S6 Ni4 31(2) . . . . ? S5 Ni3 S6 Ni4 -39.54(16) . . . . ? S9 Ni5 S7 C70 167(4) . . . . ? S10 Ni5 S7 C70 120.7(5) . . . . ? S8 Ni5 S7 C70 -64.6(5) . . . . ? Ni4 Ni5 S7 C70 -103.9(5) . . . . ? S9 Ni5 S7 Ni4 -90(4) . . . . ? S10 Ni5 S7 Ni4 -135.37(16) . . . . ? S8 Ni5 S7 Ni4 39.35(15) . . . . ? S6 Ni4 S7 C70 -124.5(5) . . . . ? S8 Ni4 S7 C70 61.5(5) . . . . ? S5 Ni4 S7 C70 -130(16) . . . . ? Ni5 Ni4 S7 C70 101.2(5) . . . . ? Ni3 Ni4 S7 C70 -164.0(5) . . . . ? S6 Ni4 S7 Ni5 134.27(17) . . . . ? S8 Ni4 S7 Ni5 -39.68(16) . . . . ? S5 Ni4 S7 Ni5 128(16) . . . . ? Ni3 Ni4 S7 Ni5 94.8(2) . . . . ? S6 Ni4 S8 C80 58(2) . . . . ? S5 Ni4 S8 C80 -35.3(4) . . . . ? S7 Ni4 S8 C80 144.5(4) . . . . ? Ni5 Ni4 S8 C80 105.2(4) . . . . ? Ni3 Ni4 S8 C80 7.3(5) . . . . ? S6 Ni4 S8 Ni5 -47(2) . . . . ? S5 Ni4 S8 Ni5 -140.50(18) . . . . ? S7 Ni4 S8 Ni5 39.34(17) . . . . ? Ni3 Ni4 S8 Ni5 -97.89(18) . . . . ? S9 Ni5 S8 C80 29.4(4) . . . . ? S10 Ni5 S8 C80 -73(3) . . . . ? S7 Ni5 S8 C80 -148.3(4) . . . . ? Ni4 Ni5 S8 C80 -108.5(4) . . . . ? S9 Ni5 S8 Ni4 137.88(17) . . . . ? S10 Ni5 S8 Ni4 36(2) . . . . ? S7 Ni5 S8 Ni4 -39.73(16) . . . . ? S10 Ni5 S9 C90 -126.4(4) . . . . ? S7 Ni5 S9 C90 -172(4) . . . . ? S8 Ni5 S9 C90 58.9(4) . . . . ? Ni4 Ni5 S9 C90 100.6(4) . . . . ? S10 Ni5 S9 Ni6 -16.21(16) . . . . ? S7 Ni5 S9 Ni6 -62(4) . . . . ? S8 Ni5 S9 Ni6 169.15(17) . . . . ? Ni4 Ni5 S9 Ni6 -149.22(13) . . . . ? S10 Ni6 S9 C90 122.9(5) . . . . ? S11 Ni6 S9 C90 -63.7(5) . . . . ? S12 Ni6 S9 C90 -99(3) . . . . ? Ni7 Ni6 S9 C90 -109.6(5) . . . . ? S10 Ni6 S9 Ni5 16.35(17) . . . . ? S11 Ni6 S9 Ni5 -170.18(16) . . . . ? S12 Ni6 S9 Ni5 155(3) . . . . ? Ni7 Ni6 S9 Ni5 143.90(14) . . . . ? S11 Ni6 S10 C100 117.9(16) . . . . ? S9 Ni6 S10 C100 -127.9(4) . . . . ? S12 Ni6 S10 C100 54.5(4) . . . . ? Ni7 Ni6 S10 C100 101.6(4) . . . . ? S11 Ni6 S10 Ni5 -130.6(16) . . . . ? S9 Ni6 S10 Ni5 -16.34(17) . . . . ? S12 Ni6 S10 Ni5 166.06(18) . . . . ? Ni7 Ni6 S10 Ni5 -146.87(14) . . . . ? S9 Ni5 S10 C100 130.5(4) . . . . ? S7 Ni5 S10 C100 -51.7(4) . . . . ? S8 Ni5 S10 C100 -127(2) . . . . ? Ni4 Ni5 S10 C100 -93.4(4) . . . . ? S9 Ni5 S10 Ni6 16.39(17) . . . . ? S7 Ni5 S10 Ni6 -165.81(18) . . . . ? S8 Ni5 S10 Ni6 119(2) . . . . ? Ni4 Ni5 S10 Ni6 152.49(14) . . . . ? S10 Ni6 S11 C110 95.2(16) . . . . ? S9 Ni6 S11 C110 -18.2(4) . . . . ? S12 Ni6 S11 C110 159.7(4) . . . . ? Ni7 Ni6 S11 C110 113.0(4) . . . . ? S10 Ni6 S11 Ni7 -17.8(17) . . . . ? S9 Ni6 S11 Ni7 -131.17(16) . . . . ? S12 Ni6 S11 Ni7 46.73(16) . . . . ? S13 Ni7 S11 C110 13.3(5) . . . . ? S12 Ni7 S11 C110 -162.2(5) . . . . ? S14 Ni7 S11 C110 167(4) . . . . ? Ni6 Ni7 S11 C110 -115.2(5) . . . . ? S13 Ni7 S11 Ni6 128.43(17) . . . . ? S12 Ni7 S11 Ni6 -46.99(16) . . . . ? S14 Ni7 S11 Ni6 -77(4) . . . . ? S13 Ni7 S12 C120 109.1(19) . . . . ? S11 Ni7 S12 C120 158.0(5) . . . . ? S14 Ni7 S12 C120 -23.5(5) . . . . ? Ni6 Ni7 S12 C120 111.3(5) . . . . ? S13 Ni7 S12 Ni6 -2.1(19) . . . . ? S11 Ni7 S12 Ni6 46.72(15) . . . . ? S14 Ni7 S12 Ni6 -134.80(18) . . . . ? S10 Ni6 S12 C120 10.7(5) . . . . ? S11 Ni6 S12 C120 -162.8(5) . . . . ? S9 Ni6 S12 C120 -127(3) . . . . ? Ni7 Ni6 S12 C120 -116.0(5) . . . . ? S10 Ni6 S12 Ni7 126.67(17) . . . . ? S11 Ni6 S12 Ni7 -46.86(16) . . . . ? S9 Ni6 S12 Ni7 -11(3) . . . . ? S12 Ni7 S13 C130 106.4(19) . . . . ? S11 Ni7 S13 C130 58.3(5) . . . . ? S14 Ni7 S13 C130 -120.4(5) . . . . ? Ni6 Ni7 S13 C130 104.4(5) . . . . ? S12 Ni7 S13 Ni8 -137.8(18) . . . . ? S11 Ni7 S13 Ni8 174.13(18) . . . . ? S14 Ni7 S13 Ni8 -4.57(19) . . . . ? Ni6 Ni7 S13 Ni8 -139.81(14) . . . . ? S16 Ni8 S13 C130 -135.6(14) . . . . ? S15 Ni8 S13 C130 -58.1(5) . . . . ? S14 Ni8 S13 C130 117.3(5) . . . . ? Ni9 Ni8 S13 C130 -100.1(5) . . . . ? S16 Ni8 S13 Ni7 111.6(14) . . . . ? S15 Ni8 S13 Ni7 -170.88(18) . . . . ? S14 Ni8 S13 Ni7 4.57(19) . . . . ? Ni9 Ni8 S13 Ni7 147.17(14) . . . . ? S13 Ni7 S14 C140 110.6(12) . . . . ? S12 Ni7 S14 C140 -73.9(12) . . . . ? S11 Ni7 S14 C140 -44(4) . . . . ? Ni6 Ni7 S14 C140 -118.7(12) . . . . ? S13 Ni7 S14 C240 104.6(12) . . . . ? S12 Ni7 S14 C240 -79.8(12) . . . . ? S11 Ni7 S14 C240 -50(4) . . . . ? Ni6 Ni7 S14 C240 -124.7(12) . . . . ? S13 Ni7 S14 Ni8 4.50(19) . . . . ? S12 Ni7 S14 Ni8 -179.95(18) . . . . ? S11 Ni7 S14 Ni8 -150(4) . . . . ? Ni6 Ni7 S14 Ni8 135.20(17) . . . . ? S13 Ni8 S14 C140 -114.5(13) . . . . ? S16 Ni8 S14 C140 75.5(13) . . . . ? S15 Ni8 S14 C140 -46(2) . . . . ? Ni9 Ni8 S14 C140 112.3(13) . . . . ? S13 Ni8 S14 C240 -102.9(17) . . . . ? S16 Ni8 S14 C240 87.1(17) . . . . ? S15 Ni8 S14 C240 -35(3) . . . . ? Ni9 Ni8 S14 C240 123.9(17) . . . . ? S13 Ni8 S14 Ni7 -4.46(19) . . . . ? S16 Ni8 S14 Ni7 -174.46(19) . . . . ? S15 Ni8 S14 Ni7 64(2) . . . . ? Ni9 Ni8 S14 Ni7 -137.61(16) . . . . ? S17 Ni9 S15 C150 -121.1(5) . . . . ? S16 Ni9 S15 C150 63.1(5) . . . . ? S18 Ni9 S15 C150 -39(3) . . . . ? Ni8 Ni9 S15 C150 101.1(6) . . . . ? Ni10 Ni9 S15 C150 -155.9(5) . . . . ? S17 Ni9 S15 Ni8 137.79(17) . . . . ? S16 Ni9 S15 Ni8 -38.05(17) . . . . ? S18 Ni9 S15 Ni8 -140(3) . . . . ? Ni10 Ni9 S15 Ni8 103.0(2) . . . . ? S13 Ni8 S15 C150 126.3(5) . . . . ? S16 Ni8 S15 C150 -63.8(5) . . . . ? S14 Ni8 S15 C150 59(2) . . . . ? Ni9 Ni8 S15 C150 -101.7(5) . . . . ? S13 Ni8 S15 Ni9 -131.94(17) . . . . ? S16 Ni8 S15 Ni9 37.90(16) . . . . ? S14 Ni8 S15 Ni9 160(2) . . . . ? S17 Ni9 S16 C160 56(3) . . . . ? S15 Ni9 S16 C160 146.7(6) . . . . ? S18 Ni9 S16 C160 -37.3(6) . . . . ? Ni8 Ni9 S16 C160 108.5(6) . . . . ? Ni10 Ni9 S16 C160 3.2(6) . . . . ? S17 Ni9 S16 Ni8 -53(3) . . . . ? S15 Ni9 S16 Ni8 38.15(18) . . . . ? S18 Ni9 S16 Ni8 -145.84(18) . . . . ? Ni10 Ni9 S16 Ni8 -105.35(18) . . . . ? S13 Ni8 S16 C160 -69.4(16) . . . . ? S15 Ni8 S16 C160 -147.9(6) . . . . ? S14 Ni8 S16 C160 36.3(6) . . . . ? Ni9 Ni8 S16 C160 -109.8(6) . . . . ? S13 Ni8 S16 Ni9 40.4(15) . . . . ? S15 Ni8 S16 Ni9 -38.04(17) . . . . ? S14 Ni8 S16 Ni9 146.15(19) . . . . ? S19 Ni10 S17 C170 30.3(5) . . . . ? S20 Ni10 S17 C170 -69(2) . . . . ? S18 Ni10 S17 C170 -146.0(5) . . . . ? Ni9 Ni10 S17 C170 -107.9(5) . . . . ? S19 Ni10 S17 Ni9 138.24(19) . . . . ? S20 Ni10 S17 Ni9 38.7(19) . . . . ? S18 Ni10 S17 Ni9 -38.06(17) . . . . ? S16 Ni9 S17 C170 54(3) . . . . ? S15 Ni9 S17 C170 -37.1(5) . . . . ? S18 Ni9 S17 C170 146.9(5) . . . . ? Ni8 Ni9 S17 C170 3.3(5) . . . . ? Ni10 Ni9 S17 C170 108.8(5) . . . . ? S16 Ni9 S17 Ni10 -55(3) . . . . ? S15 Ni9 S17 Ni10 -145.93(17) . . . . ? S18 Ni9 S17 Ni10 38.10(17) . . . . ? Ni8 Ni9 S17 Ni10 -105.52(18) . . . . ? S17 Ni9 S18 C180 68.3(5) . . . . ? S16 Ni9 S18 C180 -115.9(5) . . . . ? S15 Ni9 S18 C180 -15(3) . . . . ? Ni8 Ni9 S18 C180 -151.9(5) . . . . ? Ni10 Ni9 S18 C180 105.8(5) . . . . ? S17 Ni9 S18 Ni10 -37.56(18) . . . . ? S16 Ni9 S18 Ni10 138.28(19) . . . . ? S15 Ni9 S18 Ni10 -120(3) . . . . ? Ni8 Ni9 S18 Ni10 102.2(2) . . . . ? S17 Ni10 S18 C180 -59.9(5) . . . . ? S19 Ni10 S18 C180 -179(100) . . . . ? S20 Ni10 S18 C180 125.9(5) . . . . ? Ni9 Ni10 S18 C180 -97.6(5) . . . . ? S17 Ni10 S18 Ni9 37.65(18) . . . . ? S19 Ni10 S18 Ni9 -81(3) . . . . ? S20 Ni10 S18 Ni9 -136.6(2) . . . . ? S17 Ni10 S19 C195 48.7(6) . . . . ? S20 Ni10 S19 C195 -137.2(6) . . . . ? S18 Ni10 S19 C195 167(3) . . . . ? Ni9 Ni10 S19 C195 89.4(6) . . . . ? S17 Ni10 S19 Ni11 162.5(2) . . . . ? S20 Ni10 S19 Ni11 -23.4(2) . . . . ? S18 Ni10 S19 Ni11 -79(3) . . . . ? Ni9 Ni10 S19 Ni11 -156.80(16) . . . . ? S22 Ni11 S19 C195 -121.9(16) . . . . ? S20 Ni11 S19 C195 134.4(7) . . . . ? S21 Ni11 S19 C195 -49.1(7) . . . . ? Ni1 Ni11 S19 C195 -92.4(7) . . . . ? S22 Ni11 S19 Ni10 127.0(15) . . . . ? S20 Ni11 S19 Ni10 23.4(2) . . . . ? S21 Ni11 S19 Ni10 -160.1(2) . . . . ? Ni1 Ni11 S19 Ni10 156.58(15) . . . . ? S17 Ni10 S20 C200 -127.1(19) . . . . ? S19 Ni10 S20 C200 132.6(5) . . . . ? S18 Ni10 S20 C200 -50.9(5) . . . . ? Ni9 Ni10 S20 C200 -91.3(5) . . . . ? S17 Ni10 S20 Ni11 123.7(19) . . . . ? S19 Ni10 S20 Ni11 23.4(2) . . . . ? S18 Ni10 S20 Ni11 -160.10(19) . . . . ? Ni9 Ni10 S20 Ni11 159.50(13) . . . . ? S22 Ni11 S20 C200 54.6(5) . . . . ? S19 Ni11 S20 C200 -133.9(5) . . . . ? S21 Ni11 S20 C200 -179(100) . . . . ? Ni1 Ni11 S20 C200 98.9(5) . . . . ? S22 Ni11 S20 Ni10 165.26(19) . . . . ? S19 Ni11 S20 Ni10 -23.3(2) . . . . ? S21 Ni11 S20 Ni10 -69(3) . . . . ? Ni1 Ni11 S20 Ni10 -150.49(15) . . . . ? S22 Ni11 S21 C210 -57.8(7) . . . . ? S20 Ni11 S21 C210 175(3) . . . . ? S19 Ni11 S21 C210 130.5(7) . . . . ? Ni1 Ni11 S21 C210 -98.5(7) . . . . ? S22 Ni11 S21 Ni1 40.69(18) . . . . ? S20 Ni11 S21 Ni1 -86(3) . . . . ? S19 Ni11 S21 Ni1 -131.00(19) . . . . ? S2 Ni1 S21 C210 -30(31) . . . . ? S1 Ni1 S21 C210 -110.7(6) . . . . ? S22 Ni1 S21 C210 66.1(6) . . . . ? Ni11 Ni1 S21 C210 106.4(6) . . . . ? Ni2 Ni1 S21 C210 -150.3(6) . . . . ? S2 Ni1 S21 Ni11 -136(31) . . . . ? S1 Ni1 S21 Ni11 142.91(17) . . . . ? S22 Ni1 S21 Ni11 -40.27(17) . . . . ? Ni2 Ni1 S21 Ni11 103.24(18) . . . . ? S20 Ni11 S22 C220 20.8(5) . . . . ? S19 Ni11 S22 C220 -81.5(16) . . . . ? S21 Ni11 S22 C220 -155.2(5) . . . . ? Ni1 Ni11 S22 C220 -114.5(5) . . . . ? S20 Ni11 S22 Ni1 135.2(2) . . . . ? S19 Ni11 S22 Ni1 32.9(16) . . . . ? S21 Ni11 S22 Ni1 -40.76(18) . . . . ? S2 Ni1 S22 C220 -30.1(5) . . . . ? S1 Ni1 S22 C220 -125(4) . . . . ? S21 Ni1 S22 C220 150.4(5) . . . . ? Ni11 Ni1 S22 C220 109.8(5) . . . . ? Ni2 Ni1 S22 C220 8.4(5) . . . . ? S2 Ni1 S22 Ni11 -139.81(19) . . . . ? S1 Ni1 S22 Ni11 125(4) . . . . ? S21 Ni1 S22 Ni11 40.64(18) . . . . ? Ni2 Ni1 S22 Ni11 -101.4(2) . . . . ? Ni2 S1 C10 C11 51.8(8) . . . . ? Ni1 S1 C10 C11 -38.1(8) . . . . ? Ni2 S1 C10 C15 -129.3(6) . . . . ? Ni1 S1 C10 C15 140.8(6) . . . . ? C15 C10 C11 C12 0.0 . . . . ? S1 C10 C11 C12 178.9(10) . . . . ? C10 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 C10 0.0 . . . . ? C11 C10 C15 C14 0.0 . . . . ? S1 C10 C15 C14 -178.9(9) . . . . ? Ni2 S2 C20 C21 -39.5(7) . . . . ? Ni1 S2 C20 C21 -124.3(6) . . . . ? Ni2 S2 C20 C25 147.2(5) . . . . ? Ni1 S2 C20 C25 62.4(6) . . . . ? C25 C20 C21 C22 0.0 . . . . ? S2 C20 C21 C22 -173.2(9) . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C20 0.0 . . . . ? C21 C20 C25 C24 0.0 . . . . ? S2 C20 C25 C24 173.4(9) . . . . ? Ni3 S3 C30 C31 110.5(6) . . . . ? Ni2 S3 C30 C31 -150.9(5) . . . . ? Ni3 S3 C30 C35 -70.4(6) . . . . ? Ni2 S3 C30 C35 28.3(7) . . . . ? C35 C30 C31 C32 0.0 . . . . ? S3 C30 C31 C32 179.2(8) . . . . ? C30 C31 C32 C33 0.0 . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C30 0.0 . . . . ? C31 C30 C35 C34 0.0 . . . . ? S3 C30 C35 C34 -179.1(8) . . . . ? C45 C40 C41 C42 0.0 . . . . ? C45 C40 C41 S4 -175.5(10) . . . . ? Ni2 S4 C41 C40 -52.7(9) . . . . ? Ni3 S4 C41 C40 46.8(10) . . . . ? Ni2 S4 C41 C42 131.8(7) . . . . ? Ni3 S4 C41 C42 -128.8(8) . . . . ? C40 C41 C42 C43 0.0 . . . . ? S4 C41 C42 C43 175.6(10) . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 C40 0.0 . . . . ? C41 C40 C45 C44 0.0 . . . . ? Ni4 S5 C50 C51 59.8(8) . . . . ? Ni3 S5 C50 C51 145.9(7) . . . . ? Ni4 S5 C50 C55 -125.3(7) . . . . ? Ni3 S5 C50 C55 -39.2(8) . . . . ? C55 C50 C51 C52 0.0 . . . . ? S5 C50 C51 C52 174.9(10) . . . . ? C50 C51 C52 C53 0.0 . . . . ? C51 C52 C53 C54 0.0 . . . . ? C52 C53 C54 C55 0.0 . . . . ? C53 C54 C55 C50 0.0 . . . . ? C51 C50 C55 C54 0.0 . . . . ? S5 C50 C55 C54 -174.9(10) . . . . ? Ni4 S6 C60 C61 130.9(5) . . . . ? Ni3 S6 C60 C61 -140.0(5) . . . . ? Ni4 S6 C60 C65 -49.8(7) . . . . ? Ni3 S6 C60 C65 39.3(7) . . . . ? C65 C60 C61 C62 0.0 . . . . ? S6 C60 C61 C62 179.3(8) . . . . ? C60 C61 C62 C63 0.0 . . . . ? C61 C62 C63 C64 0.0 . . . . ? C62 C63 C64 C65 0.0 . . . . ? C63 C64 C65 C60 0.0 . . . . ? C61 C60 C65 C64 0.0 . . . . ? S6 C60 C65 C64 -179.3(8) . . . . ? Ni5 S7 C70 C71 129.7(7) . . . . ? Ni4 S7 C70 C71 45.1(8) . . . . ? Ni5 S7 C70 C75 -56.5(7) . . . . ? Ni4 S7 C70 C75 -141.1(6) . . . . ? C75 C70 C71 C72 0.0 . . . . ? S7 C70 C71 C72 173.8(10) . . . . ? C70 C71 C72 C73 0.0 . . . . ? C71 C72 C73 C74 0.0 . . . . ? C72 C73 C74 C75 0.0 . . . . ? C73 C74 C75 C70 0.0 . . . . ? C71 C70 C75 C74 0.0 . . . . ? S7 C70 C75 C74 -173.8(10) . . . . ? Ni4 S8 C80 C81 144.0(5) . . . . ? Ni5 S8 C80 C81 -128.9(5) . . . . ? Ni4 S8 C80 C85 -40.0(7) . . . . ? Ni5 S8 C80 C85 47.1(7) . . . . ? C85 C80 C81 C82 0.0 . . . . ? S8 C80 C81 C82 176.1(8) . . . . ? C80 C81 C82 C83 0.0 . . . . ? C81 C82 C83 C84 0.0 . . . . ? C82 C83 C84 C85 0.0 . . . . ? C83 C84 C85 C80 0.0 . . . . ? C81 C80 C85 C84 0.0 . . . . ? S8 C80 C85 C84 -175.9(8) . . . . ? Ni5 S9 C90 C91 -141.8(6) . . . . ? Ni6 S9 C90 C91 118.6(6) . . . . ? Ni5 S9 C90 C95 37.2(7) . . . . ? Ni6 S9 C90 C95 -62.3(7) . . . . ? C95 C90 C91 C92 0.0 . . . . ? S9 C90 C91 C92 179.1(8) . . . . ? C90 C91 C92 C93 0.0 . . . . ? C91 C92 C93 C94 0.0 . . . . ? C92 C93 C94 C95 0.0 . . . . ? C93 C94 C95 C90 0.0 . . . . ? C91 C90 C95 C94 0.0 . . . . ? S9 C90 C95 C94 -179.0(8) . . . . ? Ni6 S10 C100 C101 23.7(7) . . . . ? Ni5 S10 C100 C101 -79.1(6) . . . . ? Ni6 S10 C100 C105 -154.6(5) . . . . ? Ni5 S10 C100 C105 102.6(6) . . . . ? C105 C100 C101 C102 0.0 . . . . ? S10 C100 C101 C102 -178.2(8) . . . . ? C100 C101 C102 C103 0.0 . . . . ? C101 C102 C103 C104 0.0 . . . . ? C102 C103 C104 C105 0.0 . . . . ? C103 C104 C105 C100 0.0 . . . . ? C101 C100 C105 C104 0.0 . . . . ? S10 C100 C105 C104 178.2(8) . . . . ? Ni6 S11 C110 C111 141.3(4) . . . . ? Ni7 S11 C110 C111 -126.8(4) . . . . ? Ni6 S11 C110 C115 -36.9(7) . . . . ? Ni7 S11 C110 C115 55.0(7) . . . . ? C115 C110 C111 C112 0.0 . . . . ? S11 C110 C111 C112 -178.3(7) . . . . ? C110 C111 C112 C113 0.0 . . . . ? C111 C112 C113 C114 0.0 . . . . ? C112 C113 C114 C115 0.0 . . . . ? C113 C114 C115 C110 0.0 . . . . ? C111 C110 C115 C114 0.0 . . . . ? S11 C110 C115 C114 178.2(8) . . . . ? Ni7 S12 C120 C121 146.5(5) . . . . ? Ni6 S12 C120 C121 -122.2(5) . . . . ? Ni7 S12 C120 C125 -36.8(8) . . . . ? Ni6 S12 C120 C125 54.6(8) . . . . ? C125 C120 C121 C122 0.0 . . . . ? S12 C120 C121 C122 176.8(8) . . . . ? C120 C121 C122 C123 0.0 . . . . ? C121 C122 C123 C124 0.0 . . . . ? C122 C123 C124 C125 0.0 . . . . ? C123 C124 C125 C120 0.0 . . . . ? C121 C120 C125 C124 0.0 . . . . ? S12 C120 C125 C124 -176.7(9) . . . . ? Ni7 S13 C130 C131 36.9(8) . . . . ? Ni8 S13 C130 C131 -68.6(8) . . . . ? Ni7 S13 C130 C135 -141.7(6) . . . . ? Ni8 S13 C130 C135 112.8(7) . . . . ? C135 C130 C131 C132 0.0 . . . . ? S13 C130 C131 C132 -178.6(9) . . . . ? C130 C131 C132 C133 0.0 . . . . ? C131 C132 C133 C134 0.0 . . . . ? C132 C133 C134 C135 0.0 . . . . ? C133 C134 C135 C130 0.0 . . . . ? C131 C130 C135 C134 0.0 . . . . ? S13 C130 C135 C134 178.7(9) . . . . ? C240 S14 C140 C145 43(9) . . . . ? Ni7 S14 C140 C145 14(2) . . . . ? Ni8 S14 C140 C145 114(2) . . . . ? C240 S14 C140 C141 -147(10) . . . . ? Ni7 S14 C140 C141 -176.2(17) . . . . ? Ni8 S14 C140 C141 -76(2) . . . . ? C141 C140 C145 C144 0.0 . . . . ? S14 C140 C145 C144 170(3) . . . . ? C140 C145 C144 C143 0.0 . . . . ? C145 C144 C143 C142 0.0 . . . . ? C144 C143 C142 C141 0.0 . . . . ? C143 C142 C141 C140 0.0 . . . . ? C145 C140 C141 C142 0.0 . . . . ? S14 C140 C141 C142 -170(3) . . . . ? C140 S14 C240 C241 -84(9) . . . . ? Ni7 S14 C240 C241 68(2) . . . . ? Ni8 S14 C240 C241 164(2) . . . . ? C140 S14 C240 C245 98(10) . . . . ? Ni7 S14 C240 C245 -110(2) . . . . ? Ni8 S14 C240 C245 -14(3) . . . . ? C245 C240 C241 C242 0.0 . . . . ? S14 C240 C241 C242 -178(4) . . . . ? C240 C241 C242 C243 0.0 . . . . ? C241 C242 C243 C244 0.0 . . . . ? C242 C243 C244 C245 0.0 . . . . ? C243 C244 C245 C240 0.0 . . . . ? C241 C240 C245 C244 0.0 . . . . ? S14 C240 C245 C244 178(4) . . . . ? Ni9 S15 C150 C151 49.4(10) . . . . ? Ni8 S15 C150 C151 134.6(8) . . . . ? Ni9 S15 C150 C155 -131.0(8) . . . . ? Ni8 S15 C150 C155 -45.8(9) . . . . ? C155 C150 C151 C152 0.0 . . . . ? S15 C150 C151 C152 179.7(11) . . . . ? C150 C151 C152 C153 0.0 . . . . ? C151 C152 C153 C154 0.0 . . . . ? C152 C153 C154 C155 0.0 . . . . ? C153 C154 C155 C150 0.0 . . . . ? C151 C150 C155 C154 0.0 . . . . ? S15 C150 C155 C154 -179.7(11) . . . . ? Ni9 S16 C160 C161 -39.6(11) . . . . ? Ni8 S16 C160 C161 50.3(11) . . . . ? Ni9 S16 C160 C165 139.5(8) . . . . ? Ni8 S16 C160 C165 -130.6(8) . . . . ? C165 C160 C161 C162 0.0 . . . . ? S16 C160 C161 C162 179.1(13) . . . . ? C160 C161 C162 C163 0.0 . . . . ? C161 C162 C163 C164 0.0 . . . . ? C162 C163 C164 C165 0.0 . . . . ? C163 C164 C165 C160 0.0 . . . . ? C161 C160 C165 C164 0.0 . . . . ? S16 C160 C165 C164 -179.1(12) . . . . ? Ni10 S17 C170 C171 -127.3(6) . . . . ? Ni9 S17 C170 C171 142.3(5) . . . . ? Ni10 S17 C170 C175 51.0(7) . . . . ? Ni9 S17 C170 C175 -39.3(7) . . . . ? C175 C170 C171 C172 0.0 . . . . ? S17 C170 C171 C172 178.4(8) . . . . ? C170 C171 C172 C173 0.0 . . . . ? C171 C172 C173 C174 0.0 . . . . ? C172 C173 C174 C175 0.0 . . . . ? C173 C174 C175 C170 0.0 . . . . ? C171 C170 C175 C174 0.0 . . . . ? S17 C170 C175 C174 -178.3(9) . . . . ? Ni9 S18 C180 C181 -134.2(6) . . . . ? Ni10 S18 C180 C181 -49.2(7) . . . . ? Ni9 S18 C180 C185 48.1(7) . . . . ? Ni10 S18 C180 C185 133.2(6) . . . . ? C185 C180 C181 C182 0.0 . . . . ? S18 C180 C181 C182 -177.7(9) . . . . ? C180 C181 C182 C183 0.0 . . . . ? C181 C182 C183 C184 0.0 . . . . ? C182 C183 C184 C185 0.0 . . . . ? C183 C184 C185 C180 0.0 . . . . ? C181 C180 C185 C184 0.0 . . . . ? S18 C180 C185 C184 177.6(9) . . . . ? C195 C190 C191 C192 0.0 . . . . ? C190 C191 C192 C193 0.0 . . . . ? C191 C192 C193 C194 0.0 . . . . ? C192 C193 C194 C195 0.0 . . . . ? C193 C194 C195 C190 0.0 . . . . ? C193 C194 C195 S19 -175.6(11) . . . . ? C191 C190 C195 C194 0.0 . . . . ? C191 C190 C195 S19 175.9(10) . . . . ? Ni10 S19 C195 C194 28.4(10) . . . . ? Ni11 S19 C195 C194 -72.7(9) . . . . ? Ni10 S19 C195 C190 -147.4(7) . . . . ? Ni11 S19 C195 C190 111.5(7) . . . . ? Ni10 S20 C200 C201 107.5(7) . . . . ? Ni11 S20 C200 C201 -153.2(6) . . . . ? Ni10 S20 C200 C205 -71.5(8) . . . . ? Ni11 S20 C200 C205 27.8(8) . . . . ? C205 C200 C201 C202 0.0 . . . . ? S20 C200 C201 C202 -179.0(10) . . . . ? C200 C201 C202 C203 0.0 . . . . ? C201 C202 C203 C204 0.0 . . . . ? C202 C203 C204 C205 0.0 . . . . ? C203 C204 C205 C200 0.0 . . . . ? C201 C200 C205 C204 0.0 . . . . ? S20 C200 C205 C204 179.0(10) . . . . ? Ni11 S21 C210 C211 -35.7(14) . . . . ? Ni1 S21 C210 C211 -120.0(12) . . . . ? Ni11 S21 C210 C215 149.1(10) . . . . ? Ni1 S21 C210 C215 64.8(12) . . . . ? C215 C210 C211 C212 0.0 . . . . ? S21 C210 C211 C212 -175.0(17) . . . . ? C210 C211 C212 C213 0.0 . . . . ? C211 C212 C213 C214 0.0 . . . . ? C212 C213 C214 C215 0.0 . . . . ? C213 C214 C215 C210 0.0 . . . . ? C211 C210 C215 C214 0.0 . . . . ? S21 C210 C215 C214 175.3(16) . . . . ? Ni11 S22 C220 C221 58.1(8) . . . . ? Ni1 S22 C220 C221 -33.1(8) . . . . ? Ni11 S22 C220 C225 -119.9(6) . . . . ? Ni1 S22 C220 C225 148.9(5) . . . . ? C225 C220 C221 C222 0.0 . . . . ? S22 C220 C221 C222 -177.9(9) . . . . ? C220 C221 C222 C223 0.0 . . . . ? C221 C222 C223 C224 0.0 . . . . ? C222 C223 C224 C225 0.0 . . . . ? C223 C224 C225 C220 0.0 . . . . ? C221 C220 C225 C224 0.0 . . . . ? S22 C220 C225 C224 178.0(8) . . . . ? C4A O1A C1A C2A -32(4) . . . . ? O1A C1A C2A C3A 19(4) . . . . ? C1A C2A C3A C4A 4(3) . . . . ? C1A O1A C4A C3A 34(3) . . . . ? C2A C3A C4A O1A -26(4) . . . . ? C4B O1B C1B C2B -35(9) . . . . ? O1B C1B C2B C3B 8(9) . . . . ? C1B C2B C3B C4B 22(7) . . . . ? C1B O1B C4B C3B 50(7) . . . . ? C2B C3B C4B O1B -46(5) . . . . ? C4C O1C C1C C2C -45(5) . . . . ? O1C C1C C2C C3C 50(4) . . . . ? C1C C2C C3C C4C -34(5) . . . . ? C1C O1C C4C C3C 22(6) . . . . ? C2C C3C C4C O1C 8(6) . . . . ? C4D O1D C1D C2D -14(5) . . . . ? O1D C1D C2D C3D 31(4) . . . . ? C1D C2D C3D C4D -33(3) . . . . ? C1D O1D C4D C3D -10(6) . . . . ? C2D C3D C4D O1D 29(4) . . . . ? C4E O1E C1E C2E 51(6) . . . . ? O1E C1E C2E C3E -48(6) . . . . ? C1E C2E C3E C4E 20(6) . . . . ? C1E O1E C4E C3E -31(5) . . . . ? C2E C3E C4E O1E 7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.087 _refine_diff_density_min -0.692 _refine_diff_density_rms 0.172 data_dahl126 _database_code_CSD 186294 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H180 Ni9 O S18' _chemical_formula_weight 1735.27 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-31c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 18.0237(11) _cell_length_b 18.0237(11) _cell_length_c 21.1181(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5941.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 6795 _cell_measurement_theta_min 1.62 _cell_measurement_theta_max 23.25 _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.970 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 1.726 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.5452 _exptl_absorpt_correction_T_max 0.8464 _exptl_absorpt_process_details ; Empirical with SADABS (Blessing, 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'N/A' _diffrn_standards_interval_count 'N/A' _diffrn_standards_interval_time 'N/A' _diffrn_standards_decay_% <1 _diffrn_reflns_number 2852 _diffrn_reflns_av_R_equivalents 4585 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 23.25 _reflns_number_total 2852 _reflns_number_gt 2095 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+4.9993P] 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 2852 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.1274 _refine_ls_wR_factor_gt 0.1043 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _refine_ls_shift/su_max 0.003 _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 -0.02745(5) 0.48628(2) 0.2500 0.0631(3) Uani 1 2 d S . . Ni2 Ni -0.12303(4) 0.30270(4) 0.25125(3) 0.0644(2) Uani 1 1 d . . . S1 S -0.03460(8) 0.57323(8) 0.32092(5) 0.0698(4) Uani 1 1 d . . . S2 S -0.02683(8) 0.39363(9) 0.31745(6) 0.0711(4) Uani 1 1 d . . . S3 S -0.22408(8) 0.22244(8) 0.31864(5) 0.0692(4) Uani 1 1 d . . . C30 C -0.1808(4) 0.1800(4) 0.3742(2) 0.0831(15) Uani 1 1 d . A . C20 C -0.0716(3) 0.3936(3) 0.3927(2) 0.0686(13) Uani 1 1 d . A . C25 C -0.0302(4) 0.3856(4) 0.4457(3) 0.0982(19) Uani 1 1 d . . . H25A H 0.0194 0.3822 0.4414 0.118 Uiso 1 1 calc R A . C31 C -0.2161(4) 0.1608(5) 0.4339(3) 0.116(2) Uani 1 1 d . . . H31A H -0.2620 0.1684 0.4441 0.139 Uiso 1 1 calc R A . C21 C -0.1444(4) 0.3994(3) 0.3997(2) 0.0778(14) Uani 1 1 d . . . H21A H -0.1721 0.4047 0.3643 0.093 Uiso 1 1 calc R A . C22 C -0.1764(5) 0.3972(4) 0.4603(3) 0.103(2) Uani 1 1 d . A . H22A H -0.2254 0.4014 0.4655 0.123 Uiso 1 1 calc R . . C33 C -0.1144(6) 0.1209(7) 0.4660(5) 0.171(4) Uani 1 1 d . . . H33A H -0.0923 0.1009 0.4971 0.206 Uiso 1 1 calc R A . C34 C -0.0777(6) 0.1412(6) 0.4073(5) 0.159(3) Uani 1 1 d . A . H34A H -0.0303 0.1353 0.3985 0.190 Uiso 1 1 calc R . . C32 C -0.1821(6) 0.1298(6) 0.4786(4) 0.160(4) Uani 1 1 d . A . H32A H -0.2072 0.1149 0.5185 0.192 Uiso 1 1 calc R . . C35 C -0.1113(5) 0.1708(5) 0.3604(3) 0.116(2) Uani 1 1 d . . . H35A H -0.0869 0.1842 0.3202 0.139 Uiso 1 1 calc R A . C24 C -0.0645(7) 0.3827(5) 0.5047(3) 0.133(3) Uani 1 1 d . A . H24A H -0.0378 0.3765 0.5404 0.160 Uiso 1 1 calc R . . C23 C -0.1357(7) 0.3888(6) 0.5120(3) 0.139(3) Uani 1 1 d . . . H23A H -0.1570 0.3872 0.5524 0.167 Uiso 1 1 calc R A . C10 C 0.0534(7) 0.6828(10) 0.3193(8) 0.060(5) Uani 0.41(2) 1 d PG A 1 C15 C 0.1343(8) 0.6911(14) 0.3222(7) 0.089(7) Uani 0.41(2) 1 d PG A 1 H15A H 0.1401 0.6428 0.3192 0.107 Uiso 0.41(2) 1 calc PR A 1 C14 C 0.2064(7) 0.7715(17) 0.3296(9) 0.130(14) Uani 0.41(2) 1 d PG A 1 H14A H 0.2605 0.7771 0.3315 0.156 Uiso 0.41(2) 1 calc PR A 1 C13 C 0.1977(11) 0.8437(14) 0.3341(10) 0.117(12) Uani 0.41(2) 1 d PG A 1 H13A H 0.2459 0.8976 0.3391 0.140 Uiso 0.41(2) 1 calc PR A 1 C12 C 0.1168(13) 0.8355(10) 0.3313(10) 0.149(11) Uani 0.41(2) 1 d PG A 1 H12A H 0.1110 0.8838 0.3343 0.179 Uiso 0.41(2) 1 calc PR A 1 C11 C 0.0447(10) 0.7550(10) 0.3239(9) 0.108(7) Uani 0.41(2) 1 d PG A 1 H11A H -0.0094 0.7495 0.3220 0.129 Uiso 0.41(2) 1 calc PR A 1 C10A C 0.0733(7) 0.6605(6) 0.3195(5) 0.066(4) Uani 0.59(2) 1 d PG A 2 C15A C 0.1442(7) 0.6494(7) 0.3164(6) 0.094(4) Uani 0.59(2) 1 d PG A 2 H15B H 0.1369 0.5952 0.3093 0.113 Uiso 0.59(2) 1 calc PR A 2 C14A C 0.2261(7) 0.7193(10) 0.3240(6) 0.121(6) Uani 0.59(2) 1 d PG A 2 H14B H 0.2736 0.7119 0.3219 0.146 Uiso 0.59(2) 1 calc PR A 2 C13A C 0.2371(9) 0.8003(8) 0.3346(7) 0.126(9) Uani 0.59(2) 1 d PG A 2 H13B H 0.2919 0.8471 0.3396 0.151 Uiso 0.59(2) 1 calc PR A 2 C12A C 0.1662(12) 0.8114(6) 0.3377(7) 0.128(9) Uani 0.59(2) 1 d PG A 2 H12B H 0.1736 0.8656 0.3448 0.153 Uiso 0.59(2) 1 calc PR A 2 C11A C 0.0843(10) 0.7415(7) 0.3302(6) 0.105(6) Uani 0.59(2) 1 d PG A 2 H11B H 0.0369 0.7489 0.3323 0.126 Uiso 0.59(2) 1 calc PR A 2 O1S O 0.0029(18) 0.931(2) 0.2676(17) 0.44(3) Uiso 0.61(3) 1 d P . . C2S O 0.0000 1.0000 0.318(4) 0.56(6) Uiso 0.61(3) 3 d SP . . 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 0.0544(5) 0.0841(5) 0.0411(4) 0.0048(3) 0.000 0.0272(3) Ni2 0.0750(4) 0.0847(5) 0.0417(3) 0.0026(3) 0.0019(3) 0.0461(4) S1 0.0693(8) 0.0739(8) 0.0445(6) 0.0019(5) -0.0034(5) 0.0195(6) S2 0.0685(8) 0.1056(10) 0.0465(7) 0.0050(6) -0.0039(5) 0.0490(7) S3 0.0810(8) 0.0855(9) 0.0425(6) 0.0017(6) 0.0009(6) 0.0426(7) C30 0.086(4) 0.092(4) 0.062(3) 0.011(3) -0.005(3) 0.037(3) C20 0.076(3) 0.076(3) 0.046(3) 0.002(2) -0.002(2) 0.032(3) C25 0.117(5) 0.119(5) 0.051(3) 0.004(3) -0.016(3) 0.053(4) C31 0.099(4) 0.166(6) 0.065(4) 0.036(4) 0.003(3) 0.053(4) C21 0.085(4) 0.076(3) 0.061(3) 0.006(3) 0.012(3) 0.032(3) C22 0.116(5) 0.088(4) 0.084(5) -0.001(3) 0.038(4) 0.035(4) C33 0.117(7) 0.208(9) 0.155(9) 0.104(7) -0.013(6) 0.056(7) C34 0.145(7) 0.209(9) 0.154(8) 0.069(7) -0.001(6) 0.112(7) C32 0.122(7) 0.219(10) 0.086(5) 0.073(6) -0.009(5) 0.047(7) C35 0.118(5) 0.142(6) 0.107(5) 0.036(4) 0.012(4) 0.080(5) C24 0.183(8) 0.144(7) 0.042(4) 0.010(4) -0.016(5) 0.059(6) C23 0.178(9) 0.146(7) 0.057(5) 0.000(4) 0.033(5) 0.053(7) C10 0.069(9) 0.075(14) 0.046(7) -0.003(8) -0.012(6) 0.044(10) C15 0.067(12) 0.096(18) 0.074(10) 0.005(10) 0.009(9) 0.018(12) C14 0.071(15) 0.15(3) 0.100(15) -0.042(17) 0.001(12) 0.002(19) C13 0.077(15) 0.110(19) 0.077(12) -0.011(13) -0.006(10) -0.019(14) C12 0.12(2) 0.106(17) 0.17(2) -0.023(15) -0.015(16) 0.024(15) C11 0.097(13) 0.067(11) 0.139(17) -0.018(10) -0.020(12) 0.026(10) C10A 0.074(10) 0.060(7) 0.048(5) 0.004(5) -0.008(6) 0.023(7) C15A 0.081(8) 0.081(9) 0.098(9) 0.005(7) -0.012(6) 0.024(7) C14A 0.086(10) 0.113(12) 0.112(10) 0.006(9) -0.008(7) 0.010(8) C13A 0.118(14) 0.097(13) 0.091(10) 0.005(9) -0.005(9) -0.001(12) C12A 0.14(2) 0.062(10) 0.097(10) -0.012(9) 0.004(11) -0.009(14) C11A 0.152(17) 0.079(10) 0.078(8) -0.006(7) -0.002(9) 0.053(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 Ni1 S2 2.1991(13) . ? Ni1 S2 2.1991(13) 6_565 ? Ni1 S1 2.2177(13) 6_565 ? Ni1 S1 2.2177(13) . ? Ni1 Ni2 2.8664(8) . ? Ni1 Ni2 2.8663(8) 6_565 ? Ni2 S3 2.1909(13) . ? Ni2 S2 2.1920(14) . ? Ni2 S3 2.2040(14) 4 ? Ni2 S1 2.2120(14) 6_565 ? S1 C10A 1.789(8) . ? S1 C10 1.812(13) . ? S1 Ni2 2.2121(14) 6_565 ? S2 C20 1.782(5) . ? S3 C30 1.780(5) . ? S3 Ni2 2.2040(14) 4 ? C30 C35 1.374(8) . ? C30 C31 1.376(8) . ? C20 C21 1.375(7) . ? C20 C25 1.393(7) . ? C25 C24 1.380(10) . ? C31 C32 1.384(10) . ? C21 C22 1.397(7) . ? C22 C23 1.365(11) . ? C33 C32 1.335(13) . ? C33 C34 1.366(11) . ? C34 C35 1.400(9) . ? C24 C23 1.350(12) . ? C10 C15 1.3900 . ? C10 C11 1.3900 . ? C15 C14 1.3900 . ? C14 C13 1.3900 . ? C13 C12 1.3900 . ? C12 C11 1.3900 . ? C10A C15A 1.3900 . ? C10A C11A 1.3900 . ? C15A C14A 1.3900 . ? C14A C13A 1.3900 . ? C13A C12A 1.3900 . ? C12A C11A 1.3900 . ? O1S O1S 1.40(6) 4_665 ? O1S O1S 1.54(6) 5_455 ? O1S C2S 1.65(6) . ? C2S O1S 1.65(6) 3_465 ? C2S O1S 1.65(6) 2_675 ? 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 S2 179.50(8) . 6_565 ? S2 Ni1 S1 82.94(5) . 6_565 ? S2 Ni1 S1 97.09(5) 6_565 6_565 ? S2 Ni1 S1 97.09(5) . . ? S2 Ni1 S1 82.94(5) 6_565 . ? S1 Ni1 S1 174.23(7) 6_565 . ? S2 Ni1 Ni2 49.14(4) . . ? S2 Ni1 Ni2 131.20(4) 6_565 . ? S1 Ni1 Ni2 49.59(4) 6_565 . ? S1 Ni1 Ni2 126.57(4) . . ? S2 Ni1 Ni2 131.20(4) . 6_565 ? S2 Ni1 Ni2 49.14(4) 6_565 6_565 ? S1 Ni1 Ni2 126.57(4) 6_565 6_565 ? S1 Ni1 Ni2 49.59(4) . 6_565 ? Ni2 Ni1 Ni2 117.27(4) . 6_565 ? S3 Ni2 S2 99.50(5) . . ? S3 Ni2 S3 82.55(5) . 4 ? S2 Ni2 S3 173.04(6) . 4 ? S3 Ni2 S1 170.73(6) . 6_565 ? S2 Ni2 S1 83.23(5) . 6_565 ? S3 Ni2 S1 93.73(5) 4 6_565 ? S3 Ni2 Ni1 126.13(4) . . ? S2 Ni2 Ni1 49.36(4) . . ? S3 Ni2 Ni1 124.21(4) 4 . ? S1 Ni2 Ni1 49.76(4) 6_565 . ? C10A S1 C10 21.1(4) . . ? C10A S1 Ni2 116.9(4) . 6_565 ? C10 S1 Ni2 102.7(6) . 6_565 ? C10A S1 Ni1 100.8(5) . . ? C10 S1 Ni1 115.4(6) . . ? Ni2 S1 Ni1 80.64(4) 6_565 . ? C20 S2 Ni2 112.30(17) . . ? C20 S2 Ni1 113.80(18) . . ? Ni2 S2 Ni1 81.50(4) . . ? C30 S3 Ni2 108.3(2) . . ? C30 S3 Ni2 109.53(19) . 4 ? Ni2 S3 Ni2 94.94(5) . 4 ? C35 C30 C31 119.9(6) . . ? C35 C30 S3 122.2(5) . . ? C31 C30 S3 117.8(5) . . ? C21 C20 C25 120.2(5) . . ? C21 C20 S2 123.0(4) . . ? C25 C20 S2 116.8(4) . . ? C24 C25 C20 118.5(7) . . ? C30 C31 C32 119.0(7) . . ? C20 C21 C22 119.4(6) . . ? C23 C22 C21 119.9(7) . . ? C32 C33 C34 119.9(8) . . ? C33 C34 C35 120.0(8) . . ? C33 C32 C31 121.9(8) . . ? C30 C35 C34 119.3(7) . . ? C23 C24 C25 121.7(7) . . ? C24 C23 C22 120.2(7) . . ? C15 C10 C11 120.0 . . ? C15 C10 S1 114.6(7) . . ? C11 C10 S1 124.8(7) . . ? C14 C15 C10 120.0 . . ? C15 C14 C13 120.0 . . ? C12 C13 C14 120.0 . . ? C11 C12 C13 120.0 . . ? C12 C11 C10 120.0 . . ? C15A C10A C11A 120.0 . . ? C15A C10A S1 123.3(6) . . ? C11A C10A S1 116.2(6) . . ? C10A C15A C14A 120.0 . . ? C15A C14A C13A 120.0 . . ? C14A C13A C12A 120.0 . . ? C13A C12A C11A 120.0 . . ? C12A C11A C10A 120.0 . . ? O1S O1S O1S 97(4) 4_665 5_455 ? O1S O1S C2S 92(3) 4_665 . ? O1S O1S C2S 87(3) 5_455 . ? O1S C2S O1S 83(4) . 3_465 ? O1S C2S O1S 83(4) . 2_675 ? O1S C2S O1S 83(4) 3_465 2_675 ? 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 S2 Ni1 Ni2 S3 69.07(7) . . . . ? S2 Ni1 Ni2 S3 -111.41(7) 6_565 . . . ? S1 Ni1 Ni2 S3 -169.41(7) 6_565 . . . ? S1 Ni1 Ni2 S3 5.08(7) . . . . ? Ni2 Ni1 Ni2 S3 -53.21(5) 6_565 . . . ? S2 Ni1 Ni2 S2 179.52(7) 6_565 . . . ? S1 Ni1 Ni2 S2 121.52(6) 6_565 . . . ? S1 Ni1 Ni2 S2 -63.99(6) . . . . ? Ni2 Ni1 Ni2 S2 -122.28(5) 6_565 . . . ? S2 Ni1 Ni2 S3 176.65(7) . . . 4 ? S2 Ni1 Ni2 S3 -3.83(8) 6_565 . . 4 ? S1 Ni1 Ni2 S3 -61.83(6) 6_565 . . 4 ? S1 Ni1 Ni2 S3 112.66(6) . . . 4 ? Ni2 Ni1 Ni2 S3 54.37(5) 6_565 . . 4 ? S2 Ni1 Ni2 S1 -121.52(6) . . . 6_565 ? S2 Ni1 Ni2 S1 58.00(7) 6_565 . . 6_565 ? S1 Ni1 Ni2 S1 174.49(7) . . . 6_565 ? Ni2 Ni1 Ni2 S1 116.20(4) 6_565 . . 6_565 ? S2 Ni1 S1 C10A 104.2(4) . . . . ? S2 Ni1 S1 C10A -75.3(4) 6_565 . . . ? S1 Ni1 S1 C10A -165.9(4) 6_565 . . . ? Ni2 Ni1 S1 C10A 147.4(4) . . . . ? Ni2 Ni1 S1 C10A -115.9(4) 6_565 . . . ? S2 Ni1 S1 C10 120.3(6) . . . . ? S2 Ni1 S1 C10 -59.2(6) 6_565 . . . ? S1 Ni1 S1 C10 -149.8(6) 6_565 . . . ? Ni2 Ni1 S1 C10 163.5(6) . . . . ? Ni2 Ni1 S1 C10 -99.7(6) 6_565 . . . ? S2 Ni1 S1 Ni2 -139.99(5) . . . 6_565 ? S2 Ni1 S1 Ni2 40.52(5) 6_565 . . 6_565 ? S1 Ni1 S1 Ni2 -50.10(3) 6_565 . . 6_565 ? Ni2 Ni1 S1 Ni2 -96.76(5) . . . 6_565 ? S3 Ni2 S2 C20 -17.79(19) . . . . ? S3 Ni2 S2 C20 88.8(5) 4 . . . ? S1 Ni2 S2 C20 153.26(19) 6_565 . . . ? Ni1 Ni2 S2 C20 112.32(19) . . . . ? S3 Ni2 S2 Ni1 -130.10(5) . . . . ? S3 Ni2 S2 Ni1 -23.5(4) 4 . . . ? S1 Ni2 S2 Ni1 40.94(5) 6_565 . . . ? S2 Ni1 S2 C20 115.5(14) 6_565 . . . ? S1 Ni1 S2 C20 -151.54(19) 6_565 . . . ? S1 Ni1 S2 C20 22.64(19) . . . . ? Ni2 Ni1 S2 C20 -110.69(19) . . . . ? Ni2 Ni1 S2 C20 -18.0(2) 6_565 . . . ? S2 Ni1 S2 Ni2 -133.8(13) 6_565 . . . ? S1 Ni1 S2 Ni2 -40.85(5) 6_565 . . . ? S1 Ni1 S2 Ni2 133.33(5) . . . . ? Ni2 Ni1 S2 Ni2 92.74(6) 6_565 . . . ? S2 Ni2 S3 C30 -57.4(2) . . . . ? S3 Ni2 S3 C30 129.3(2) 4 . . . ? S1 Ni2 S3 C30 -163.9(4) 6_565 . . . ? Ni1 Ni2 S3 C30 -103.4(2) . . . . ? S2 Ni2 S3 Ni2 -169.89(5) . . . 4 ? S3 Ni2 S3 Ni2 16.84(7) 4 . . 4 ? S1 Ni2 S3 Ni2 83.6(4) 6_565 . . 4 ? Ni1 Ni2 S3 Ni2 144.18(3) . . . 4 ? Ni2 S3 C30 C35 -24.2(6) . . . . ? Ni2 S3 C30 C35 78.1(6) 4 . . . ? Ni2 S3 C30 C31 152.0(5) . . . . ? Ni2 S3 C30 C31 -105.6(5) 4 . . . ? Ni2 S2 C20 C21 -48.9(5) . . . . ? Ni1 S2 C20 C21 41.4(5) . . . . ? Ni2 S2 C20 C25 129.8(4) . . . . ? Ni1 S2 C20 C25 -139.8(4) . . . . ? C21 C20 C25 C24 0.7(9) . . . . ? S2 C20 C25 C24 -178.1(5) . . . . ? C35 C30 C31 C32 -2.0(11) . . . . ? S3 C30 C31 C32 -178.3(6) . . . . ? C25 C20 C21 C22 0.0(8) . . . . ? S2 C20 C21 C22 178.7(4) . . . . ? C20 C21 C22 C23 -0.4(9) . . . . ? C32 C33 C34 C35 -0.4(17) . . . . ? C34 C33 C32 C31 -1.1(18) . . . . ? C30 C31 C32 C33 2.3(15) . . . . ? C31 C30 C35 C34 0.5(11) . . . . ? S3 C30 C35 C34 176.7(7) . . . . ? C33 C34 C35 C30 0.6(14) . . . . ? C20 C25 C24 C23 -1.0(12) . . . . ? C25 C24 C23 C22 0.6(14) . . . . ? C21 C22 C23 C24 0.1(12) . . . . ? C10A S1 C10 C15 -3.1(17) . . . . ? Ni2 S1 C10 C15 -137.9(8) 6_565 . . . ? Ni1 S1 C10 C15 -52.4(10) . . . . ? C10A S1 C10 C11 -174(3) . . . . ? Ni2 S1 C10 C11 50.8(9) 6_565 . . . ? Ni1 S1 C10 C11 136.4(8) . . . . ? C11 C10 C15 C14 0.0 . . . . ? S1 C10 C15 C14 -171.7(12) . . . . ? C10 C15 C14 C13 0.0 . . . . ? C15 C14 C13 C12 0.0 . . . . ? C14 C13 C12 C11 0.0 . . . . ? C13 C12 C11 C10 0.0 . . . . ? C15 C10 C11 C12 0.0 . . . . ? S1 C10 C11 C12 170.8(13) . . . . ? C10 S1 C10A C15A -177(3) . . . . ? Ni2 S1 C10A C15A -126.0(6) 6_565 . . . ? Ni1 S1 C10A C15A -41.1(6) . . . . ? C10 S1 C10A C11A 11.3(19) . . . . ? Ni2 S1 C10A C11A 62.2(8) 6_565 . . . ? Ni1 S1 C10A C11A 147.1(6) . . . . ? C11A C10A C15A C14A 0.0 . . . . ? S1 C10A C15A C14A -171.5(9) . . . . ? C10A C15A C14A C13A 0.0 . . . . ? C15A C14A C13A C12A 0.0 . . . . ? C14A C13A C12A C11A 0.0 . . . . ? C13A C12A C11A C10A 0.0 . . . . ? C15A C10A C11A C12A 0.0 . . . . ? S1 C10A C11A C12A 172.1(8) . . . . ? O1S O1S C2S O1S 91(3) 4_665 . . 3_465 ? O1S O1S C2S O1S -6(2) 5_455 . . 3_465 ? O1S O1S C2S O1S 7(3) 4_665 . . 2_675 ? O1S O1S C2S O1S -90(3) 5_455 . . 2_675 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.342 _refine_diff_density_min -0.278 _refine_diff_density_rms 0.054