# ic980131p.cif # SUBMISSION DETAILS _publ_contact_author Dr. Berthold Kersting Institut fuer Anorganische und Analytische Chemie Albertstr. 21 79104 Freiburg Germany _publ_contact_author_phone '+49/(0)761/203 6116' _publ_contact_author_fax '+49/(0)761/203 6001' _publ_contact_author_email 'kerstber@sun2.ruf.uni-freiburg.de' _publ_requested_journal 'Inorg. Chem.' #Compound: [Ni2(L)2][BPh4]2xMeOHxCH3CN data_ni2l2 _audit_creation_method SHELXL _chemical_name_systematic ; Di(2,6-di(aminomethyl)-4-tert-butyl-thiophenolato)dinickel(II)- di(tetraphenylborate)-methanol-acetonitrile ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ; [(4-t-Bu-2,6(CH2NH2)2-C6H2SH)2Ni2][B(C6H5)4]2MeOHCH3CN ; _chemical_formula_analytical ? _chemical_formula_sum 'C75 H85 B2 N5 Ni2 O S2' _chemical_formula_weight 1275.64 _chemical_melting_point 232-234oC _chemical_compound_source MeOH-CH3CN loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic P' _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 21.940(4) _cell_length_b 13.901(3) _cell_length_c 23.918(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.00(3) _cell_angle_gamma 90.00 _cell_volume 6854.8(24) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent blocks' _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 1.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method ? _exptl_crystal_F_000 2704 _exptl_absorpt_coefficient_mu 0.657 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.96 _exptl_special_details ; Crystals were grown by recrystallization from MeOH/CH3CN solution ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius-Turbo-CAD4' _diffrn_measurement_method 'Omega-2Theta' _diffrn_standards_number 2 _diffrn_standards_interval_count 'OCR every 200 refl.' _diffrn_standards_interval_time 'ICR every 1800 s.' _diffrn_standards_decay_% ? _diffrn_reflns_number 13792 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 26.07 _reflns_number_total 13460 _reflns_number_observed 8937 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 28 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0814P)^2^+5.8367P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13432 _refine_ls_number_parameters 780 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1093 _refine_ls_R_factor_obs 0.0580 _refine_ls_wR_factor_all 0.1852 _refine_ls_wR_factor_obs 0.1475 _refine_ls_goodness_of_fit_all 1.161 _refine_ls_goodness_of_fit_obs 1.159 _refine_ls_restrained_S_all 1.173 _refine_ls_restrained_S_obs 1.159 _refine_ls_shift/esd_max -0.202 _refine_ls_shift/esd_mean 0.007 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 1.03615(2) 0.95483(4) 0.16848(2) 0.0479(2) Uani 1 d . . Ni2 Ni 0.90173(2) 0.93152(4) 0.16924(2) 0.04369(15) Uani 1 d . . S1 S 0.98536(5) 0.83482(8) 0.19243(4) 0.0486(2) Uani 1 d . . N1 N 1.1192(2) 0.9268(3) 0.2280(2) 0.0616(10) Uani 1 d . . H1A H 1.1481(2) 0.9221(3) 0.2091(2) 0.080 Uiso 1 calc R . H1B H 1.1305(2) 0.9786(3) 0.2520(2) 0.080 Uiso 1 calc R . N2 N 0.8722(2) 0.8913(3) 0.23314(15) 0.0544(8) Uani 1 d . . H2A H 0.8755(2) 0.9425(3) 0.25703(15) 0.080 Uiso 1 calc R . H2B H 0.8297(2) 0.8774(3) 0.21685(15) 0.080 Uiso 1 calc R . C11 C 1.0160(2) 0.8340(3) 0.2716(2) 0.0498(9) Uani 1 d . . C12 C 1.0827(2) 0.8417(3) 0.3017(2) 0.0569(11) Uani 1 d . . C13 C 1.1049(2) 0.8474(3) 0.3632(2) 0.0653(12) Uani 1 d . . H13A H 1.1493(2) 0.8530(3) 0.3832(2) 0.080 Uiso 1 calc R . C14 C 1.0639(3) 0.8453(4) 0.3963(2) 0.0669(13) Uani 1 d . . C15 C 0.9986(2) 0.8321(3) 0.3650(2) 0.0603(11) Uani 1 d . . H15A H 0.9700(2) 0.8275(3) 0.3860(2) 0.080 Uiso 1 calc R . C16 C 0.9741(2) 0.8255(3) 0.3034(2) 0.0516(10) Uani 1 d . . C17 C 1.1282(2) 0.8413(4) 0.2670(2) 0.0662(13) Uani 1 d . . H17A H 1.1725(2) 0.8399(4) 0.2944(2) 0.080 Uiso 1 calc R . H17B H 1.1209(2) 0.7836(4) 0.2428(2) 0.080 Uiso 1 calc R . C18 C 0.9037(2) 0.8090(3) 0.2716(2) 0.0610(11) Uani 1 d . . H18A H 0.8982(2) 0.7516(3) 0.2473(2) 0.080 Uiso 1 calc R . H18B H 0.8824(2) 0.7981(3) 0.3005(2) 0.080 Uiso 1 calc R . C19 C 1.0886(3) 0.8597(4) 0.4640(2) 0.086(2) Uani 1 d . . C31A C 1.1669(6) 0.8758(11) 0.4897(6) 0.093(4) Uiso 0.506(13) d P . H31A H 1.1833(6) 0.8847(11) 0.5320(6) 0.080 Uiso 0.506(13) d PR . H31B H 1.1843(6) 0.8176(11) 0.4797(6) 0.080 Uiso 0.506(13) d PR . H31C H 1.1793(6) 0.9295(11) 0.4707(6) 0.080 Uiso 0.506(13) d PR . C32A C 1.0817(9) 0.7651(12) 0.4922(7) 0.121(6) Uiso 0.506(13) d P . H32A H 1.0360(9) 0.7540(12) 0.4813(7) 0.080 Uiso 0.506(13) d PR . H32B H 1.1012(9) 0.7132(12) 0.4778(7) 0.080 Uiso 0.506(13) d PR . H32C H 1.1008(9) 0.7688(12) 0.5348(7) 0.080 Uiso 0.506(13) d PR . C33A C 1.0551(6) 0.9364(9) 0.4823(5) 0.080(4) Uiso 0.506(13) d P . H33A H 1.0087(6) 0.9302(9) 0.4684(5) 0.080 Uiso 0.506(13) d PR . H33B H 1.0711(6) 0.9421(9) 0.5249(5) 0.080 Uiso 0.506(13) d PR . H33C H 1.0669(6) 0.9927(9) 0.4651(5) 0.080 Uiso 0.506(13) d PR . C31B C 1.1472(6) 0.8201(11) 0.4963(6) 0.090(4) Uiso 0.494(13) d P . H31D H 1.1798(6) 0.8439(11) 0.4815(6) 0.080 Uiso 0.494(13) d PR . H31E H 1.1567(6) 0.8414(11) 0.5366(6) 0.080 Uiso 0.494(13) d PR . H31F H 1.1469(6) 0.7511(11) 0.4952(6) 0.080 Uiso 0.494(13) d PR . C32B C 1.0397(10) 0.8104(15) 0.4939(8) 0.144(7) Uiso 0.494(13) d P . H32D H 1.0562(10) 0.8203(15) 0.5362(8) 0.080 Uiso 0.494(13) d PR . H32E H 0.9984(10) 0.8417(15) 0.4773(8) 0.080 Uiso 0.494(13) d PR . H32F H 1.0347(10) 0.7427(15) 0.4857(8) 0.080 Uiso 0.494(13) d PR . C33B C 1.0841(8) 0.9669(10) 0.4757(6) 0.096(4) Uiso 0.494(13) d P . H33D H 1.1135(8) 0.9961(10) 0.4588(6) 0.080 Uiso 0.494(13) d PR . H33E H 1.0411(8) 0.9907(10) 0.4558(6) 0.080 Uiso 0.494(13) d PR . H33F H 1.0973(8) 0.9823(10) 0.5173(6) 0.080 Uiso 0.494(13) d PR . S2 S 0.94086(5) 0.97206(8) 0.10009(4) 0.0479(2) Uani 1 d . . N3 N 1.0734(2) 1.0701(3) 0.1475(2) 0.0614(10) Uani 1 d . . H3A H 1.0767(2) 1.1142(3) 0.1759(2) 0.080 Uiso 1 calc R . H3B H 1.1141(2) 1.0556(3) 0.1494(2) 0.080 Uiso 1 calc R . N4 N 0.83134(15) 1.0239(2) 0.1451(2) 0.0515(8) Uani 1 d . . H4A H 0.79581(15) 0.9943(2) 0.1474(2) 0.080 Uiso 1 calc R . H4B H 0.84133(15) 1.0713(2) 0.1724(2) 0.080 Uiso 1 calc R . C21 C 0.9265(2) 1.0972(3) 0.0879(2) 0.0471(9) Uani 1 d . . C22 C 0.9750(2) 1.1577(3) 0.0843(2) 0.0550(10) Uani 1 d . . C23 C 0.9631(2) 1.2543(4) 0.0746(2) 0.0633(12) Uani 1 d . . H23A H 0.9964(2) 1.2940(4) 0.0725(2) 0.080 Uiso 1 calc R . C24 C 0.9030(2) 1.2951(3) 0.0676(2) 0.0613(11) Uani 1 d . . C25 C 0.8548(2) 1.2322(3) 0.0710(2) 0.0566(11) Uani 1 d . . H25A H 0.8139(2) 1.2568(3) 0.0662(2) 0.080 Uiso 1 calc R . C26 C 0.8655(2) 1.1346(3) 0.0812(2) 0.0497(9) Uani 1 d . . C27 C 1.0402(2) 1.1168(4) 0.0888(2) 0.0664(13) Uani 1 d . . H27A H 1.0344(2) 1.0699(4) 0.0574(2) 0.080 Uiso 1 calc R . H27B H 1.0675(2) 1.1681(4) 0.0829(2) 0.080 Uiso 1 calc R . C28 C 0.8125(2) 1.0707(3) 0.0850(2) 0.0553(10) Uani 1 d . . H28A H 0.8036(2) 1.0215(3) 0.0545(2) 0.080 Uiso 1 calc R . H28B H 0.7733(2) 1.1081(3) 0.0781(2) 0.080 Uiso 1 calc R . C29 C 0.8902(3) 1.4027(4) 0.0576(3) 0.0792(15) Uani 1 d . . C41A C 0.9108(9) 1.4396(11) 0.0119(8) 0.125(6) Uiso 0.528(13) d P . H41A H 0.8894(9) 1.4093(11) -0.0258(8) 0.080 Uiso 0.528(13) d PR . H41B H 0.9039(9) 1.5079(11) 0.0080(8) 0.080 Uiso 0.528(13) d PR . H41C H 0.9564(9) 1.4263(11) 0.0246(8) 0.080 Uiso 0.528(13) d PR . C42A C 0.9270(9) 1.4553(11) 0.1182(7) 0.117(5) Uiso 0.528(13) d P . H42A H 0.9729(9) 1.4440(11) 0.1305(7) 0.080 Uiso 0.528(13) d PR . H42B H 0.9188(9) 1.5232(11) 0.1150(7) 0.080 Uiso 0.528(13) d PR . H42C H 0.9103(9) 1.4283(11) 0.1470(7) 0.080 Uiso 0.528(13) d PR . C43A C 0.8185(7) 1.4325(10) 0.0489(7) 0.110(5) Uiso 0.528(13) d P . H43A H 0.7908(7) 1.4070(10) 0.0115(7) 0.080 Uiso 0.528(13) d PR . H43B H 0.8061(7) 1.4063(10) 0.0805(7) 0.080 Uiso 0.528(13) d PR . H43C H 0.8145(7) 1.5013(10) 0.0485(7) 0.080 Uiso 0.528(13) d PR . C41B C 0.9465(8) 1.4569(10) 0.0429(7) 0.095(4) Uiso 0.472(13) d P . H41D H 0.9875(8) 1.4553(10) 0.0747(7) 0.080 Uiso 0.472(13) d PR . H41E H 0.9501(8) 1.4244(10) 0.0088(7) 0.080 Uiso 0.472(13) d PR . H41F H 0.9339(8) 1.5225(10) 0.0328(7) 0.080 Uiso 0.472(13) d PR . C42B C 0.8844(11) 1.4468(13) 0.1088(8) 0.126(6) Uiso 0.472(13) d P . H42D H 0.8521(11) 1.4144(13) 0.1206(8) 0.080 Uiso 0.472(13) d PR . H42E H 0.9258(11) 1.4412(13) 0.1399(8) 0.080 Uiso 0.472(13) d PR . H42F H 0.8732(11) 1.5135(13) 0.1017(8) 0.080 Uiso 0.472(13) d PR . C43B C 0.8294(7) 1.4154(11) 0.0032(7) 0.109(5) Uiso 0.472(13) d P . H43D H 0.7936(7) 1.3857(11) 0.0110(7) 0.080 Uiso 0.472(13) d PR . H43E H 0.8199(7) 1.4822(11) -0.0059(7) 0.080 Uiso 0.472(13) d PR . H43F H 0.8362(7) 1.3840(11) -0.0299(7) 0.080 Uiso 0.472(13) d PR . B1 B 0.8221(2) 1.3091(3) 0.2842(2) 0.0447(10) Uani 1 d . . C101 C 0.8705(2) 1.4008(3) 0.3099(2) 0.0517(10) Uani 1 d . . C102 C 0.9106(2) 1.4040(4) 0.3700(2) 0.0747(14) Uani 1 d . . H10A H 0.9065(2) 1.3561(4) 0.3956(2) 0.080 Uiso 1 calc R . C103 C 0.9556(3) 1.4758(6) 0.3921(3) 0.106(2) Uani 1 d . . H10B H 0.9810(3) 1.4752(6) 0.4322(3) 0.080 Uiso 1 calc R . C104 C 0.9638(4) 1.5472(6) 0.3568(4) 0.113(2) Uani 1 d . . H10C H 0.9931(4) 1.5967(6) 0.3727(4) 0.080 Uiso 1 calc R . C105 C 0.9287(3) 1.5452(4) 0.2981(4) 0.107(2) Uani 1 d . . H10D H 0.9353(3) 1.5921(4) 0.2731(4) 0.080 Uiso 1 calc R . C106 C 0.8823(3) 1.4729(4) 0.2748(3) 0.0763(14) Uani 1 d . . H10E H 0.8586(3) 1.4733(4) 0.2343(3) 0.080 Uiso 1 calc R . C111 C 0.7682(2) 1.3263(3) 0.2173(2) 0.0490(9) Uani 1 d . . C112 C 0.7383(2) 1.4156(4) 0.1980(2) 0.0635(12) Uani 1 d . . H11A H 0.7507(2) 1.4681(4) 0.2235(2) 0.080 Uiso 1 calc R . C113 C 0.6910(3) 1.4287(5) 0.1426(3) 0.084(2) Uani 1 d . . H11B H 0.6733(3) 1.4893(5) 0.1313(3) 0.080 Uiso 1 calc R . C114 C 0.6707(3) 1.3527(6) 0.1047(2) 0.092(2) Uani 1 d . . H11C H 0.6395(3) 1.3616(6) 0.0673(2) 0.080 Uiso 1 calc R . C115 C 0.6964(2) 1.2633(5) 0.1221(2) 0.085(2) Uani 1 d . . H11D H 0.6815(2) 1.2106(5) 0.0971(2) 0.080 Uiso 1 calc R . C116 C 0.7448(2) 1.2515(4) 0.1772(2) 0.0671(13) Uani 1 d . . H11E H 0.7624(2) 1.1905(4) 0.1876(2) 0.080 Uiso 1 calc R . C121 C 0.8716(2) 1.2210(3) 0.2835(2) 0.0443(9) Uani 1 d . . C122 C 0.9010(2) 1.2169(3) 0.2396(2) 0.0522(10) Uani 1 d . . H12A H 0.8873(2) 1.2595(3) 0.2077(2) 0.080 Uiso 1 calc R . C123 C 0.9492(2) 1.1519(4) 0.2421(2) 0.0625(12) Uani 1 d . . H12B H 0.9672(2) 1.1510(4) 0.2121(2) 0.080 Uiso 1 calc R . C124 C 0.9711(2) 1.0880(4) 0.2889(3) 0.0691(13) Uani 1 d . . H12C H 1.0042(2) 1.0448(4) 0.2911(3) 0.080 Uiso 1 calc R . C125 C 0.9431(3) 1.0896(4) 0.3319(3) 0.0770(14) Uani 1 d . . H12D H 0.9570(3) 1.0466(4) 0.3635(3) 0.080 Uiso 1 calc R . C126 C 0.8942(2) 1.1547(3) 0.3288(2) 0.0616(11) Uani 1 d . . H12E H 0.8759(2) 1.1535(3) 0.3586(2) 0.080 Uiso 1 calc R . C131 C 0.7795(2) 1.2809(3) 0.3268(2) 0.0448(9) Uani 1 d . . C132 C 0.7432(2) 1.1958(3) 0.3157(2) 0.0574(11) Uani 1 d . . H13B H 0.7452(2) 1.1555(3) 0.2854(2) 0.080 Uiso 1 calc R . C133 C 0.7044(2) 1.1692(4) 0.3481(2) 0.0693(13) Uani 1 d . . H13C H 0.6813(2) 1.1118(4) 0.3393(2) 0.080 Uiso 1 calc R . C134 C 0.6996(2) 1.2263(4) 0.3928(2) 0.0682(13) Uani 1 d . . H13D H 0.6733(2) 1.2083(4) 0.4143(2) 0.080 Uiso 1 calc R . C135 C 0.7341(2) 1.3101(4) 0.4056(2) 0.0638(12) Uani 1 d . . H13E H 0.7315(2) 1.3494(4) 0.4362(2) 0.080 Uiso 1 calc R . C136 C 0.7733(2) 1.3373(3) 0.3729(2) 0.0515(10) Uani 1 d . . H13F H 0.7960(2) 1.3950(3) 0.3821(2) 0.080 Uiso 1 calc R . B2 B 1.2633(3) 1.0188(4) 0.1301(2) 0.0561(12) Uani 1 d . . C201 C 1.2256(2) 1.1231(3) 0.1122(2) 0.0590(11) Uani 1 d . . C202 C 1.1952(3) 1.1537(4) 0.0544(3) 0.088(2) Uani 1 d . . H20A H 1.1960(3) 1.1135(4) 0.0236(3) 0.080 Uiso 1 calc R . C203 C 1.1631(3) 1.2420(5) 0.0399(3) 0.113(3) Uani 1 d . . H20B H 1.1437(3) 1.2599(5) 0.0003(3) 0.080 Uiso 1 calc R . C204 C 1.1606(3) 1.3019(4) 0.0845(4) 0.098(2) Uani 1 d . . H20C H 1.1402(3) 1.3614(4) 0.0755(4) 0.080 Uiso 1 calc R . C205 C 1.1881(3) 1.2738(4) 0.1424(3) 0.085(2) Uani 1 d . . H20D H 1.1856(3) 1.3133(4) 0.1729(3) 0.080 Uiso 1 calc R . C206 C 1.2197(2) 1.1863(3) 0.1555(2) 0.0657(12) Uani 1 d . . H20E H 1.2381(2) 1.1686(3) 0.1952(2) 0.080 Uiso 1 calc R . C211 C 1.3183(2) 1.0306(3) 0.1967(2) 0.0612(11) Uani 1 d . . C212 C 1.3800(3) 1.0655(4) 0.2051(3) 0.082(2) Uani 1 d . . H21A H 1.3913(3) 1.0788(4) 0.1718(3) 0.080 Uiso 1 calc R . C213 C 1.4254(3) 1.0812(5) 0.2608(4) 0.105(2) Uani 1 d . . H21B H 1.4660(3) 1.1054(5) 0.2639(4) 0.080 Uiso 1 calc R . C214 C 1.4120(4) 1.0622(5) 0.3108(3) 0.104(2) Uani 1 d . . H21C H 1.4432(4) 1.0720(5) 0.3480(3) 0.080 Uiso 1 calc R . C215 C 1.3512(4) 1.0280(4) 0.3055(3) 0.092(2) Uani 1 d . . H21D H 1.3408(4) 1.0146(4) 0.3393(3) 0.080 Uiso 1 calc R . C216 C 1.3064(3) 1.0142(4) 0.2496(2) 0.0754(14) Uani 1 d . . H21E H 1.2654(3) 0.9923(4) 0.2468(2) 0.080 Uiso 1 calc R . C221 C 1.2986(2) 0.9859(4) 0.0819(2) 0.0611(11) Uani 1 d . . C222 C 1.3283(3) 1.0504(4) 0.0553(3) 0.080(2) Uani 1 d . . H22A H 1.3262(3) 1.1158(4) 0.0627(3) 0.080 Uiso 1 calc R . C223 C 1.3616(3) 1.0204(6) 0.0174(3) 0.090(2) Uani 1 d . . H22B H 1.3806(3) 1.0661(6) 0.0002(3) 0.080 Uiso 1 calc R . C224 C 1.3664(3) 0.9269(5) 0.0059(2) 0.085(2) Uani 1 d . . H22C H 1.3896(3) 0.9075(5) -0.0182(2) 0.080 Uiso 1 calc R . C225 C 1.3367(3) 0.8608(5) 0.0299(2) 0.081(2) Uani 1 d . . H22D H 1.3388(3) 0.7958(5) 0.0215(2) 0.080 Uiso 1 calc R . C226 C 1.3032(2) 0.8904(4) 0.0672(2) 0.0683(13) Uani 1 d . . H22E H 1.2831(2) 0.8439(4) 0.0828(2) 0.080 Uiso 1 calc R . C231 C 1.2110(2) 0.9338(3) 0.1275(2) 0.0555(10) Uani 1 d . . C232 C 1.1489(2) 0.9320(4) 0.0838(2) 0.0636(12) Uani 1 d . . H23B H 1.1360(2) 0.9840(4) 0.0580(2) 0.080 Uiso 1 calc R . C233 C 1.1060(3) 0.8562(5) 0.0775(2) 0.0793(15) Uani 1 d . . H23C H 1.0648(3) 0.8593(5) 0.0488(2) 0.080 Uiso 1 calc R . C234 C 1.1240(3) 0.7765(4) 0.1132(3) 0.081(2) Uani 1 d . . H23D H 1.0956(3) 0.7251(4) 0.1087(3) 0.080 Uiso 1 calc R . C235 C 1.1843(3) 0.7739(4) 0.1554(2) 0.0760(14) Uani 1 d . . H23E H 1.1969(3) 0.7199(4) 0.1796(2) 0.080 Uiso 1 calc R . C236 C 1.2270(2) 0.8499(3) 0.1632(2) 0.0644(12) Uani 1 d . . H23F H 1.2676(2) 0.8458(3) 0.1927(2) 0.080 Uiso 1 calc R . N5 N 1.0974(4) 1.2465(7) 0.2483(4) 0.159(3) Uani 1 d . . C51 C 1.0740(4) 1.2966(7) 0.2737(5) 0.120(3) Uani 1 d . . C52 C 1.0444(4) 1.3510(6) 0.3080(4) 0.144(3) Uani 1 d . . H52A H 1.0432(4) 1.4178(6) 0.2974(4) 0.080 Uiso 1 d R . H52B H 1.0010(4) 1.3282(6) 0.3004(4) 0.080 Uiso 1 d R . H52C H 1.0691(4) 1.3434(6) 0.3495(4) 0.080 Uiso 1 d R . C53 C 1.1888(8) 1.0921(10) 0.3680(5) 0.227(7) Uani 1 d . . O1 O 1.1728(4) 1.0890(6) 0.3064(4) 0.206(3) Uani 1 d . . 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 0.0358(3) 0.0651(3) 0.0423(3) -0.0014(2) 0.0130(2) 0.0063(2) Ni2 0.0343(2) 0.0540(3) 0.0399(3) -0.0034(2) 0.0090(2) -0.0009(2) S1 0.0474(5) 0.0554(6) 0.0397(5) -0.0040(4) 0.0108(4) 0.0061(4) N1 0.040(2) 0.086(3) 0.058(2) 0.001(2) 0.014(2) 0.011(2) N2 0.042(2) 0.070(2) 0.050(2) -0.001(2) 0.013(2) -0.003(2) C11 0.049(2) 0.052(2) 0.044(2) -0.001(2) 0.010(2) 0.009(2) C12 0.049(2) 0.066(3) 0.052(2) 0.001(2) 0.012(2) 0.016(2) C13 0.057(3) 0.075(3) 0.050(3) 0.003(2) 0.001(2) 0.021(2) C14 0.080(3) 0.069(3) 0.044(2) 0.007(2) 0.010(2) 0.028(3) C15 0.070(3) 0.064(3) 0.047(2) 0.012(2) 0.020(2) 0.021(2) C16 0.055(2) 0.050(2) 0.049(2) 0.007(2) 0.016(2) 0.007(2) C17 0.043(2) 0.090(3) 0.058(3) 0.010(2) 0.008(2) 0.023(2) C18 0.061(3) 0.066(3) 0.060(3) 0.007(2) 0.026(2) -0.005(2) C19 0.099(4) 0.098(4) 0.044(3) 0.002(3) 0.003(3) 0.043(3) S2 0.0430(5) 0.0592(6) 0.0385(5) -0.0027(4) 0.0103(4) 0.0050(4) N3 0.038(2) 0.084(3) 0.066(2) 0.004(2) 0.022(2) 0.002(2) N4 0.036(2) 0.057(2) 0.060(2) -0.001(2) 0.0141(15) -0.0042(15) C21 0.044(2) 0.065(3) 0.034(2) 0.000(2) 0.015(2) 0.002(2) C22 0.048(2) 0.071(3) 0.049(2) 0.006(2) 0.020(2) 0.003(2) C23 0.065(3) 0.072(3) 0.058(3) 0.007(2) 0.027(2) -0.005(2) C24 0.066(3) 0.064(3) 0.051(2) 0.006(2) 0.016(2) 0.003(2) C25 0.053(2) 0.064(3) 0.048(2) 0.004(2) 0.012(2) 0.008(2) C26 0.044(2) 0.062(3) 0.040(2) -0.001(2) 0.009(2) 0.003(2) C27 0.053(3) 0.088(3) 0.068(3) 0.017(3) 0.035(2) 0.003(2) C28 0.036(2) 0.062(3) 0.059(3) 0.003(2) 0.005(2) 0.005(2) C29 0.090(4) 0.065(3) 0.086(4) 0.012(3) 0.035(3) 0.008(3) B1 0.048(2) 0.048(2) 0.040(2) 0.002(2) 0.017(2) 0.006(2) C101 0.053(2) 0.050(2) 0.054(2) -0.001(2) 0.020(2) 0.005(2) C102 0.059(3) 0.090(4) 0.065(3) -0.008(3) 0.009(2) -0.012(3) C103 0.071(4) 0.128(6) 0.103(5) -0.037(5) 0.008(3) -0.018(4) C104 0.086(5) 0.096(5) 0.144(7) -0.031(5) 0.023(5) -0.033(4) C105 0.088(4) 0.063(4) 0.169(8) 0.017(4) 0.044(5) -0.009(3) C106 0.066(3) 0.066(3) 0.093(4) 0.010(3) 0.021(3) -0.004(3) C111 0.046(2) 0.062(3) 0.043(2) 0.003(2) 0.020(2) 0.007(2) C112 0.059(3) 0.068(3) 0.060(3) 0.016(2) 0.016(2) 0.008(2) C113 0.073(3) 0.100(4) 0.072(4) 0.038(3) 0.015(3) 0.021(3) C114 0.065(3) 0.154(6) 0.049(3) 0.011(4) 0.010(2) 0.022(4) C115 0.061(3) 0.133(5) 0.051(3) -0.030(3) 0.008(2) 0.016(3) C116 0.054(3) 0.088(3) 0.053(3) -0.016(2) 0.011(2) 0.015(2) C121 0.044(2) 0.045(2) 0.042(2) -0.004(2) 0.012(2) 0.000(2) C122 0.044(2) 0.065(3) 0.048(2) -0.007(2) 0.015(2) -0.002(2) C123 0.041(2) 0.078(3) 0.070(3) -0.028(3) 0.021(2) -0.006(2) C124 0.047(2) 0.061(3) 0.092(4) -0.017(3) 0.014(2) 0.009(2) C125 0.075(3) 0.069(3) 0.084(4) 0.020(3) 0.023(3) 0.024(3) C126 0.067(3) 0.064(3) 0.058(3) 0.009(2) 0.027(2) 0.019(2) C131 0.043(2) 0.053(2) 0.036(2) 0.002(2) 0.010(2) 0.009(2) C132 0.062(3) 0.060(3) 0.052(2) -0.004(2) 0.022(2) 0.002(2) C133 0.068(3) 0.078(3) 0.067(3) 0.003(3) 0.031(2) -0.011(3) C134 0.066(3) 0.087(4) 0.062(3) 0.018(3) 0.035(2) 0.012(3) C135 0.067(3) 0.084(3) 0.044(2) 0.004(2) 0.024(2) 0.025(3) C136 0.048(2) 0.060(3) 0.044(2) 0.001(2) 0.012(2) 0.013(2) B2 0.060(3) 0.061(3) 0.057(3) 0.009(2) 0.032(2) 0.011(2) C201 0.057(3) 0.067(3) 0.065(3) 0.015(2) 0.037(2) 0.007(2) C202 0.105(4) 0.098(4) 0.080(4) 0.033(3) 0.058(3) 0.044(3) C203 0.125(5) 0.133(6) 0.115(5) 0.078(5) 0.086(5) 0.062(5) C204 0.096(4) 0.070(4) 0.150(6) 0.045(4) 0.073(5) 0.029(3) C205 0.075(3) 0.054(3) 0.130(5) -0.008(3) 0.039(4) 0.006(3) C206 0.054(3) 0.061(3) 0.079(3) -0.005(2) 0.020(2) 0.000(2) C211 0.061(3) 0.062(3) 0.064(3) 0.005(2) 0.026(2) 0.013(2) C212 0.068(3) 0.096(4) 0.084(4) -0.011(3) 0.030(3) 0.002(3) C213 0.067(4) 0.120(5) 0.118(6) -0.031(4) 0.020(4) 0.001(4) C214 0.098(5) 0.096(5) 0.088(5) -0.027(4) -0.005(4) 0.027(4) C215 0.130(6) 0.078(4) 0.060(3) 0.002(3) 0.020(3) 0.015(4) C216 0.085(4) 0.080(4) 0.061(3) -0.001(3) 0.024(3) 0.000(3) C221 0.051(2) 0.082(3) 0.055(3) 0.007(2) 0.024(2) 0.012(2) C222 0.075(3) 0.092(4) 0.089(4) 0.010(3) 0.050(3) 0.008(3) C223 0.073(4) 0.131(6) 0.083(4) 0.011(4) 0.046(3) 0.000(4) C224 0.057(3) 0.141(6) 0.061(3) -0.018(3) 0.025(2) 0.008(3) C225 0.072(3) 0.109(4) 0.069(3) -0.020(3) 0.032(3) 0.012(3) C226 0.062(3) 0.087(4) 0.060(3) -0.002(2) 0.026(2) 0.012(3) C231 0.056(2) 0.066(3) 0.053(2) 0.003(2) 0.030(2) 0.014(2) C232 0.066(3) 0.080(3) 0.050(2) 0.002(2) 0.026(2) 0.010(3) C233 0.069(3) 0.108(4) 0.061(3) -0.015(3) 0.022(3) -0.007(3) C234 0.094(4) 0.079(4) 0.075(4) -0.013(3) 0.035(3) -0.018(3) C235 0.100(4) 0.061(3) 0.078(3) 0.004(3) 0.043(3) 0.001(3) C236 0.068(3) 0.064(3) 0.064(3) 0.009(2) 0.027(2) 0.010(2) N5 0.103(5) 0.192(8) 0.212(8) -0.038(7) 0.091(5) -0.042(5) C51 0.075(5) 0.122(6) 0.170(8) -0.001(6) 0.049(5) -0.022(4) C52 0.088(5) 0.115(6) 0.199(9) -0.042(6) 0.009(6) -0.018(5) C53 0.300(17) 0.219(13) 0.121(8) -0.025(9) 0.021(10) -0.110(12) O1 0.193(7) 0.192(7) 0.226(9) -0.095(7) 0.063(7) -0.045(6) _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 N1 1.930(3) . ? Ni1 N3 1.941(4) . ? Ni1 S2 2.1828(13) . ? Ni1 S1 2.1885(13) . ? Ni1 Ni2 2.9731(9) . ? Ni2 N2 1.935(3) . ? Ni2 N4 1.939(3) . ? Ni2 S2 2.1819(12) . ? Ni2 S1 2.1875(12) . ? S1 C11 1.779(4) . ? N1 C17 1.481(6) . ? N2 C18 1.482(6) . ? C11 C12 1.396(6) . ? C11 C16 1.384(6) . ? C12 C13 1.385(6) . ? C12 C17 1.500(6) . ? C13 C14 1.386(7) . ? C14 C15 1.384(7) . ? C14 C19 1.534(6) . ? C15 C16 1.389(6) . ? C16 C18 1.488(6) . ? C19 C31A 1.630(14) . ? C19 C31B 1.370(13) . ? C19 C32A 1.51(2) . ? C19 C32B 1.63(2) . ? C19 C33A 1.445(12) . ? C19 C33B 1.525(14) . ? S2 C21 1.774(4) . ? N3 C27 1.493(6) . ? N4 C28 1.500(5) . ? C21 C22 1.382(6) . ? C21 C26 1.394(5) . ? C22 C23 1.373(6) . ? C22 C27 1.508(6) . ? C23 C24 1.392(6) . ? C24 C25 1.396(6) . ? C24 C29 1.526(7) . ? C25 C26 1.385(6) . ? C26 C28 1.491(6) . ? C29 C41A 1.41(2) . ? C29 C42B 1.41(2) . ? C29 C42A 1.58(2) . ? C29 C41B 1.585(15) . ? C29 C43B 1.52(2) . ? C29 C43A 1.569(14) . ? B1 C101 1.638(6) . ? B1 C111 1.649(6) . ? B1 C121 1.641(6) . ? B1 C131 1.649(6) . ? C101 C102 1.405(6) . ? C101 C106 1.388(7) . ? C102 C103 1.376(8) . ? C103 C104 1.355(10) . ? C104 C105 1.350(10) . ? C105 C106 1.403(8) . ? C111 C112 1.406(6) . ? C111 C116 1.389(6) . ? C112 C113 1.388(7) . ? C113 C114 1.363(8) . ? C114 C115 1.369(8) . ? C115 C116 1.391(7) . ? C121 C122 1.410(5) . ? C121 C126 1.380(6) . ? C122 C123 1.378(6) . ? C123 C124 1.380(7) . ? C124 C125 1.366(7) . ? C125 C126 1.387(6) . ? C131 C132 1.400(6) . ? C131 C136 1.397(5) . ? C132 C133 1.381(6) . ? C133 C134 1.365(7) . ? C134 C135 1.366(7) . ? C135 C136 1.398(6) . ? B2 C201 1.651(7) . ? B2 C211 1.645(7) . ? B2 C221 1.658(6) . ? B2 C231 1.635(7) . ? C201 C202 1.382(7) . ? C201 C206 1.397(6) . ? C202 C203 1.398(8) . ? C203 C204 1.369(10) . ? C204 C205 1.363(9) . ? C205 C206 1.381(7) . ? C211 C212 1.386(7) . ? C211 C216 1.395(7) . ? C212 C213 1.380(9) . ? C213 C214 1.352(10) . ? C214 C215 1.381(10) . ? C215 C216 1.377(8) . ? C221 C222 1.384(7) . ? C221 C226 1.386(7) . ? C222 C223 1.408(7) . ? C223 C224 1.340(9) . ? C224 C225 1.362(8) . ? C225 C226 1.397(6) . ? C231 C232 1.404(6) . ? C231 C236 1.417(6) . ? C232 C233 1.386(7) . ? C233 C234 1.372(8) . ? C234 C235 1.362(8) . ? C235 C236 1.381(7) . ? N5 C51 1.153(10) . ? C51 C52 1.425(11) . ? C53 O1 1.393(12) . ? 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 N1 Ni1 S1 95.12(12) . . ? N1 Ni1 S2 174.64(13) . . ? N1 Ni1 N3 89.0(2) . . ? N3 Ni1 S2 95.52(11) . . ? N3 Ni1 S1 173.76(11) . . ? S2 Ni1 S1 80.61(4) . . ? N2 Ni2 S1 95.76(11) . . ? N2 Ni2 S2 176.32(10) . . ? N2 Ni2 N4 88.80(14) . . ? N4 Ni2 S1 175.09(10) . . ? N4 Ni2 S2 94.75(11) . . ? S2 Ni2 S1 80.65(4) . . ? Ni1 S1 Ni2 85.60(4) . . ? C11 S1 Ni1 104.02(15) . . ? C11 S1 Ni2 104.66(14) . . ? C17 N1 Ni1 121.0(3) . . ? C18 N2 Ni2 120.1(3) . . ? S1 C11 C12 119.8(3) . . ? S1 C11 C16 120.3(3) . . ? C12 C11 C16 119.9(4) . . ? C11 C12 C13 118.7(4) . . ? C11 C12 C17 119.4(4) . . ? C13 C12 C17 121.9(4) . . ? C12 C13 C14 122.9(4) . . ? C13 C14 C15 116.7(4) . . ? C13 C14 C19 122.4(5) . . ? C15 C14 C19 120.9(5) . . ? C14 C15 C16 122.4(4) . . ? C11 C16 C15 119.3(4) . . ? C11 C16 C18 120.1(4) . . ? C15 C16 C18 120.6(4) . . ? N1 C17 C12 112.0(4) . . ? N2 C18 C16 112.4(4) . . ? C14 C19 C31A 111.2(6) . . ? C14 C19 C32A 107.8(8) . . ? C14 C19 C33A 112.6(6) . . ? C14 C19 C31B 117.9(7) . . ? C14 C19 C32B 111.2(8) . . ? C14 C19 C33B 107.5(6) . . ? C31A C19 C32A 101.7(8) . . ? C31A C19 C33A 111.3(8) . . ? C32A C19 C33A 111.6(9) . . ? C31B C19 C32B 102.4(10) . . ? C31B C19 C33B 113.3(9) . . ? C32B C19 C33B 103.7(10) . . ? Ni1 S2 Ni2 85.87(4) . . ? C21 S2 Ni1 107.54(13) . . ? C21 S2 Ni2 106.55(13) . . ? C27 N3 Ni1 119.3(3) . . ? C28 N4 Ni2 120.2(3) . . ? S2 C21 C22 120.7(3) . . ? S2 C21 C26 119.6(3) . . ? C22 C21 C26 119.7(4) . . ? C21 C22 C23 120.0(4) . . ? C21 C22 C27 119.9(4) . . ? C23 C22 C27 120.1(4) . . ? C22 C23 C24 122.4(4) . . ? C23 C24 C25 116.3(4) . . ? C23 C24 C29 122.3(5) . . ? C25 C24 C29 121.4(4) . . ? C24 C25 C26 122.6(4) . . ? C21 C26 C25 118.9(4) . . ? C21 C26 C28 120.7(4) . . ? C25 C26 C28 120.4(4) . . ? N3 C27 C22 112.1(3) . . ? N4 C28 C26 110.6(3) . . ? C24 C29 C41A 112.8(8) . . ? C24 C29 C42A 107.5(7) . . ? C24 C29 C43A 113.7(7) . . ? C24 C29 C41B 112.6(7) . . ? C24 C29 C42B 110.8(8) . . ? C24 C29 C43B 108.0(7) . . ? C41A C29 C42A 110.1(10) . . ? C41A C29 C43A 111.8(9) . . ? C42A C29 C43A 100.1(9) . . ? C41B C29 C42B 107.1(11) . . ? C41B C29 C43B 106.1(9) . . ? C42B C29 C43B 112.3(11) . . ? C101 B1 C111 114.2(3) . . ? C101 B1 C121 103.8(3) . . ? C101 B1 C131 112.6(3) . . ? C111 B1 C121 110.8(3) . . ? C111 B1 C131 105.3(3) . . ? C121 B1 C131 110.2(3) . . ? C102 C101 B1 120.5(4) . . ? C106 C101 B1 124.5(4) . . ? C102 C101 C106 114.4(4) . . ? C101 C102 C103 122.2(6) . . ? C102 C103 C104 121.4(7) . . ? C103 C104 C105 118.9(6) . . ? C104 C105 C106 120.4(7) . . ? C101 C106 C105 122.5(6) . . ? C112 C111 B1 123.0(4) . . ? C116 C111 B1 122.3(4) . . ? C112 C111 C116 114.4(4) . . ? C111 C112 C113 122.8(5) . . ? C112 C113 C114 120.1(5) . . ? C113 C114 C115 119.6(5) . . ? C114 C115 C116 119.7(5) . . ? C111 C116 C115 123.3(5) . . ? C122 C121 B1 120.7(3) . . ? C126 C121 B1 123.6(3) . . ? C122 C121 C126 115.2(4) . . ? C121 C122 C123 122.3(4) . . ? C122 C123 C124 120.4(4) . . ? C123 C124 C125 118.7(4) . . ? C124 C125 C126 120.6(5) . . ? C121 C126 C125 122.8(4) . . ? C132 C131 B1 119.4(3) . . ? C136 C131 B1 125.6(4) . . ? C132 C131 C136 114.9(4) . . ? C131 C132 C136 122.6(4) . . ? C132 C133 C134 120.7(5) . . ? C133 C134 C135 119.1(4) . . ? C134 C135 C136 120.3(4) . . ? C131 C136 C135 122.3(4) . . ? C201 B2 C211 107.4(4) . . ? C201 B2 C221 112.0(4) . . ? C201 B2 C231 110.0(4) . . ? C211 B2 C221 109.8(4) . . ? C211 B2 C231 112.5(4) . . ? C221 B2 C231 105.3(4) . . ? C202 C201 B2 123.8(4) . . ? C206 C201 B2 121.7(4) . . ? C202 C201 C206 114.4(4) . . ? C201 C202 C203 123.2(6) . . ? C202 C203 C204 119.5(6) . . ? C203 C204 C205 119.6(5) . . ? C204 C205 C206 119.8(6) . . ? C201 C206 C205 123.5(5) . . ? C212 C211 B2 122.1(4) . . ? C216 C211 B2 124.0(4) . . ? C212 C211 C216 113.7(5) . . ? C211 C212 C213 122.9(6) . . ? C212 C213 C214 121.2(7) . . ? C213 C214 C215 118.9(6) . . ? C214 C215 C216 118.9(6) . . ? C211 C216 C215 124.4(6) . . ? C222 C221 B2 123.1(5) . . ? C226 C221 B2 122.2(4) . . ? C222 C221 C226 114.7(4) . . ? C221 C222 C223 122.2(6) . . ? C222 C223 C224 121.0(6) . . ? C223 C224 C225 119.0(5) . . ? C224 C225 C226 120.2(6) . . ? C221 C226 C225 122.9(5) . . ? C232 C231 C236 114.3(4) . . ? C232 C231 B2 122.1(4) . . ? C236 C231 B2 123.1(4) . . ? C231 C232 C233 123.0(5) . . ? C232 C233 C234 120.4(5) . . ? C233 C234 C235 118.8(5) . . ? C234 C235 C236 121.4(5) . . ? C231 C236 C235 122.0(5) . . ? N5 C51 C52 174.8(10) . . ? _refine_diff_density_max 0.791 _refine_diff_density_min -0.775 _refine_diff_density_rms 0.071 #Compound: [L3Ni2][BPh4]2xMeOH data_nii _audit_creation_method SHELXL _chemical_name_systematic ; Tris(2,6-di(aminomethyl)-4-tert-butyl-thiophenolato)dinickel(III,II) -di(tetraphenylborate)-methanol ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ; [(2,6(CH2NH2)2-4-t-Bu-C6H2S)3Ni2][B(C6H5)4]2MeOH ;? _chemical_formula_analytical ? _chemical_formula_sum 'C85 H101 B2 N6 Ni2 O S3' _chemical_formula_weight 1457.94 _chemical_melting_point ? _chemical_compound_source MeOH loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic P' _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.678(5) _cell_length_b 20.090(4) _cell_length_c 16.797(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.16(3) _cell_angle_gamma 90.00 _cell_volume 7674.5(26) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method ? _exptl_crystal_F_000 3100 _exptl_absorpt_coefficient_mu 0.622 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 0.98 _exptl_special_details ; Crystals were grown from methanol ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device STOE-IPDS _diffrn_measurement_method ; STOE IPDS MEASUREMENT AND DATA EVALUATION SUMMARY for NII EXPOSE Date and time 09-Dec-97 15:17 Wavelength [A] 0.71073 (First) exposure 1 Tube power [kW] 1.75 Tube voltage [kV] 50 Tube current [mA] 35 Collimator size [mm] 0.5 Temperature [K] 213.0 Detector distance [mm] 70.0 2theta range [degrees] 8.1 52.1 d(hkl) range [A] 5.013 0.809 Phi movement mode Rotation Phi start [degrees] 160.0 Phi end [degrees] 360.0 Phi incr. [degrees] 1.0 Number of exposures 200 Irradiation / exposure [min] 4.00 Measurement duration [h] 27 PROFILE Profile function Dynamic Smallest profile diameter [pixels] 13 Largest profile diameter [pixels] 17 Chi^2 of fit [pixels^2] 0.1 INTEGRATE Profile function Dynamic Smallest profile diameter [pixels] 13 Largest profile diameter [pixels] 17 Automated overlap check? Yes Overlap tolerance [pixel] 0 Exposure range 1 182 Control reflections 50 200 I/sigma limit for control reflections 8.0 Crystal system triclinic Lattice type P Initial a [A] 16.80 Initial b [A] 20.08 Initial c [A] 23.68 Initial alpha [degrees] 90.07 Initial beta [degrees] 106.18 Initial gamma [degrees] 90.06 Effective mosaic spread 0.011 Direction cosines? Yes q vector mode (6 indices)? No Overlapped reflections 0 Overloaded reflections 18 Total number of stored reflections 55230 100% Reflections with Fo2 > 1 * sigma(Fo2) 43061 78% Reflections with Fo2 > 2 * sigma(Fo2) 37605 68% Reflections with Fo2 > 4 * sigma(Fo2) 30233 55% Mean Fo2/sigma(Fo2) 12.8 SELECT Minimum input phi [degrees] 160.0 Maximum input phi [degrees] 342.0 Minimum output phi [degrees] 160.0 Maximum output phi [degrees] 342.0 Minimum input 2theta [degrees] 8.9 Maximum input 2theta [degrees] 52.0 Minimum output 2theta [degrees] 8.9 Maximum output 2theta [degrees] 52.0 Minimum input I/sigma(I) 8.0 Maximum input I/sigma(I) 910.3 Minimum output I/sigma(I) 8.0 Maximum output I/sigma(I) 910.3 Minimum input Chi^2 [A^-2] 0.23E-08 Maximum input Chi^2 [A^-2] 0.18E-03 CELL Number of reflections 5000 Lattice triclinic P A [A] 16.7966 0.0011 B [A] 20.0905 0.0013 C [A] 23.6785 0.0015 Alpha [degrees] 89.968 0.007 Beta [degrees] 106.158 0.007 Gamma [degrees] 90.055 0.007 Volume [A^3] 7674.7 Orientation [A^-1] -0.023258 -0.044485 -0.015005 0.057037 -0.019430 0.011979 -0.006921 -0.011007 0.039556 DECAY Correction desired. Smooth factor: 0 First exposure number 1 Last exposure number 182 Number of stored reflections 55230 Direction cosines Stored ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54356 _diffrn_reflns_av_R_equivalents 0.1148 _diffrn_reflns_av_sigmaI/netI 0.0760 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.37 _diffrn_reflns_theta_max 26.01 _reflns_number_total 14892 _reflns_number_observed 11240 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+6.4051P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14890 _refine_ls_number_parameters 882 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_obs 0.0504 _refine_ls_wR_factor_all 0.1360 _refine_ls_wR_factor_obs 0.1202 _refine_ls_goodness_of_fit_all 0.999 _refine_ls_goodness_of_fit_obs 1.025 _refine_ls_restrained_S_all 1.000 _refine_ls_restrained_S_obs 1.025 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.319587(14) 0.40959(2) 0.26724(2) 0.03022(10) Uani 1 d . . Ni2 Ni 0.187463(14) 0.43618(2) 0.19928(2) 0.03113(10) Uani 1 d . . S1 S 0.23975(3) 0.37666(4) 0.31836(5) 0.0345(2) Uani 1 d . . C101 C 0.22819(12) 0.29278(15) 0.2871(2) 0.0348(6) Uani 1 d . . C102 C 0.27524(13) 0.2479(2) 0.3014(2) 0.0401(7) Uani 1 d . . C103 C 0.26422(15) 0.1813(2) 0.2806(2) 0.0454(8) Uani 1 d . . H13 H 0.29575(15) 0.1519(2) 0.2902(2) 0.080 Uiso 1 calc R . C104 C 0.20794(14) 0.1570(2) 0.2461(2) 0.0415(7) Uani 1 d . . C105 C 0.16172(14) 0.2026(2) 0.2309(2) 0.0387(7) Uani 1 d . . H15 H 0.12357(14) 0.1877(2) 0.2071(2) 0.080 Uiso 1 calc R . C106 C 0.17104(13) 0.2697(2) 0.2504(2) 0.0360(7) Uani 1 d . . C107 C 0.33750(13) 0.2699(2) 0.3396(2) 0.0433(8) Uani 1 d . . H17A H 0.34023(13) 0.2926(2) 0.3916(2) 0.080 Uiso 1 calc R . H17B H 0.36306(13) 0.2313(2) 0.3514(2) 0.080 Uiso 1 calc R . N1 N 0.35723(10) 0.31567(13) 0.2826(2) 0.0381(6) Uani 1 d . . H1A H 0.34957(10) 0.29611(13) 0.2325(2) 0.080 Uiso 1 calc R . H1B H 0.39648(10) 0.32043(13) 0.3017(2) 0.080 Uiso 1 calc R . C108 C 0.1955(2) 0.0837(2) 0.2234(3) 0.0480(8) Uani 1 d . . C109 C 0.11989(13) 0.3167(2) 0.2299(2) 0.0413(7) Uani 1 d . . H19A H 0.08355(13) 0.2918(2) 0.2106(2) 0.080 Uiso 1 calc R . H19B H 0.11869(13) 0.3412(2) 0.2792(2) 0.080 Uiso 1 calc R . N2 N 0.12547(10) 0.36424(13) 0.1642(2) 0.0389(6) Uani 1 d . . H2A H 0.09041(10) 0.38413(13) 0.1432(2) 0.080 Uiso 1 calc R . H2B H 0.13330(10) 0.34065(13) 0.1229(2) 0.080 Uiso 1 calc R . C110 C 0.1503(2) 0.0563(2) 0.2622(4) 0.087(2) Uani 1 d . . H10A H 0.1147(2) 0.0818(2) 0.2444(4) 0.080 Uiso 1 d R . H10B H 0.1422(2) 0.0107(2) 0.2458(4) 0.080 Uiso 1 d R . H10C H 0.1653(2) 0.0588(2) 0.3214(4) 0.080 Uiso 1 d R . C111 C 0.2509(2) 0.0407(2) 0.2536(4) 0.0827(15) Uani 1 d . . H11A H 0.2652(2) 0.0436(2) 0.3129(4) 0.080 Uiso 1 d R . H11B H 0.2419(2) -0.0048(2) 0.2377(4) 0.080 Uiso 1 d R . H11C H 0.2804(2) 0.0569(2) 0.2291(4) 0.080 Uiso 1 d R . C112 C 0.1738(3) 0.0780(2) 0.1304(3) 0.0846(15) Uani 1 d . . H12A H 0.1388(3) 0.1042(2) 0.1103(3) 0.080 Uiso 1 d R . H12B H 0.2036(3) 0.0939(2) 0.1066(3) 0.080 Uiso 1 d R . H12C H 0.1652(3) 0.0322(2) 0.1151(3) 0.080 Uiso 1 d R . S2 S 0.26454(3) 0.50912(4) 0.24390(5) 0.0320(2) Uani 1 d . . C201 C 0.26272(12) 0.53631(15) 0.3426(2) 0.0336(6) Uani 1 d . . C202 C 0.31496(12) 0.5402(2) 0.4076(2) 0.0356(7) Uani 1 d . . C203 C 0.31375(14) 0.5705(2) 0.4812(2) 0.0382(7) Uani 1 d . . H23 H 0.34861(14) 0.5739(2) 0.5235(2) 0.080 Uiso 1 calc R . C204 C 0.26251(14) 0.5960(2) 0.4942(2) 0.0408(7) Uani 1 d . . C205 C 0.21074(14) 0.5885(2) 0.4306(2) 0.0417(7) Uani 1 d . . H25 H 0.17563(14) 0.6033(2) 0.4390(2) 0.080 Uiso 1 calc R . C206 C 0.20969(13) 0.5598(2) 0.3551(2) 0.0377(7) Uani 1 d . . C207 C 0.37270(12) 0.5141(2) 0.3994(2) 0.0372(7) Uani 1 d . . H27A H 0.38208(12) 0.5361(2) 0.3532(2) 0.080 Uiso 1 calc R . H27B H 0.40357(12) 0.5245(2) 0.4493(2) 0.080 Uiso 1 calc R . N3 N 0.37075(10) 0.44127(13) 0.3858(2) 0.0364(6) Uani 1 d . . H3A H 0.35642(10) 0.42196(13) 0.4244(2) 0.080 Uiso 1 calc R . H3B H 0.40778(10) 0.42649(13) 0.3936(2) 0.080 Uiso 1 calc R . C208 C 0.2637(2) 0.6332(2) 0.5741(3) 0.0539(9) Uani 1 d . . C209 C 0.15266(13) 0.5558(2) 0.2875(2) 0.0413(7) Uani 1 d . . H29A H 0.12194(13) 0.5774(2) 0.3061(2) 0.080 Uiso 1 calc R . H29B H 0.15669(13) 0.5796(2) 0.2391(2) 0.080 Uiso 1 calc R . N4 N 0.13530(10) 0.48620(13) 0.2642(2) 0.0378(6) Uani 1 d . . H4A H 0.09774(10) 0.48599(13) 0.2326(2) 0.080 Uiso 1 calc R . H4B H 0.13668(10) 0.46315(13) 0.3106(2) 0.080 Uiso 1 calc R . C210 C 0.2071(3) 0.6347(3) 0.5969(4) 0.0466(15) Uiso 0.601(8) d P 1 H10D H 0.1775(3) 0.6566(3) 0.5541(4) 0.080 Uiso 0.601(8) d PR 1 H10E H 0.1948(3) 0.5900(3) 0.6034(4) 0.080 Uiso 0.601(8) d PR 1 H10F H 0.2127(3) 0.6584(3) 0.6481(4) 0.080 Uiso 0.601(8) d PR 1 C211 C 0.3091(3) 0.5946(4) 0.6531(5) 0.064(2) Uiso 0.601(8) d P 1 H11D H 0.3102(3) 0.6175(4) 0.7036(5) 0.080 Uiso 0.601(8) d PR 1 H11E H 0.2958(3) 0.5497(4) 0.6561(5) 0.080 Uiso 0.601(8) d PR 1 H11F H 0.3478(3) 0.5939(4) 0.6454(5) 0.080 Uiso 0.601(8) d PR 1 C212 C 0.2902(4) 0.6985(4) 0.5737(5) 0.073(2) Uiso 0.601(8) d P 1 H12D H 0.2661(4) 0.7244(4) 0.5290(5) 0.080 Uiso 0.601(8) d PR 1 H12E H 0.2934(4) 0.7207(4) 0.6253(5) 0.080 Uiso 0.601(8) d PR 1 H12F H 0.3286(4) 0.6933(4) 0.5659(5) 0.080 Uiso 0.601(8) d PR 1 C213 C 0.2213(7) 0.6017(9) 0.6114(10) 0.098(5) Uiso 0.399(8) d P 2 H13A H 0.2350(7) 0.5595(9) 0.6360(10) 0.080 Uiso 0.399(8) d PR 2 H13B H 0.2134(7) 0.6306(9) 0.6527(10) 0.080 Uiso 0.399(8) d PR 2 H13C H 0.1859(7) 0.5954(9) 0.5673(10) 0.080 Uiso 0.399(8) d PR 2 C214 C 0.3181(5) 0.6537(7) 0.6206(8) 0.074(4) Uiso 0.399(8) d P 2 H14A H 0.3406(5) 0.6155(7) 0.6452(8) 0.080 Uiso 0.399(8) d PR 2 H14B H 0.3376(5) 0.6758(7) 0.5850(8) 0.080 Uiso 0.399(8) d PR 2 H14C H 0.3146(5) 0.6837(7) 0.6634(8) 0.080 Uiso 0.399(8) d PR 2 C215 C 0.2281(6) 0.7049(7) 0.5367(9) 0.082(4) Uiso 0.399(8) d P 2 H15A H 0.2534(6) 0.7302(7) 0.5124(9) 0.080 Uiso 0.399(8) d PR 2 H15B H 0.1921(6) 0.6950(7) 0.4952(9) 0.080 Uiso 0.399(8) d PR 2 H15C H 0.2197(6) 0.7302(7) 0.5805(9) 0.080 Uiso 0.399(8) d PR 2 S3 S 0.25394(3) 0.38432(4) 0.12996(5) 0.0341(2) Uani 1 d . . C301 C 0.26978(13) 0.45105(15) 0.0703(2) 0.0332(6) Uani 1 d . . C302 C 0.32833(12) 0.4669(2) 0.0745(2) 0.0348(6) Uani 1 d . . C303 C 0.33999(13) 0.5199(2) 0.0287(2) 0.0382(7) Uani 1 d . . H33 H 0.37897(13) 0.5299(2) 0.0323(2) 0.080 Uiso 1 calc R . C304 C 0.29614(14) 0.5588(2) -0.0221(2) 0.0396(7) Uani 1 d . . C305 C 0.23849(14) 0.5423(2) -0.0249(2) 0.0396(7) Uani 1 d . . H35 H 0.20803(14) 0.5676(2) -0.0582(2) 0.080 Uiso 1 calc R . C306 C 0.22459(13) 0.4896(2) 0.0202(2) 0.0373(7) Uani 1 d . . C307 C 0.37897(13) 0.4290(2) 0.1298(2) 0.0371(7) Uani 1 d . . H37A H 0.37228(13) 0.3816(2) 0.1212(2) 0.080 Uiso 1 calc R . H37B H 0.41494(13) 0.4403(2) 0.1160(2) 0.080 Uiso 1 calc R . N5 N 0.38521(10) 0.44563(13) 0.2177(2) 0.0339(5) Uani 1 d . . H5A H 0.38638(10) 0.49024(13) 0.2230(2) 0.080 Uiso 1 calc R . H5B H 0.42000(10) 0.42975(13) 0.2485(2) 0.080 Uiso 1 calc R . C308 C 0.3128(2) 0.6178(2) -0.0687(2) 0.0502(8) Uani 1 d . . C309 C 0.16134(13) 0.4752(2) 0.0146(2) 0.0427(7) Uani 1 d . . H39A H 0.13617(13) 0.5003(2) -0.0309(2) 0.080 Uiso 1 calc R . H39B H 0.15354(13) 0.4282(2) 0.0033(2) 0.080 Uiso 1 calc R . N6 N 0.14733(11) 0.49311(14) 0.0928(2) 0.0398(6) Uani 1 d . . H6A H 0.10811(11) 0.49026(14) 0.0837(2) 0.080 Uiso 1 calc R . H6B H 0.15738(11) 0.53599(14) 0.1042(2) 0.080 Uiso 1 calc R . C310 C 0.2589(2) 0.6517(2) -0.1251(3) 0.0707(12) Uani 1 d . . H10G H 0.2382(2) 0.6206(2) -0.1664(3) 0.080 Uiso 1 d R . H10H H 0.2335(2) 0.6661(2) -0.0927(3) 0.080 Uiso 1 d R . H10I H 0.2707(2) 0.6894(2) -0.1516(3) 0.080 Uiso 1 d R . C311 C 0.3534(2) 0.5952(2) -0.1199(3) 0.0723(12) Uani 1 d . . H11G H 0.3328(2) 0.5640(2) -0.1611(3) 0.080 Uiso 1 d R . H11H H 0.3651(2) 0.6329(2) -0.1467(3) 0.080 Uiso 1 d R . H11I H 0.3876(2) 0.5743(2) -0.0843(3) 0.080 Uiso 1 d R . C312 C 0.3461(2) 0.6680(2) -0.0034(3) 0.0716(12) Uani 1 d . . H12G H 0.3206(2) 0.6824(2) 0.0288(3) 0.080 Uiso 1 d R . H12H H 0.3803(2) 0.6471(2) 0.0323(3) 0.080 Uiso 1 d R . H12I H 0.3578(2) 0.7057(2) -0.0301(3) 0.080 Uiso 1 d R . B1 B -0.03577(15) 0.2867(2) 0.0064(2) 0.0402(8) Uani 1 d . . C401 C -0.03549(13) 0.3510(2) 0.0683(2) 0.0422(7) Uani 1 d . . C402 C -0.00829(14) 0.4108(2) 0.0603(2) 0.0452(8) Uani 1 d . . H402 H 0.01232(14) 0.4137(2) 0.0207(2) 0.080 Uiso 1 calc R . C403 C -0.01025(14) 0.4673(2) 0.1090(2) 0.0493(9) Uani 1 d . . H403 H 0.00803(14) 0.5066(2) 0.1005(2) 0.080 Uiso 1 calc R . C404 C -0.0394(2) 0.4639(2) 0.1691(3) 0.0628(11) Uani 1 d . . H404 H -0.0400(2) 0.5003(2) 0.2031(3) 0.080 Uiso 1 calc R . C405 C -0.0677(2) 0.4061(2) 0.1781(3) 0.0667(11) Uani 1 d . . H405 H -0.0880(2) 0.4035(2) 0.2182(3) 0.080 Uiso 1 calc R . C406 C -0.0664(2) 0.3512(2) 0.1281(3) 0.0600(10) Uani 1 d . . H406 H -0.0870(2) 0.3132(2) 0.1348(3) 0.080 Uiso 1 calc R . C407 C 0.02649(13) 0.2866(2) -0.0202(2) 0.0377(7) Uani 1 d . . C408 C 0.07549(14) 0.2498(2) 0.0229(2) 0.0435(8) Uani 1 d . . H408 H 0.07208(14) 0.2229(2) 0.0664(2) 0.080 Uiso 1 calc R . C409 C 0.12883(15) 0.2513(2) 0.0043(2) 0.0513(9) Uani 1 d . . H409 H 0.16030(15) 0.2264(2) 0.0358(2) 0.080 Uiso 1 calc R . C410 C 0.1355(2) 0.2892(2) -0.0602(2) 0.0540(9) Uani 1 d . . H410 H 0.1712(2) 0.2900(2) -0.0732(2) 0.080 Uiso 1 calc R . C411 C 0.0885(2) 0.3259(2) -0.1051(3) 0.0572(10) Uani 1 d . . H411 H 0.0922(2) 0.3515(2) -0.1495(3) 0.080 Uiso 1 calc R . C412 C 0.0353(2) 0.3249(2) -0.0850(2) 0.0492(8) Uani 1 d . . H412 H 0.0045(2) 0.3509(2) -0.1159(2) 0.080 Uiso 1 calc R . C413 C -0.03896(13) 0.2143(2) 0.0510(2) 0.0426(7) Uani 1 d . . C414 C -0.01930(14) 0.2023(2) 0.1361(2) 0.0505(9) Uani 1 d . . H414 H -0.00849(14) 0.2386(2) 0.1716(2) 0.080 Uiso 1 calc R . C415 C -0.0151(2) 0.1391(2) 0.1706(3) 0.0614(11) Uani 1 d . . H415 H -0.0018(2) 0.1338(2) 0.2278(3) 0.080 Uiso 1 calc R . C416 C -0.0305(2) 0.0843(2) 0.1203(3) 0.0657(12) Uani 1 d . . H416 H -0.0269(2) 0.0416(2) 0.1428(3) 0.080 Uiso 1 calc R . C417 C -0.0514(2) 0.0936(2) 0.0362(3) 0.0621(10) Uani 1 d . . H417 H -0.0627(2) 0.0571(2) 0.0014(3) 0.080 Uiso 1 calc R . C418 C -0.0559(2) 0.1572(2) 0.0028(3) 0.0511(9) Uani 1 d . . H418 H -0.0708(2) 0.1621(2) -0.0543(3) 0.080 Uiso 1 calc R . C419 C -0.09297(13) 0.2952(2) -0.0752(2) 0.0412(7) Uani 1 d . . C420 C -0.0957(2) 0.2679(2) -0.1528(2) 0.0505(8) Uani 1 d . . H420 H -0.0625(2) 0.2468(2) -0.1601(2) 0.080 Uiso 1 calc R . C421 C -0.1459(2) 0.2709(2) -0.2195(3) 0.0596(10) Uani 1 d . . H421 H -0.1458(2) 0.2519(2) -0.2699(3) 0.080 Uiso 1 calc R . C422 C -0.1957(2) 0.3015(2) -0.2114(3) 0.0652(12) Uani 1 d . . H422 H -0.2295(2) 0.3030(2) -0.2558(3) 0.080 Uiso 1 calc R . C423 C -0.1950(2) 0.3300(2) -0.1369(3) 0.0626(11) Uani 1 d . . H423 H -0.2284(2) 0.3513(2) -0.1308(3) 0.080 Uiso 1 calc R . C424 C -0.14481(15) 0.3271(2) -0.0709(3) 0.0517(9) Uani 1 d . . H424 H -0.14540(15) 0.3472(2) -0.0212(3) 0.080 Uiso 1 calc R . B2 B 0.46524(15) 0.4050(2) 0.7171(2) 0.0368(7) Uani 1 d . . C501 C 0.52521(13) 0.3731(2) 0.7010(2) 0.0383(7) Uani 1 d . . C502 C 0.5273(2) 0.3421(2) 0.6274(3) 0.0514(9) Uani 1 d . . H502 H 0.4925(2) 0.3378(2) 0.5850(3) 0.080 Uiso 1 calc R . C503 C 0.5789(2) 0.3176(2) 0.6148(3) 0.0691(12) Uani 1 d . . H503 H 0.5782(2) 0.2978(2) 0.5645(3) 0.080 Uiso 1 calc R . C504 C 0.6304(2) 0.3223(2) 0.6757(3) 0.0690(12) Uani 1 d . . H504 H 0.6649(2) 0.3052(2) 0.6677(3) 0.080 Uiso 1 calc R . C505 C 0.63076(15) 0.3529(2) 0.7493(3) 0.0593(10) Uani 1 d . . H505 H 0.66570(15) 0.3562(2) 0.7915(3) 0.080 Uiso 1 calc R . C506 C 0.57928(14) 0.3788(2) 0.7608(2) 0.0456(8) Uani 1 d . . H506 H 0.58087(14) 0.4007(2) 0.8101(2) 0.080 Uiso 1 calc R . C507 C 0.40563(13) 0.3768(2) 0.6492(2) 0.0364(7) Uani 1 d . . C508 C 0.36080(13) 0.4169(2) 0.6024(2) 0.0412(7) Uani 1 d . . H508 H 0.36505(13) 0.4628(2) 0.6075(2) 0.080 Uiso 1 calc R . C509 C 0.30967(14) 0.3912(2) 0.5483(2) 0.0491(8) Uani 1 d . . H509 H 0.28095(14) 0.4200(2) 0.5178(2) 0.080 Uiso 1 calc R . C510 C 0.3016(2) 0.3237(2) 0.5396(2) 0.0528(9) Uani 1 d . . H510 H 0.2675(2) 0.3063(2) 0.5038(2) 0.080 Uiso 1 calc R . C511 C 0.3452(2) 0.2822(2) 0.5856(2) 0.0555(9) Uani 1 d . . H511 H 0.3403(2) 0.2363(2) 0.5806(2) 0.080 Uiso 1 calc R . C512 C 0.39583(15) 0.3078(2) 0.6386(2) 0.0475(8) Uani 1 d . . H512 H 0.42443(15) 0.2785(2) 0.6683(2) 0.080 Uiso 1 calc R . C513 C 0.47092(12) 0.4863(2) 0.7062(2) 0.0390(7) Uani 1 d . . C514 C 0.47712(13) 0.5112(2) 0.6306(2) 0.0450(8) Uani 1 d . . H514 H 0.47861(13) 0.4811(2) 0.5893(2) 0.080 Uiso 1 calc R . C515 C 0.48113(14) 0.5791(2) 0.6149(3) 0.0531(10) Uani 1 d . . H515 H 0.48476(14) 0.5933(2) 0.5639(3) 0.080 Uiso 1 calc R . C516 C 0.47966(15) 0.6252(2) 0.6761(3) 0.0611(11) Uani 1 d . . H516 H 0.48194(15) 0.6706(2) 0.6663(3) 0.080 Uiso 1 calc R . C517 C 0.47478(15) 0.6028(2) 0.7513(3) 0.0559(10) Uani 1 d . . H517 H 0.47424(15) 0.6332(2) 0.7928(3) 0.080 Uiso 1 calc R . C518 C 0.47064(13) 0.5353(2) 0.7659(2) 0.0460(8) Uani 1 d . . H518 H 0.46755(13) 0.5218(2) 0.8175(2) 0.080 Uiso 1 calc R . C519 C 0.45835(13) 0.3830(2) 0.8083(2) 0.0396(7) Uani 1 d . . C520 C 0.4159(2) 0.4131(2) 0.8406(2) 0.0482(8) Uani 1 d . . H520 H 0.3922(2) 0.4463(2) 0.8099(2) 0.080 Uiso 1 calc R . C521 C 0.4080(2) 0.3952(2) 0.9166(3) 0.0619(11) Uani 1 d . . H521 H 0.3799(2) 0.4170(2) 0.9361(3) 0.080 Uiso 1 calc R . C522 C 0.4412(2) 0.3459(3) 0.9629(3) 0.0682(12) Uani 1 d . . H522 H 0.4365(2) 0.3346(3) 1.0143(3) 0.080 Uiso 1 calc R . C523 C 0.4817(2) 0.3135(2) 0.9323(3) 0.0641(11) Uani 1 d . . H523 H 0.5038(2) 0.2789(2) 0.9624(3) 0.080 Uiso 1 calc R . C524 C 0.48989(15) 0.3319(2) 0.8567(2) 0.0494(8) Uani 1 d . . H524 H 0.51767(15) 0.3090(2) 0.8375(2) 0.080 Uiso 1 calc R . O O 0.1079(2) 0.4073(2) 0.4033(3) 0.1009(12) Uiso 1 d . . H1 H 0.1155(9) 0.4429(19) 0.4280(42) 0.151 Uiso 1 calc R . C1 C 0.0512(3) 0.3921(4) 0.3934(5) 0.114(2) Uiso 1 d . . H1A H 0.0451(6) 0.3457(7) 0.3804(35) 0.171 Uiso 1 calc R . H1B H 0.0270(3) 0.4182(20) 0.3490(23) 0.171 Uiso 1 calc R . H1C H 0.0410(7) 0.4016(27) 0.4437(12) 0.171 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0227(2) 0.0329(2) 0.0346(2) -0.0022(2) 0.00719(14) 0.00035(14) Ni2 0.0223(2) 0.0315(2) 0.0380(2) -0.0008(2) 0.00582(14) -0.00059(14) S1 0.0275(3) 0.0368(4) 0.0379(4) 0.0001(3) 0.0072(3) 0.0008(3) C101 0.0321(14) 0.034(2) 0.040(2) 0.0065(13) 0.0113(12) 0.0015(12) C102 0.0319(15) 0.040(2) 0.048(2) 0.0106(14) 0.0112(13) 0.0031(12) C103 0.042(2) 0.034(2) 0.061(2) 0.011(2) 0.017(2) 0.0058(13) C104 0.043(2) 0.038(2) 0.046(2) 0.0056(14) 0.0167(14) -0.0012(13) C105 0.038(2) 0.038(2) 0.041(2) 0.0031(14) 0.0135(13) -0.0044(13) C106 0.0343(15) 0.035(2) 0.040(2) 0.0037(13) 0.0123(13) -0.0014(12) C107 0.035(2) 0.040(2) 0.054(2) 0.0122(15) 0.0086(14) 0.0067(13) N1 0.0298(12) 0.0379(14) 0.048(2) -0.0010(12) 0.0135(11) 0.0021(10) C108 0.051(2) 0.033(2) 0.064(2) -0.001(2) 0.024(2) -0.0008(14) C109 0.0272(14) 0.038(2) 0.058(2) 0.0009(15) 0.0108(13) -0.0054(12) N2 0.0261(12) 0.0369(14) 0.048(2) 0.0019(12) 0.0015(11) -0.0003(10) C110 0.105(4) 0.040(2) 0.141(5) -0.002(3) 0.075(4) -0.007(2) C111 0.083(3) 0.042(2) 0.116(4) -0.004(3) 0.017(3) 0.007(2) C112 0.110(4) 0.053(3) 0.088(4) -0.014(2) 0.023(3) 0.002(3) S2 0.0257(3) 0.0329(4) 0.0369(4) -0.0025(3) 0.0081(3) -0.0001(3) C201 0.0318(14) 0.0293(15) 0.041(2) -0.0029(12) 0.0124(12) -0.0001(11) C202 0.0314(14) 0.033(2) 0.044(2) -0.0019(13) 0.0126(13) 0.0001(12) C203 0.039(2) 0.038(2) 0.037(2) -0.0068(13) 0.0094(13) -0.0029(13) C204 0.044(2) 0.032(2) 0.051(2) -0.0060(14) 0.0200(15) -0.0039(13) C205 0.038(2) 0.035(2) 0.057(2) -0.0078(15) 0.0216(15) 0.0032(13) C206 0.0336(15) 0.032(2) 0.049(2) -0.0013(13) 0.0132(13) 0.0015(12) C207 0.0276(14) 0.042(2) 0.041(2) -0.0107(14) 0.0079(12) -0.0022(12) N3 0.0256(11) 0.0434(15) 0.0383(15) -0.0058(11) 0.0057(10) 0.0032(10) C208 0.060(2) 0.049(2) 0.063(2) -0.024(2) 0.034(2) -0.012(2) C209 0.0303(15) 0.039(2) 0.056(2) -0.0072(15) 0.0136(14) 0.0071(12) N4 0.0257(11) 0.0413(14) 0.046(2) -0.0027(12) 0.0091(10) -0.0003(10) S3 0.0286(3) 0.0336(4) 0.0383(4) -0.0016(3) 0.0061(3) -0.0022(3) C301 0.0347(14) 0.035(2) 0.030(2) -0.0041(12) 0.0091(12) -0.0007(12) C302 0.0318(14) 0.040(2) 0.033(2) -0.0070(13) 0.0101(12) -0.0002(12) C303 0.036(2) 0.043(2) 0.038(2) -0.0036(14) 0.0145(13) -0.0054(13) C304 0.044(2) 0.041(2) 0.034(2) -0.0049(14) 0.0121(13) -0.0040(13) C305 0.043(2) 0.040(2) 0.033(2) 0.0003(13) 0.0069(13) 0.0052(13) C306 0.0320(14) 0.044(2) 0.034(2) -0.0046(13) 0.0058(12) 0.0004(12) C307 0.0308(14) 0.045(2) 0.038(2) -0.0017(13) 0.0130(12) 0.0020(12) N5 0.0267(11) 0.0405(14) 0.0339(14) -0.0028(11) 0.0076(10) -0.0005(10) C308 0.055(2) 0.044(2) 0.052(2) 0.004(2) 0.016(2) -0.005(2) C309 0.033(2) 0.051(2) 0.038(2) 0.0006(15) 0.0010(13) -0.0013(13) N6 0.0303(12) 0.0420(15) 0.046(2) 0.0021(12) 0.0081(11) 0.0017(11) C310 0.076(3) 0.062(3) 0.072(3) 0.027(2) 0.017(2) 0.000(2) C311 0.087(3) 0.068(3) 0.075(3) 0.011(2) 0.044(3) -0.006(2) C312 0.090(3) 0.045(2) 0.073(3) 0.006(2) 0.011(2) -0.017(2) B1 0.033(2) 0.047(2) 0.040(2) -0.004(2) 0.0093(14) -0.0025(15) C401 0.0320(15) 0.051(2) 0.041(2) -0.0031(15) 0.0058(13) 0.0016(13) C402 0.0322(15) 0.054(2) 0.046(2) 0.000(2) 0.0049(13) 0.0069(14) C403 0.033(2) 0.050(2) 0.056(2) -0.005(2) -0.0023(15) 0.0106(14) C404 0.054(2) 0.068(3) 0.058(3) -0.019(2) 0.002(2) 0.015(2) C405 0.073(3) 0.079(3) 0.054(3) -0.012(2) 0.027(2) 0.011(2) C406 0.058(2) 0.071(3) 0.059(2) -0.008(2) 0.028(2) -0.002(2) C407 0.0356(15) 0.041(2) 0.037(2) -0.0091(13) 0.0107(13) -0.0056(13) C408 0.037(2) 0.053(2) 0.040(2) -0.006(2) 0.0110(14) -0.0015(14) C409 0.040(2) 0.063(2) 0.052(2) -0.011(2) 0.015(2) 0.001(2) C410 0.041(2) 0.069(3) 0.057(2) -0.013(2) 0.021(2) -0.009(2) C411 0.057(2) 0.068(3) 0.052(2) 0.003(2) 0.025(2) -0.011(2) C412 0.044(2) 0.054(2) 0.050(2) 0.004(2) 0.016(2) -0.003(2) C413 0.0294(14) 0.052(2) 0.047(2) 0.000(2) 0.0117(13) -0.0021(13) C414 0.039(2) 0.064(2) 0.048(2) 0.006(2) 0.0108(15) -0.010(2) C415 0.048(2) 0.082(3) 0.054(2) 0.019(2) 0.014(2) -0.007(2) C416 0.056(2) 0.066(3) 0.078(3) 0.024(2) 0.024(2) 0.004(2) C417 0.062(2) 0.054(2) 0.072(3) 0.003(2) 0.021(2) -0.001(2) C418 0.047(2) 0.051(2) 0.056(2) 0.002(2) 0.016(2) 0.001(2) C419 0.036(2) 0.036(2) 0.049(2) 0.0027(14) 0.0084(14) -0.0037(13) C420 0.049(2) 0.052(2) 0.047(2) -0.002(2) 0.006(2) -0.002(2) C421 0.064(2) 0.055(2) 0.049(2) 0.003(2) -0.003(2) -0.012(2) C422 0.047(2) 0.060(3) 0.070(3) 0.012(2) -0.014(2) -0.012(2) C423 0.036(2) 0.061(3) 0.082(3) 0.005(2) 0.002(2) 0.001(2) C424 0.040(2) 0.050(2) 0.062(2) -0.002(2) 0.009(2) 0.0005(15) B2 0.034(2) 0.038(2) 0.038(2) -0.0010(15) 0.0097(14) 0.0021(14) C501 0.0348(15) 0.034(2) 0.047(2) 0.0008(13) 0.0125(13) 0.0009(12) C502 0.041(2) 0.054(2) 0.062(2) -0.013(2) 0.017(2) -0.001(2) C503 0.052(2) 0.070(3) 0.092(3) -0.028(2) 0.031(2) 0.001(2) C504 0.041(2) 0.061(3) 0.109(4) -0.009(2) 0.027(2) 0.011(2) C505 0.033(2) 0.057(2) 0.082(3) 0.013(2) 0.006(2) 0.005(2) C506 0.036(2) 0.045(2) 0.053(2) 0.006(2) 0.0088(14) -0.0020(14) C507 0.0326(14) 0.041(2) 0.038(2) -0.0012(13) 0.0141(13) -0.0028(12) C508 0.0335(15) 0.045(2) 0.045(2) -0.0001(15) 0.0117(13) -0.0029(13) C509 0.036(2) 0.061(2) 0.048(2) 0.007(2) 0.0082(14) -0.0048(15) C510 0.047(2) 0.064(2) 0.045(2) -0.003(2) 0.009(2) -0.020(2) C511 0.061(2) 0.048(2) 0.057(2) -0.003(2) 0.015(2) -0.018(2) C512 0.046(2) 0.040(2) 0.054(2) 0.005(2) 0.011(2) -0.0033(14) C513 0.0243(13) 0.041(2) 0.050(2) 0.0005(14) 0.0064(12) 0.0008(12) C514 0.0306(15) 0.045(2) 0.054(2) 0.006(2) 0.0032(14) -0.0040(13) C515 0.031(2) 0.050(2) 0.072(3) 0.016(2) 0.004(2) -0.0022(14) C516 0.037(2) 0.037(2) 0.103(4) 0.009(2) 0.007(2) -0.0013(14) C517 0.038(2) 0.042(2) 0.088(3) -0.008(2) 0.017(2) 0.0017(14) C518 0.032(2) 0.044(2) 0.061(2) -0.008(2) 0.0121(15) -0.0011(13) C519 0.0352(15) 0.041(2) 0.042(2) -0.0052(14) 0.0101(13) -0.0046(13) C520 0.047(2) 0.046(2) 0.057(2) -0.010(2) 0.022(2) -0.0075(15) C521 0.070(3) 0.066(3) 0.061(3) -0.018(2) 0.037(2) -0.017(2) C522 0.080(3) 0.086(3) 0.042(2) -0.009(2) 0.022(2) -0.029(3) C523 0.055(2) 0.079(3) 0.054(2) 0.017(2) 0.008(2) -0.008(2) C524 0.042(2) 0.059(2) 0.048(2) 0.010(2) 0.014(2) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.072(3) . ? Ni1 N3 2.120(3) . ? Ni1 N5 2.085(2) . ? Ni1 S1 2.3773(9) . ? Ni1 S2 2.3593(9) . ? Ni1 S3 2.4486(12) . ? Ni2 N2 2.027(3) . ? Ni2 N4 2.115(3) . ? Ni2 N6 2.113(3) . ? Ni2 S1 2.3632(10) . ? Ni2 S2 2.2975(9) . ? Ni2 S3 2.4370(9) . ? S1 C101 1.764(3) . ? C101 C102 1.401(4) . ? C101 C106 1.401(4) . ? C102 C103 1.390(5) . ? C102 C107 1.501(4) . ? C103 C104 1.385(5) . ? C104 C105 1.395(5) . ? C104 C108 1.530(5) . ? C105 C106 1.390(4) . ? C106 C109 1.498(4) . ? C107 N1 1.493(4) . ? C109 N2 1.493(4) . ? C108 C110 1.505(5) . ? C108 C111 1.534(6) . ? C108 C112 1.506(7) . ? S2 C201 1.757(3) . ? C201 C202 1.406(4) . ? C201 C206 1.410(4) . ? C202 C203 1.385(4) . ? C202 C207 1.506(4) . ? C203 C204 1.389(4) . ? C204 C205 1.392(5) . ? C204 C208 1.530(5) . ? C205 C206 1.388(5) . ? C206 C209 1.505(5) . ? C207 N3 1.480(4) . ? C209 N4 1.480(4) . ? C208 C210 1.494(7) . ? C208 C211 1.650(9) . ? C208 C212 1.454(9) . ? C208 C213 1.47(2) . ? C208 C214 1.370(13) . ? C208 C215 1.698(14) . ? S3 C301 1.775(3) . ? C301 C302 1.405(4) . ? C301 C306 1.397(4) . ? C302 C303 1.385(4) . ? C302 C307 1.503(4) . ? C303 C304 1.386(5) . ? C304 C305 1.392(4) . ? C304 C308 1.531(5) . ? C305 C306 1.394(5) . ? C306 C309 1.503(4) . ? C307 N5 1.481(4) . ? C309 N6 1.486(4) . ? C308 C310 1.522(6) . ? C308 C311 1.527(6) . ? C308 C312 1.537(6) . ? B1 C401 1.656(5) . ? B1 C407 1.656(4) . ? B1 C413 1.648(5) . ? B1 C419 1.646(5) . ? C401 C402 1.388(5) . ? C401 C406 1.398(5) . ? C402 C403 1.406(5) . ? C403 C404 1.375(6) . ? C404 C405 1.369(7) . ? C405 C406 1.391(6) . ? C407 C408 1.396(5) . ? C407 C412 1.396(5) . ? C408 C409 1.383(5) . ? C409 C410 1.368(6) . ? C410 C411 1.373(6) . ? C411 C412 1.391(5) . ? C413 C414 1.395(5) . ? C413 C418 1.397(5) . ? C414 C415 1.389(6) . ? C415 C416 1.374(7) . ? C416 C417 1.374(6) . ? C417 C418 1.388(6) . ? C419 C420 1.399(5) . ? C419 C424 1.405(5) . ? C420 C421 1.389(5) . ? C421 C422 1.369(6) . ? C422 C423 1.373(6) . ? C423 C424 1.383(5) . ? B2 C501 1.647(4) . ? B2 C507 1.649(5) . ? B2 C513 1.654(5) . ? B2 C519 1.645(5) . ? C501 C502 1.397(5) . ? C501 C506 1.395(5) . ? C502 C503 1.387(5) . ? C503 C504 1.359(7) . ? C504 C505 1.380(6) . ? C505 C506 1.387(5) . ? C507 C508 1.389(5) . ? C507 C512 1.409(5) . ? C508 C509 1.395(5) . ? C509 C510 1.372(5) . ? C510 C511 1.384(6) . ? C511 C512 1.378(5) . ? C513 C514 1.410(5) . ? C513 C518 1.406(5) . ? C514 C515 1.396(5) . ? C515 C516 1.391(6) . ? C516 C517 1.376(6) . ? C517 C518 1.386(5) . ? C519 C520 1.405(5) . ? C519 C524 1.392(5) . ? C520 C521 1.388(6) . ? C521 C522 1.364(7) . ? C522 C523 1.372(6) . ? C523 C524 1.387(5) . ? O C1 1.341(7) . ? 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 N1 Ni1 N3 92.46(11) . . ? N1 Ni1 N5 91.35(10) . . ? N3 Ni1 N5 88.60(10) . . ? N1 Ni1 S2 172.34(7) . . ? N3 Ni1 S2 92.66(7) . . ? N5 Ni1 S2 94.47(7) . . ? N1 Ni1 S1 93.40(7) . . ? N5 Ni1 S1 174.99(7) . . ? N3 Ni1 S1 92.77(7) . . ? S2 Ni1 S1 80.66(3) . . ? N1 Ni1 S3 93.83(8) . . ? N5 Ni1 S3 92.56(7) . . ? N3 Ni1 S3 173.57(7) . . ? S2 Ni1 S3 80.95(3) . . ? S1 Ni1 S3 85.54(3) . . ? N2 Ni2 N6 91.21(11) . . ? N2 Ni2 N4 90.53(10) . . ? N6 Ni2 N4 89.40(11) . . ? N2 Ni2 S2 174.14(8) . . ? N6 Ni2 S2 93.45(8) . . ? N4 Ni2 S2 93.08(7) . . ? N2 Ni2 S1 92.97(8) . . ? N6 Ni2 S1 175.29(7) . . ? N4 Ni2 S1 92.74(8) . . ? S2 Ni2 S1 82.25(4) . . ? N2 Ni2 S3 93.90(8) . . ? N6 Ni2 S3 91.44(8) . . ? N4 Ni2 S3 175.48(7) . . ? S2 Ni2 S3 82.44(3) . . ? S1 Ni2 S3 86.11(3) . . ? Ni1 S1 Ni2 80.53(3) . . ? C101 S1 Ni1 103.38(10) . . ? C101 S1 Ni2 103.30(11) . . ? C102 C101 S1 120.9(2) . . ? C106 C101 S1 119.9(2) . . ? C102 C101 C106 119.2(3) . . ? C101 C102 C103 119.5(3) . . ? C101 C102 C107 121.6(3) . . ? C103 C102 C107 119.0(3) . . ? C102 C103 C104 122.3(3) . . ? C103 C104 C105 117.4(3) . . ? C103 C104 C108 122.6(3) . . ? C105 C104 C108 120.0(3) . . ? C106 C105 C104 121.9(3) . . ? C101 C106 C105 119.7(3) . . ? C101 C106 C109 120.9(3) . . ? C105 C106 C109 119.4(3) . . ? N1 C107 C102 110.6(3) . . ? N2 C109 C106 109.9(2) . . ? C107 N1 Ni1 116.1(2) . . ? C109 N2 Ni2 116.6(2) . . ? C104 C108 C110 110.8(3) . . ? C104 C108 C111 111.8(3) . . ? C104 C108 C112 108.6(3) . . ? C110 C108 C111 107.2(4) . . ? C110 C108 C112 110.0(4) . . ? C111 C108 C112 108.3(4) . . ? C201 S2 Ni1 105.32(10) . . ? C201 S2 Ni2 106.27(10) . . ? Ni1 S2 Ni2 82.28(3) . . ? C202 C201 S2 120.2(2) . . ? C206 C201 S2 120.0(2) . . ? C202 C201 C206 119.6(3) . . ? C201 C202 C203 119.0(3) . . ? C201 C202 C207 122.3(3) . . ? C203 C202 C207 118.6(3) . . ? C202 C203 C204 122.6(3) . . ? C203 C204 C205 117.4(3) . . ? C203 C204 C208 120.9(3) . . ? C205 C204 C208 121.6(3) . . ? C204 C205 C206 122.3(3) . . ? C201 C206 C205 119.0(3) . . ? C201 C206 C209 121.3(3) . . ? C205 C206 C209 119.7(3) . . ? N3 C207 C202 111.6(2) . . ? N4 C209 C206 112.0(3) . . ? C207 N3 Ni1 115.3(2) . . ? C209 N4 Ni2 115.2(2) . . ? C204 C208 C210 115.8(4) . . ? C204 C208 C211 108.9(4) . . ? C204 C208 C212 109.8(4) . . ? C204 C208 C213 108.4(7) . . ? C204 C208 C214 115.6(6) . . ? C204 C208 C215 101.8(6) . . ? C210 C208 C211 103.5(4) . . ? C210 C208 C212 113.7(5) . . ? C211 C208 C212 104.1(5) . . ? C213 C208 C214 122.2(9) . . ? C213 C208 C215 101.2(9) . . ? C214 C208 C215 104.4(8) . . ? C301 S3 Ni1 101.32(10) . . ? C301 S3 Ni2 102.28(10) . . ? Ni2 S3 Ni1 77.68(3) . . ? C302 C301 S3 120.3(2) . . ? C306 C301 S3 120.8(2) . . ? C302 C301 C306 118.9(3) . . ? C301 C302 C303 119.5(3) . . ? C301 C302 C307 121.5(3) . . ? C303 C302 C307 119.0(3) . . ? C302 C303 C304 122.9(3) . . ? C303 C304 C305 116.5(3) . . ? C303 C304 C308 119.7(3) . . ? C305 C304 C308 123.7(3) . . ? C304 C305 C306 122.6(3) . . ? C301 C306 C305 119.5(3) . . ? C301 C306 C309 120.9(3) . . ? C305 C306 C309 119.6(3) . . ? N5 C307 C302 110.1(2) . . ? N6 C309 C306 111.2(3) . . ? C307 N5 Ni1 116.2(2) . . ? C309 N6 Ni2 117.3(2) . . ? C304 C308 C311 112.0(3) . . ? C304 C308 C312 110.5(3) . . ? C304 C308 C313 107.3(3) . . ? C310 C308 C311 109.4(4) . . ? C310 C308 C312 109.0(4) . . ? C311 C308 C312 108.5(4) . . ? C401 B1 C407 108.8(3) . . ? C401 B1 C413 113.3(3) . . ? C401 B1 C419 107.5(3) . . ? C407 B1 C413 106.2(3) . . ? C407 B1 C419 111.3(3) . . ? C413 B1 C419 109.8(3) . . ? C402 C401 B1 122.4(3) . . ? C406 C401 B1 122.9(3) . . ? C402 C401 C406 114.6(3) . . ? C401 C402 C403 123.5(3) . . ? C402 C403 C404 119.4(4) . . ? C403 C404 C405 119.0(4) . . ? C404 C405 C406 120.7(4) . . ? C401 C406 C405 122.8(4) . . ? C408 C407 C412 114.4(3) . . ? C408 C407 B1 122.3(3) . . ? C412 C407 B1 123.2(3) . . ? C409 C408 C407 123.4(3) . . ? C408 C409 C410 120.3(4) . . ? C409 C410 C411 118.7(3) . . ? C410 C411 C412 120.6(4) . . ? C407 C412 C411 122.6(4) . . ? C414 C413 C418 114.4(3) . . ? C414 C413 B1 124.9(3) . . ? C418 C413 B1 120.2(3) . . ? C413 C414 C415 123.3(4) . . ? C414 C415 C416 120.1(4) . . ? C415 C416 C417 118.7(4) . . ? C416 C417 C418 120.5(4) . . ? C413 C418 C417 122.9(4) . . ? C420 C419 C424 114.4(3) . . ? C420 C419 B1 123.4(3) . . ? C424 C419 B1 122.1(3) . . ? C419 C420 C421 122.7(4) . . ? C420 C421 C422 120.5(4) . . ? C421 C422 C423 119.0(4) . . ? C422 C423 C424 120.2(4) . . ? C419 C424 C423 123.1(4) . . ? C501 B2 C507 111.3(3) . . ? C501 B2 C513 105.4(2) . . ? C501 B2 C519 111.2(3) . . ? C507 B2 C513 110.1(3) . . ? C507 B2 C519 105.3(2) . . ? C513 B2 C519 113.6(3) . . ? C502 C501 B2 124.2(3) . . ? C506 C501 B2 120.7(3) . . ? C502 C501 C506 115.0(3) . . ? C501 C502 C503 122.8(4) . . ? C502 C503 C504 120.3(4) . . ? C503 C504 C505 119.1(3) . . ? C504 C505 C506 120.4(4) . . ? C501 C506 C505 122.3(4) . . ? C508 C507 B2 124.3(3) . . ? C512 C507 B2 120.3(3) . . ? C508 C507 C512 115.2(3) . . ? C507 C508 C509 122.8(3) . . ? C508 C509 C510 120.3(3) . . ? C509 C510 C511 118.5(3) . . ? C510 C511 C512 121.0(4) . . ? C507 C512 C511 122.1(3) . . ? C514 C513 B2 118.8(3) . . ? C518 C513 B2 126.6(3) . . ? C514 C513 C518 114.6(3) . . ? C513 C514 C515 123.1(4) . . ? C514 C515 C516 119.6(4) . . ? C515 C516 C517 119.0(4) . . ? C516 C517 C518 120.7(4) . . ? C513 C518 C517 123.0(4) . . ? C520 C519 B2 120.8(3) . . ? C524 C519 B2 124.5(3) . . ? C520 C519 C524 114.6(3) . . ? C519 C520 C521 122.5(4) . . ? C520 C521 C522 120.6(4) . . ? C521 C522 C523 118.9(4) . . ? C522 C523 C524 120.4(4) . . ? C519 C524 C523 122.9(4) . . ? _refine_diff_density_max 0.604 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.061