# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _audit_creation_method 'manual editing of form.cif' _publ_contact_author_name 'Berthold Kersting' _publ_contact_author_address ; Institut fuer Anorganische Chemie Universitat Leipzig, Johannisallee 29 04103 Leipzig Germany3 ; _publ_contact_author_email b.kersting@uni-leipzig.de _publ_contact_author_phone '+49/(0)341/973 6143' _publ_contact_author_fax '+49/(0)341/973 6199' _publ_contact_letter ; Please consider this CIF submission for publication in Chem. Commun. Manuscript No. _____________ ; # TITLE AND AUTHORLIST _publ_section_title ; Stabilisation of a paramagnetic dinickel borohydride complex by a macrodinucleating hexaaza-dithiophenolate ligand macrocycles ; loop_ _publ_author_name 'Berthold Kersting' 'Julia Hausmann' 'Yves Journaux' 'Vasile Lozan' data_3 _database_code_depnum_ccdc_archive 'CCDC 280004' _chemical_formula_structural ; [(L)Ni2(u1,3-BH4)]BPh4(MeCN)2 ; _chemical_formula_sum 'C66 H94 B2 N8 Ni2 S2' _chemical_formula_weight 1202.65 _chemical_melting_point ? _chemical_compound_source ; Crystals were grown by recrystallization from acetonitrile ; #CRYSTAL DATA _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 15.992(3) _cell_length_b 16.080(3) _cell_length_c 16.515(3) _cell_angle_alpha 63.82(3) _cell_angle_beta 70.97(3) _cell_angle_gamma 66.47(3) _cell_volume 3435.8(12) _cell_formula_units_Z 2 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pale-green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.162 _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 0.651 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'BRUKER AXS' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31047 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0947 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 28.86 #REFINEMENT DATA _reflns_number_total 16023 _reflns_number_gt 8515 _reflns_threshold_expression >2sigma(I) _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^)+(0.1412P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method 'riding model' _refine_ls_extinction_coef ? _refine_ls_number_reflns 16021 _refine_ls_number_parameters 724 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.1345 _refine_ls_R_factor_gt 0.0749 _refine_ls_wR_factor_ref 0.2442 _refine_ls_wR_factor_gt 0.2053 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.862 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.113 _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (FARRUGIA)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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' 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' 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 0.21526(4) 1.29510(4) -0.23737(4) 0.03446(17) Uani 1 1 d . . . Ni2 Ni 0.37664(4) 1.39107(4) -0.24274(4) 0.03248(17) Uani 1 1 d . . . S1 S 0.36483(8) 1.22778(8) -0.18916(8) 0.0376(3) Uani 1 1 d . . . S2 S 0.20823(8) 1.42298(8) -0.18972(8) 0.0372(3) Uani 1 1 d . . . B1 B 0.3260(4) 1.4034(4) -0.4028(4) 0.0405(13) Uani 1 1 d D . . H1 H 0.263(3) 1.364(3) -0.363(3) 0.049 Uiso 1 1 d D . . H2 H 0.365(3) 1.420(4) -0.360(3) 0.049 Uiso 1 1 d D . . H3 H 0.381(3) 1.353(3) -0.437(3) 0.049 Uiso 1 1 d D . . H4 H 0.288(3) 1.478(3) -0.446(3) 0.049 Uiso 1 1 d D . . N1 N 0.2459(3) 1.1697(3) -0.2774(3) 0.0430(10) Uani 1 1 d . . . N2 N 0.1391(3) 1.2130(3) -0.1151(3) 0.0540(12) Uani 1 1 d . . . N3 N 0.0691(3) 1.3770(3) -0.2697(4) 0.0513(12) Uani 1 1 d . . . N4 N 0.3614(3) 1.5505(3) -0.2847(3) 0.0391(9) Uani 1 1 d . . . N5 N 0.4140(3) 1.3813(3) -0.1253(3) 0.0456(10) Uani 1 1 d . . . N6 N 0.5323(3) 1.3335(3) -0.2819(3) 0.0473(11) Uani 1 1 d . . . C1 C 0.4448(3) 1.1762(3) -0.2700(3) 0.0335(10) Uani 1 1 d . . . C2 C 0.4213(3) 1.1205(3) -0.2994(3) 0.0382(11) Uani 1 1 d . . . C3 C 0.4850(3) 1.0811(4) -0.3640(4) 0.0425(12) Uani 1 1 d . . . H3B H 0.4677 1.0463 -0.3849 0.051 Uiso 1 1 calc R . . C4 C 0.5733(3) 1.0921(4) -0.3983(3) 0.0401(11) Uani 1 1 d . . . C5 C 0.5964(3) 1.1448(4) -0.3651(4) 0.0427(12) Uani 1 1 d . . . H5 H 0.6551 1.1530 -0.3862 0.051 Uiso 1 1 calc R . . C6 C 0.5338(3) 1.1855(3) -0.3011(3) 0.0361(10) Uani 1 1 d . . . C7 C 0.3345(3) 1.0914(3) -0.2532(4) 0.0451(12) Uani 1 1 d . . . H7A H 0.3304 1.0681 -0.1874 0.054 Uiso 1 1 calc R . . H7B H 0.3397 1.0375 -0.2684 0.054 Uiso 1 1 calc R . . C8 C 0.2505(4) 1.1940(5) -0.3763(4) 0.0666(17) Uani 1 1 d . . . H8A H 0.2542 1.1378 -0.3857 0.100 Uiso 1 1 calc R . . H8B H 0.3044 1.2146 -0.4115 0.100 Uiso 1 1 calc R . . H8C H 0.1959 1.2455 -0.3957 0.100 Uiso 1 1 calc R . . C9 C 0.1705(4) 1.1249(4) -0.2199(4) 0.0541(15) Uani 1 1 d . . . H9A H 0.1880 1.0600 -0.2205 0.065 Uiso 1 1 calc R . . H9B H 0.1143 1.1632 -0.2455 0.065 Uiso 1 1 calc R . . C10 C 0.1521(4) 1.1196(4) -0.1218(4) 0.0559(15) Uani 1 1 d . . . H10A H 0.0969 1.0994 -0.0883 0.067 Uiso 1 1 calc R . . H10B H 0.2037 1.0705 -0.0926 0.067 Uiso 1 1 calc R . . C11 C 0.1729(6) 1.1892(6) -0.0305(4) 0.095(3) Uani 1 1 d . . . H11A H 0.1573 1.2477 -0.0190 0.142 Uiso 1 1 calc R . . H11B H 0.2390 1.1602 -0.0392 0.142 Uiso 1 1 calc R . . H11C H 0.1440 1.1445 0.0209 0.142 Uiso 1 1 calc R . . C12 C 0.0421(5) 1.2711(4) -0.1071(6) 0.089(3) Uani 1 1 d . . . H12A H 0.0338 1.3219 -0.0860 0.107 Uiso 1 1 calc R . . H12B H 0.0045 1.2302 -0.0618 0.107 Uiso 1 1 calc R . . C13 C 0.0099(4) 1.3161(5) -0.1969(7) 0.087(3) Uani 1 1 d . . . H13A H -0.0542 1.3564 -0.1899 0.104 Uiso 1 1 calc R . . H13B H 0.0129 1.2654 -0.2155 0.104 Uiso 1 1 calc R . . C14 C 0.0590(5) 1.3972(5) -0.3600(6) 0.085(2) Uani 1 1 d . . . H14A H 0.0723 1.3373 -0.3679 0.127 Uiso 1 1 calc R . . H14B H 0.1014 1.4316 -0.4045 0.127 Uiso 1 1 calc R . . H14C H -0.0034 1.4363 -0.3682 0.127 Uiso 1 1 calc R . . C15 C 0.0298(3) 1.4709(3) -0.2536(4) 0.0477(13) Uani 1 1 d . . . H15A H 0.0241 1.4565 -0.1888 0.057 Uiso 1 1 calc R . . H15B H -0.0322 1.5019 -0.2678 0.057 Uiso 1 1 calc R . . C16 C 0.0843(3) 1.5418(3) -0.3074(3) 0.0372(10) Uani 1 1 d . . . C17 C 0.1615(3) 1.5313(3) -0.2773(3) 0.0352(10) Uani 1 1 d . . . C18 C 0.1969(3) 1.6088(3) -0.3141(3) 0.0361(10) Uani 1 1 d . . . C19 C 0.1622(4) 1.6914(4) -0.3878(4) 0.0476(13) Uani 1 1 d . . . H19 H 0.1877 1.7422 -0.4127 0.057 Uiso 1 1 calc R . . C20 C 0.0912(4) 1.7000(4) -0.4252(4) 0.0527(14) Uani 1 1 d . A . C21 C 0.0510(3) 1.6251(4) -0.3805(4) 0.0460(12) Uani 1 1 d . . . H21 H 0.0000 1.6306 -0.4000 0.055 Uiso 1 1 calc R . . C22 C 0.2631(3) 1.6100(3) -0.2678(4) 0.0396(11) Uani 1 1 d . . . H22A H 0.2618 1.6768 -0.2871 0.047 Uiso 1 1 calc R . . H22B H 0.2401 1.5879 -0.2021 0.047 Uiso 1 1 calc R . . C23 C 0.3999(4) 1.5995(4) -0.3797(4) 0.0622(16) Uani 1 1 d . . . H23A H 0.3839 1.6676 -0.3917 0.093 Uiso 1 1 calc R . . H23B H 0.3750 1.5909 -0.4201 0.093 Uiso 1 1 calc R . . H23C H 0.4662 1.5722 -0.3900 0.093 Uiso 1 1 calc R . . C24 C 0.4071(4) 1.5538(4) -0.2208(4) 0.0575(16) Uani 1 1 d . . . H24A H 0.4733 1.5403 -0.2440 0.069 Uiso 1 1 calc R . . H24B H 0.3832 1.6184 -0.2182 0.069 Uiso 1 1 calc R . . C25 C 0.3901(4) 1.4816(4) -0.1270(4) 0.0498(14) Uani 1 1 d . . . H25A H 0.4264 1.4805 -0.0893 0.060 Uiso 1 1 calc R . . H25B H 0.3251 1.5022 -0.1000 0.060 Uiso 1 1 calc R . . C26 C 0.3645(7) 1.3260(6) -0.0377(4) 0.100(3) Uani 1 1 d . . . H26A H 0.3800 1.2606 -0.0343 0.149 Uiso 1 1 calc R . . H26B H 0.2988 1.3563 -0.0345 0.149 Uiso 1 1 calc R . . H26C H 0.3826 1.3253 0.0127 0.149 Uiso 1 1 calc R . . C27 C 0.5143(5) 1.3345(6) -0.1293(5) 0.092(3) Uani 1 1 d . . . H27A H 0.5356 1.3557 -0.0952 0.111 Uiso 1 1 calc R . . H27B H 0.5258 1.2647 -0.0995 0.111 Uiso 1 1 calc R . . C28 C 0.5684(4) 1.3555(6) -0.2229(7) 0.102(3) Uani 1 1 d . . . H28A H 0.6328 1.3168 -0.2209 0.123 Uiso 1 1 calc R . . H28B H 0.5657 1.4235 -0.2497 0.123 Uiso 1 1 calc R . . C29 C 0.5707(5) 1.3763(5) -0.3808(5) 0.079(2) Uani 1 1 d . . . H29A H 0.5416 1.4453 -0.4026 0.118 Uiso 1 1 calc R . . H29B H 0.5589 1.3482 -0.4150 0.118 Uiso 1 1 calc R . . H29C H 0.6363 1.3630 -0.3887 0.118 Uiso 1 1 calc R . . C30 C 0.5667(3) 1.2263(4) -0.2552(4) 0.0445(12) Uani 1 1 d . . . H30A H 0.5480 1.1975 -0.1893 0.053 Uiso 1 1 calc R . . H30B H 0.6339 1.2066 -0.2687 0.053 Uiso 1 1 calc R . . C31 C 0.6427(4) 1.0457(4) -0.4674(4) 0.0495(13) Uani 1 1 d . . . C32 C 0.6584(6) 0.9348(5) -0.4263(5) 0.091(3) Uani 1 1 d . . . H32A H 0.6790 0.9079 -0.3689 0.136 Uiso 1 1 calc R . . H32B H 0.7047 0.9054 -0.4680 0.136 Uiso 1 1 calc R . . H32C H 0.6014 0.9222 -0.4163 0.136 Uiso 1 1 calc R . . C33 C 0.7353(5) 1.0623(6) -0.4932(6) 0.090(3) Uani 1 1 d . . . H33A H 0.7270 1.1307 -0.5157 0.134 Uiso 1 1 calc R . . H33B H 0.7739 1.0364 -0.5400 0.134 Uiso 1 1 calc R . . H33C H 0.7643 1.0303 -0.4402 0.134 Uiso 1 1 calc R . . C34 C 0.6001(6) 1.0896(6) -0.5558(5) 0.091(2) Uani 1 1 d . . . H34A H 0.5428 1.0753 -0.5403 0.136 Uiso 1 1 calc R . . H34B H 0.6428 1.0617 -0.6001 0.136 Uiso 1 1 calc R . . H34C H 0.5887 1.1588 -0.5811 0.136 Uiso 1 1 calc R . . C35 C 0.0557(5) 1.7893(5) -0.5062(5) 0.085(2) Uani 1 1 d . . . C36 C 0.1268(7) 1.8321(7) -0.5709(6) 0.140(5) Uani 1 1 d . A 1 H36A H 0.1011 1.8847 -0.6223 0.210 Uiso 1 1 calc R A 1 H36B H 0.1767 1.7839 -0.5918 0.210 Uiso 1 1 calc R A 1 H36C H 0.1499 1.8563 -0.5414 0.210 Uiso 1 1 calc R A 1 C37 C 0.0002(13) 1.7768(10) -0.5473(11) 0.298(13) Uani 1 1 d . A 1 H37A H -0.0313 1.8389 -0.5874 0.447 Uiso 1 1 calc R A 1 H37B H -0.0446 1.7472 -0.5008 0.447 Uiso 1 1 calc R A 1 H37C H 0.0383 1.7358 -0.5821 0.447 Uiso 1 1 calc R A 1 C38 C -0.0075(13) 1.8701(10) -0.4679(9) 0.338(16) Uani 1 1 d . A 1 H38A H 0.0294 1.8909 -0.4494 0.506 Uiso 1 1 calc R A 1 H38B H -0.0518 1.8456 -0.4160 0.506 Uiso 1 1 calc R A 1 H38C H -0.0396 1.9241 -0.5145 0.506 Uiso 1 1 calc R A 1 B2 B 0.7442(4) 1.2370(4) 0.0404(4) 0.0398(12) Uani 1 1 d . B 1 C101 C 0.6386(3) 1.2599(3) 0.1015(4) 0.0395(11) Uani 1 1 d . B 1 C102 C 0.5680(3) 1.3484(3) 0.0726(3) 0.0367(10) Uani 1 1 d . B 1 H102 H 0.5833 1.3983 0.0197 0.044 Uiso 1 1 calc R B 1 C103 C 0.4771(3) 1.3645(4) 0.1195(4) 0.0468(12) Uani 1 1 d . B 1 H103 H 0.4330 1.4241 0.0981 0.056 Uiso 1 1 calc R B 1 C104 C 0.4522(4) 1.2913(5) 0.1985(4) 0.0647(17) Uani 1 1 d . B 1 H104 H 0.3911 1.3008 0.2297 0.078 Uiso 1 1 calc R B 1 C105 C 0.5175(4) 1.2063(5) 0.2294(5) 0.078(2) Uani 1 1 d . B 1 H105 H 0.5016 1.1580 0.2836 0.094 Uiso 1 1 calc R B 1 C106 C 0.6091(4) 1.1895(4) 0.1814(5) 0.0647(17) Uani 1 1 d . B 1 H106 H 0.6519 1.1291 0.2037 0.078 Uiso 1 1 calc R B 1 C201 C 0.8211(3) 1.1602(3) 0.1061(3) 0.0394(11) Uani 1 1 d . B 1 C202 C 0.9031(3) 1.0976(3) 0.0757(3) 0.0379(11) Uani 1 1 d . B 1 H202 H 0.9112 1.0950 0.0184 0.046 Uiso 1 1 calc R B 1 C203 C 0.8130(4) 1.1585(4) 0.1947(4) 0.0553(14) Uani 1 1 d . B 1 H203 H 0.7589 1.1967 0.2198 0.066 Uiso 1 1 calc R B 1 C204 C 0.9733(4) 1.0391(4) 0.1266(4) 0.0474(13) Uani 1 1 d . B 1 H204 H 1.0265 0.9981 0.1036 0.057 Uiso 1 1 calc R B 1 C205 C 0.9639(4) 1.0419(5) 0.2116(4) 0.0622(16) Uani 1 1 d . B 1 H205 H 1.0114 1.0040 0.2453 0.075 Uiso 1 1 calc R B 1 C206 C 0.8850(5) 1.1001(5) 0.2459(4) 0.0675(17) Uani 1 1 d . B 1 H206 H 0.8783 1.1015 0.3034 0.081 Uiso 1 1 calc R B 1 C301 C 0.7711(4) 1.3394(4) -0.0156(4) 0.0522(14) Uani 1 1 d . B 1 C302 C 0.8214(4) 1.3680(4) 0.0170(5) 0.0668(18) Uani 1 1 d . B 1 H302 H 0.8428 1.3264 0.0717 0.080 Uiso 1 1 calc R B 1 C303 C 0.8409(6) 1.4570(6) -0.0292(7) 0.100(3) Uani 1 1 d . B 1 H303 H 0.8751 1.4734 -0.0056 0.120 Uiso 1 1 calc R B 1 C304 C 0.8093(6) 1.5199(6) -0.1095(8) 0.110(4) Uani 1 1 d . B 1 H304 H 0.8216 1.5792 -0.1402 0.133 Uiso 1 1 calc R B 1 C305 C 0.7605(5) 1.4956(6) -0.1438(6) 0.100(3) Uani 1 1 d . B 1 H305 H 0.7394 1.5384 -0.1984 0.120 Uiso 1 1 calc R B 1 C306 C 0.7414(4) 1.4079(5) -0.0989(5) 0.075(2) Uani 1 1 d . B 1 H306 H 0.7076 1.3932 -0.1245 0.090 Uiso 1 1 calc R B 1 C401 C 0.7456(4) 1.1886(4) -0.0294(4) 0.0566(15) Uani 1 1 d . B 1 C402 C 0.8076(5) 1.1989(6) -0.1151(5) 0.082(2) Uani 1 1 d . B 1 H402 H 0.8438 1.2398 -0.1351 0.098 Uiso 1 1 calc R B 1 C403 C 0.8157(7) 1.1498(8) -0.1698(7) 0.125(5) Uani 1 1 d . B 1 H403 H 0.8589 1.1569 -0.2242 0.150 Uiso 1 1 calc R B 1 C404 C 0.7645(10) 1.0936(8) -0.1474(10) 0.144(6) Uani 1 1 d . B 1 H404 H 0.7709 1.0620 -0.1855 0.173 Uiso 1 1 calc R B 1 C405 C 0.7013(8) 1.0822(6) -0.0666(9) 0.120(4) Uani 1 1 d . B 1 H405 H 0.6641 1.0433 -0.0510 0.144 Uiso 1 1 calc R B 1 C406 C 0.6913(5) 1.1287(4) -0.0063(6) 0.077(2) Uani 1 1 d . B 1 H406 H 0.6487 1.1192 0.0484 0.092 Uiso 1 1 calc R B 1 N7A N 0.4990(12) 1.0277(13) 0.0266(11) 0.132(3) Uani 0.50 1 d PDU . 1 C39A C 0.4577(12) 1.0551(15) 0.0841(13) 0.132(3) Uani 0.50 1 d PDU C 1 C40A C 0.3910(13) 1.0872(15) 0.1590(12) 0.132(3) Uani 0.50 1 d PDU C 1 H40A H 0.3288 1.1025 0.1515 0.198 Uiso 0.50 1 calc PR C 1 H40B H 0.3999 1.1437 0.1569 0.198 Uiso 0.50 1 calc PR C 1 H40C H 0.4010 1.0360 0.2171 0.198 Uiso 0.50 1 calc PR C 1 N7B N 0.0115 1.3796 0.1008 0.132(3) Uani 0.50 1 d PDU D 1 C39B C 0.0333(10) 1.3039(6) 0.1525(10) 0.132(3) Uani 0.50 1 d PDU D 1 C40B C 0.0844(14) 1.2081(6) 0.2129(11) 0.132(3) Uani 0.50 1 d PDU D 1 H40D H 0.0824 1.1574 0.1983 0.198 Uiso 0.50 1 calc PR D 1 H40E H 0.0561 1.1994 0.2758 0.198 Uiso 0.50 1 calc PR D 1 H40F H 0.1478 1.2055 0.2034 0.198 Uiso 0.50 1 calc PR D 1 N8A N -0.1694(17) 1.631(2) -0.4236(13) 0.178(6) Uani 0.50 1 d PDU E 1 C41A C -0.2075(16) 1.5760(18) -0.3976(18) 0.178(6) Uani 0.50 1 d PDU E 1 C42A C -0.2661(17) 1.5124(19) -0.3683(13) 0.178(6) Uani 0.50 1 d PDU E 1 H42A H -0.2285 1.4518 -0.3764 0.267 Uiso 0.50 1 calc PR E 1 H42B H -0.3137 1.5437 -0.4048 0.267 Uiso 0.50 1 calc PR E 1 H42C H -0.2941 1.5003 -0.3048 0.267 Uiso 0.50 1 calc PR E 1 N8B N -0.1829(14) 1.640(2) -0.3979(13) 0.178(6) Uani 0.50 1 d PDU F 2 C41B C -0.2505(13) 1.634(2) -0.3978(19) 0.178(6) Uani 0.50 1 d PDU F 2 C42B C -0.3441(13) 1.634(2) -0.3951(13) 0.178(6) Uani 0.50 1 d PDU F 2 H42D H -0.3847 1.6438 -0.3404 0.267 Uiso 0.50 1 calc PR F 2 H42E H -0.3404 1.5730 -0.3950 0.267 Uiso 0.50 1 calc PR F 2 H42F H -0.3679 1.6856 -0.4480 0.267 Uiso 0.50 1 calc PR F 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 0.0330(3) 0.0287(3) 0.0381(3) -0.0128(3) 0.0019(3) -0.0115(2) Ni2 0.0346(3) 0.0329(3) 0.0338(3) -0.0163(3) -0.0091(2) -0.0068(2) S1 0.0406(6) 0.0328(6) 0.0362(6) -0.0167(5) -0.0045(5) -0.0050(5) S2 0.0380(6) 0.0288(6) 0.0376(6) -0.0117(5) -0.0016(5) -0.0073(5) B1 0.043(3) 0.046(3) 0.040(3) -0.019(3) -0.004(2) -0.020(3) N1 0.039(2) 0.039(2) 0.051(3) -0.022(2) -0.0014(19) -0.0111(18) N2 0.059(3) 0.037(2) 0.053(3) -0.017(2) 0.018(2) -0.024(2) N3 0.035(2) 0.041(2) 0.081(3) -0.023(2) -0.013(2) -0.0117(19) N4 0.041(2) 0.038(2) 0.039(2) -0.0123(18) -0.0104(18) -0.0118(18) N5 0.065(3) 0.038(2) 0.039(2) -0.0152(19) -0.024(2) -0.007(2) N6 0.034(2) 0.051(3) 0.071(3) -0.040(2) -0.010(2) -0.0053(19) C1 0.034(2) 0.029(2) 0.036(2) -0.0172(19) -0.0036(19) -0.0038(18) C2 0.038(3) 0.027(2) 0.048(3) -0.017(2) -0.002(2) -0.010(2) C3 0.039(3) 0.043(3) 0.056(3) -0.032(2) 0.003(2) -0.016(2) C4 0.041(3) 0.041(3) 0.042(3) -0.026(2) 0.005(2) -0.014(2) C5 0.035(3) 0.046(3) 0.055(3) -0.028(2) -0.002(2) -0.015(2) C6 0.036(2) 0.034(2) 0.042(3) -0.021(2) -0.009(2) -0.004(2) C7 0.048(3) 0.034(3) 0.052(3) -0.022(2) 0.001(2) -0.013(2) C8 0.061(4) 0.077(4) 0.062(4) -0.042(4) -0.009(3) -0.005(3) C9 0.041(3) 0.053(3) 0.079(4) -0.038(3) 0.005(3) -0.020(3) C10 0.048(3) 0.031(3) 0.069(4) -0.014(3) 0.014(3) -0.018(2) C11 0.153(8) 0.103(6) 0.037(4) -0.025(4) 0.026(4) -0.082(6) C12 0.061(4) 0.038(3) 0.112(6) -0.019(4) 0.045(4) -0.017(3) C13 0.031(3) 0.055(4) 0.169(9) -0.043(5) 0.002(4) -0.018(3) C14 0.087(5) 0.073(5) 0.127(7) -0.059(5) -0.063(5) 0.006(4) C15 0.032(3) 0.034(3) 0.074(4) -0.019(3) -0.006(2) -0.010(2) C16 0.030(2) 0.033(2) 0.045(3) -0.017(2) -0.002(2) -0.0072(19) C17 0.033(2) 0.030(2) 0.040(3) -0.016(2) -0.004(2) -0.0055(19) C18 0.033(2) 0.032(2) 0.047(3) -0.016(2) -0.009(2) -0.0089(19) C19 0.045(3) 0.031(2) 0.061(3) -0.004(2) -0.017(3) -0.015(2) C20 0.051(3) 0.038(3) 0.065(4) -0.003(3) -0.025(3) -0.016(2) C21 0.037(3) 0.043(3) 0.058(3) -0.012(2) -0.016(2) -0.015(2) C22 0.042(3) 0.032(2) 0.050(3) -0.017(2) -0.012(2) -0.011(2) C23 0.056(4) 0.056(4) 0.052(3) -0.006(3) -0.005(3) -0.014(3) C24 0.054(3) 0.043(3) 0.088(5) -0.018(3) -0.035(3) -0.015(3) C25 0.071(4) 0.040(3) 0.047(3) -0.022(2) -0.028(3) -0.004(3) C26 0.198(10) 0.094(6) 0.036(3) -0.009(3) -0.028(5) -0.081(6) C27 0.080(5) 0.109(6) 0.110(6) -0.086(5) -0.069(5) 0.044(4) C28 0.042(4) 0.135(7) 0.202(10) -0.139(8) -0.033(5) 0.000(4) C29 0.063(4) 0.057(4) 0.098(5) -0.037(4) 0.031(4) -0.026(3) C30 0.036(3) 0.051(3) 0.056(3) -0.032(3) -0.018(2) -0.001(2) C31 0.050(3) 0.058(3) 0.052(3) -0.037(3) 0.011(3) -0.024(3) C32 0.107(6) 0.056(4) 0.089(5) -0.046(4) 0.030(5) -0.021(4) C33 0.062(4) 0.127(7) 0.108(6) -0.086(6) 0.032(4) -0.045(4) C34 0.094(6) 0.118(7) 0.075(5) -0.059(5) 0.004(4) -0.034(5) C35 0.062(4) 0.070(5) 0.091(5) 0.022(4) -0.039(4) -0.028(4) C36 0.140(8) 0.160(9) 0.088(6) 0.069(6) -0.074(6) -0.099(7) C37 0.45(2) 0.237(15) 0.267(17) 0.194(13) -0.314(19) -0.283(18) C38 0.37(2) 0.194(14) 0.111(10) -0.013(10) -0.055(13) 0.206(16) B2 0.039(3) 0.034(3) 0.041(3) -0.016(2) -0.006(2) -0.005(2) C101 0.036(3) 0.032(2) 0.050(3) -0.016(2) -0.009(2) -0.007(2) C102 0.036(3) 0.036(2) 0.039(3) -0.015(2) -0.007(2) -0.011(2) C103 0.032(3) 0.048(3) 0.055(3) -0.024(3) -0.004(2) -0.004(2) C104 0.042(3) 0.076(4) 0.060(4) -0.021(3) 0.004(3) -0.016(3) C105 0.047(4) 0.063(4) 0.072(4) 0.015(3) 0.001(3) -0.020(3) C106 0.052(3) 0.040(3) 0.076(4) -0.005(3) -0.006(3) -0.010(3) C201 0.038(3) 0.034(2) 0.048(3) -0.018(2) -0.008(2) -0.008(2) C202 0.036(3) 0.033(2) 0.044(3) -0.015(2) -0.007(2) -0.009(2) C203 0.050(3) 0.061(4) 0.055(3) -0.029(3) -0.013(3) -0.005(3) C204 0.039(3) 0.043(3) 0.052(3) -0.011(2) -0.016(2) -0.004(2) C205 0.055(4) 0.064(4) 0.059(4) -0.014(3) -0.024(3) -0.008(3) C206 0.075(4) 0.077(4) 0.050(4) -0.022(3) -0.023(3) -0.014(4) C301 0.033(3) 0.040(3) 0.061(4) -0.018(3) 0.004(2) 0.000(2) C302 0.064(4) 0.048(3) 0.085(5) -0.038(3) 0.013(3) -0.019(3) C303 0.088(6) 0.065(5) 0.136(8) -0.054(5) 0.041(6) -0.039(4) C304 0.080(6) 0.049(4) 0.128(8) -0.023(5) 0.056(6) -0.017(4) C305 0.053(4) 0.064(5) 0.094(6) 0.008(4) 0.016(4) 0.004(4) C306 0.046(3) 0.064(4) 0.066(4) 0.003(3) 0.003(3) -0.007(3) C401 0.042(3) 0.051(3) 0.072(4) -0.032(3) -0.031(3) 0.018(3) C402 0.053(4) 0.118(6) 0.076(5) -0.065(5) -0.027(3) 0.019(4) C403 0.101(7) 0.160(10) 0.115(7) -0.107(8) -0.075(6) 0.069(7) C404 0.164(12) 0.124(9) 0.185(12) -0.121(9) -0.141(11) 0.078(8) C405 0.148(9) 0.064(5) 0.188(11) -0.064(7) -0.127(9) 0.027(5) C406 0.088(5) 0.041(3) 0.113(6) -0.034(4) -0.060(5) 0.009(3) N7A 0.186(9) 0.118(7) 0.128(8) -0.050(5) -0.055(6) -0.055(7) C39A 0.186(9) 0.118(7) 0.128(8) -0.050(5) -0.055(6) -0.055(7) C40A 0.186(9) 0.118(7) 0.128(8) -0.050(5) -0.055(6) -0.055(7) N7B 0.186(9) 0.118(7) 0.128(8) -0.050(5) -0.055(6) -0.055(7) C39B 0.186(9) 0.118(7) 0.128(8) -0.050(5) -0.055(6) -0.055(7) C40B 0.186(9) 0.118(7) 0.128(8) -0.050(5) -0.055(6) -0.055(7) N8A 0.181(10) 0.325(14) 0.064(5) -0.019(8) -0.021(6) -0.169(10) C41A 0.181(10) 0.325(14) 0.064(5) -0.019(8) -0.021(6) -0.169(10) C42A 0.181(10) 0.325(14) 0.064(5) -0.019(8) -0.021(6) -0.169(10) N8B 0.181(10) 0.325(14) 0.064(5) -0.019(8) -0.021(6) -0.169(10) C41B 0.181(10) 0.325(14) 0.064(5) -0.019(8) -0.021(6) -0.169(10) C42B 0.181(10) 0.325(14) 0.064(5) -0.019(8) -0.021(6) -0.169(10) _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 N2 2.152(4) . ? Ni1 N1 2.219(4) . ? Ni1 N3 2.284(4) . ? Ni1 S1 2.4374(16) . ? Ni1 S2 2.4588(14) . ? Ni1 H1 1.93(4) . ? Ni2 N5 2.135(4) . ? Ni2 N6 2.260(4) . ? Ni2 N4 2.271(4) . ? Ni2 S1 2.4393(15) . ? Ni2 S2 2.4574(15) . ? Ni2 H2 1.84(4) . ? S1 C1 1.767(4) . ? S2 C17 1.769(5) . ? B1 H1 1.25(4) . ? B1 H2 1.24(4) . ? B1 H3 1.12(4) . ? B1 H4 1.12(4) . ? N1 C8 1.486(7) . ? N1 C9 1.489(7) . ? N1 C7 1.501(6) . ? N2 C12 1.454(8) . ? N2 C10 1.481(6) . ? N2 C11 1.499(9) . ? N3 C14 1.429(8) . ? N3 C15 1.494(6) . ? N3 C13 1.504(8) . ? N4 C23 1.460(7) . ? N4 C22 1.488(6) . ? N4 C24 1.493(7) . ? N5 C27 1.467(8) . ? N5 C26 1.481(8) . ? N5 C25 1.490(6) . ? N6 C29 1.487(8) . ? N6 C30 1.483(6) . ? N6 C28 1.496(7) . ? C1 C6 1.392(6) . ? C1 C2 1.397(6) . ? C2 C3 1.397(6) . ? C2 C7 1.496(7) . ? C3 C4 1.392(7) . ? C3 H3B 0.9300 . ? C4 C5 1.396(7) . ? C4 C31 1.534(6) . ? C5 C6 1.395(6) . ? C5 H5 0.9300 . ? C6 C30 1.503(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.520(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.497(11) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.498(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.398(7) . ? C16 C21 1.400(7) . ? C17 C18 1.383(6) . ? C18 C19 1.407(7) . ? C18 C22 1.505(6) . ? C19 C20 1.394(7) . ? C19 H19 0.9300 . ? C20 C21 1.390(7) . ? C20 C35 1.524(8) . ? C21 H21 0.9300 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.488(8) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.468(12) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C33 1.500(8) . ? C31 C32 1.545(8) . ? C31 C34 1.564(9) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C37 1.394(12) . ? C35 C36 1.447(10) . ? C35 C38 1.540(15) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? B2 C201 1.640(8) . ? B2 C401 1.643(8) . ? B2 C301 1.647(8) . ? B2 C101 1.651(7) . ? C101 C106 1.395(8) . ? C101 C102 1.413(6) . ? C102 C103 1.387(7) . ? C102 H102 0.9300 . ? C103 C104 1.389(8) . ? C103 H103 0.9300 . ? C104 C105 1.346(8) . ? C104 H104 0.9300 . ? C105 C106 1.400(8) . ? C105 H105 0.9300 . ? C106 H106 0.9300 . ? C201 C202 1.395(6) . ? C201 C203 1.416(7) . ? C202 C204 1.388(7) . ? C202 H202 0.9300 . ? C203 C206 1.411(8) . ? C203 H203 0.9300 . ? C204 C205 1.382(8) . ? C204 H204 0.9300 . ? C205 C206 1.360(9) . ? C205 H205 0.9300 . ? C206 H206 0.9300 . ? C301 C302 1.395(9) . ? C301 C306 1.415(8) . ? C302 C303 1.402(9) . ? C302 H302 0.9300 . ? C303 C304 1.372(14) . ? C303 H303 0.9300 . ? C304 C305 1.345(13) . ? C304 H304 0.9300 . ? C305 C306 1.380(11) . ? C305 H305 0.9300 . ? C306 H306 0.9300 . ? C401 C406 1.397(9) . ? C401 C402 1.423(9) . ? C402 C403 1.389(11) . ? C402 H402 0.9300 . ? C403 C404 1.312(17) . ? C403 H403 0.9300 . ? C404 C405 1.374(17) . ? C404 H404 0.9300 . ? C405 C406 1.427(11) . ? C405 H405 0.9300 . ? C406 H406 0.9300 . ? N7A C39A 1.1232(19) . ? N7A N7A 1.49(3) 2_675 ? C39A C40A 1.481(2) . ? C40A H40A 0.9600 . ? C40A H40B 0.9600 . ? C40A H40C 0.9600 . ? N7B C39B 1.127(2) . ? C39B C40B 1.485(2) . ? C40B H40D 0.9600 . ? C40B H40E 0.9600 . ? C40B H40F 0.9600 . ? N8A C41A 1.1212(19) . ? C41A C42A 1.4812(19) . ? C42A H42A 0.9600 . ? C42A H42B 0.9600 . ? C42A H42C 0.9600 . ? N8B C41B 1.1209(19) . ? C41B C42B 1.4810(19) . ? C42B H42D 0.9600 . ? C42B H42E 0.9600 . ? C42B H42F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N1 82.44(16) . . ? N2 Ni1 N3 80.89(19) . . ? N1 Ni1 N3 99.06(16) . . ? N2 Ni1 S1 98.56(15) . . ? N1 Ni1 S1 90.97(12) . . ? N3 Ni1 S1 169.77(12) . . ? N2 Ni1 S2 100.26(13) . . ? N1 Ni1 S2 170.53(12) . . ? N3 Ni1 S2 90.35(12) . . ? S1 Ni1 S2 79.67(5) . . ? N2 Ni1 H1 164.4(13) . . ? N1 Ni1 H1 88.1(14) . . ? N3 Ni1 H1 88.4(14) . . ? S1 Ni1 H1 93.9(13) . . ? S2 Ni1 H1 91.1(14) . . ? N5 Ni2 N6 81.62(17) . . ? N5 Ni2 N4 81.80(15) . . ? N6 Ni2 N4 99.55(15) . . ? N5 Ni2 S1 99.46(12) . . ? N6 Ni2 S1 90.07(12) . . ? N4 Ni2 S1 170.38(11) . . ? N5 Ni2 S2 99.38(13) . . ? N6 Ni2 S2 169.72(12) . . ? N4 Ni2 S2 90.72(11) . . ? S1 Ni2 S2 79.66(6) . . ? N5 Ni2 H2 164.7(14) . . ? N6 Ni2 H2 89.9(15) . . ? N4 Ni2 H2 87.1(14) . . ? S1 Ni2 H2 93.2(14) . . ? S2 Ni2 H2 91.2(15) . . ? C1 S1 Ni1 105.96(16) . . ? C1 S1 Ni2 105.49(16) . . ? Ni1 S1 Ni2 90.33(5) . . ? C17 S2 Ni2 103.53(16) . . ? C17 S2 Ni1 103.14(16) . . ? Ni2 S2 Ni1 89.41(5) . . ? H1 B1 H2 122(3) . . ? H1 B1 H3 104(3) . . ? H2 B1 H3 107(3) . . ? H1 B1 H4 103(3) . . ? H2 B1 H4 103(3) . . ? H3 B1 H4 120(4) . . ? C8 N1 C9 110.8(5) . . ? C8 N1 C7 106.3(4) . . ? C9 N1 C7 105.5(4) . . ? C8 N1 Ni1 115.2(3) . . ? C9 N1 Ni1 104.8(3) . . ? C7 N1 Ni1 113.9(3) . . ? C12 N2 C10 111.8(5) . . ? C12 N2 C11 108.8(6) . . ? C10 N2 C11 107.1(5) . . ? C12 N2 Ni1 108.1(4) . . ? C10 N2 Ni1 109.0(3) . . ? C11 N2 Ni1 112.2(4) . . ? C14 N3 C15 107.7(5) . . ? C14 N3 C13 112.0(6) . . ? C15 N3 C13 103.7(5) . . ? C14 N3 Ni1 116.1(4) . . ? C15 N3 Ni1 112.0(3) . . ? C13 N3 Ni1 104.7(4) . . ? C23 N4 C22 106.5(4) . . ? C23 N4 C24 110.2(4) . . ? C22 N4 C24 105.2(4) . . ? C23 N4 Ni2 116.5(3) . . ? C22 N4 Ni2 112.5(3) . . ? C24 N4 Ni2 105.4(3) . . ? C27 N5 C26 109.0(6) . . ? C27 N5 C25 109.4(5) . . ? C26 N5 C25 107.9(5) . . ? C27 N5 Ni2 109.2(3) . . ? C26 N5 Ni2 112.9(4) . . ? C25 N5 Ni2 108.5(3) . . ? C29 N6 C30 107.6(4) . . ? C29 N6 C28 111.7(6) . . ? C30 N6 C28 105.6(5) . . ? C29 N6 Ni2 115.0(4) . . ? C30 N6 Ni2 113.1(3) . . ? C28 N6 Ni2 103.5(3) . . ? C6 C1 C2 119.0(4) . . ? C6 C1 S1 120.6(3) . . ? C2 C1 S1 120.3(4) . . ? C1 C2 C3 119.5(4) . . ? C1 C2 C7 120.6(4) . . ? C3 C2 C7 119.4(4) . . ? C4 C3 C2 122.4(4) . . ? C4 C3 H3B 118.8 . . ? C2 C3 H3B 118.8 . . ? C3 C4 C5 116.9(4) . . ? C3 C4 C31 121.3(4) . . ? C5 C4 C31 121.8(4) . . ? C6 C5 C4 121.8(4) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C1 C6 C5 120.2(4) . . ? C1 C6 C30 119.4(4) . . ? C5 C6 C30 119.7(4) . . ? C2 C7 N1 115.8(4) . . ? C2 C7 H7A 108.3 . . ? N1 C7 H7A 108.3 . . ? C2 C7 H7B 108.3 . . ? N1 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C10 110.7(4) . . ? N1 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? N2 C10 C9 113.3(4) . . ? N2 C10 H10A 108.9 . . ? C9 C10 H10A 108.9 . . ? N2 C10 H10B 108.9 . . ? C9 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? N2 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C13 111.5(6) . . ? N2 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? N2 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? C12 C13 N3 110.7(5) . . ? C12 C13 H13A 109.5 . . ? N3 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? N3 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? N3 C14 H14A 109.5 . . ? N3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 C16 115.9(4) . . ? N3 C15 H15A 108.3 . . ? C16 C15 H15A 108.3 . . ? N3 C15 H15B 108.3 . . ? C16 C15 H15B 108.3 . . ? H15A C15 H15B 107.4 . . ? C17 C16 C21 119.9(4) . . ? C17 C16 C15 119.9(4) . . ? C21 C16 C15 119.7(4) . . ? C18 C17 C16 118.7(4) . . ? C18 C17 S2 121.1(4) . . ? C16 C17 S2 120.1(4) . . ? C17 C18 C19 119.6(4) . . ? C17 C18 C22 119.9(4) . . ? C19 C18 C22 120.0(4) . . ? C20 C19 C18 122.7(5) . . ? C20 C19 H19 118.7 . . ? C18 C19 H19 118.7 . . ? C21 C20 C19 115.9(5) . . ? C21 C20 C35 122.0(5) . . ? C19 C20 C35 121.9(5) . . ? C20 C21 C16 122.5(5) . . ? C20 C21 H21 118.7 . . ? C16 C21 H21 118.7 . . ? N4 C22 C18 116.9(4) . . ? N4 C22 H22A 108.1 . . ? C18 C22 H22A 108.1 . . ? N4 C22 H22B 108.1 . . ? C18 C22 H22B 108.1 . . ? H22A C22 H22B 107.3 . . ? N4 C23 H23A 109.5 . . ? N4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 N4 111.1(4) . . ? C25 C24 H24A 109.4 . . ? N4 C24 H24A 109.4 . . ? C25 C24 H24B 109.4 . . ? N4 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? N5 C25 C24 113.5(4) . . ? N5 C25 H25A 108.9 . . ? C24 C25 H25A 108.9 . . ? N5 C25 H25B 108.9 . . ? C24 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? N5 C26 H26A 109.5 . . ? N5 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N5 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 N5 113.8(5) . . ? C28 C27 H27A 108.8 . . ? N5 C27 H27A 108.8 . . ? C28 C27 H27B 108.8 . . ? N5 C27 H27B 108.8 . . ? H27A C27 H27B 107.7 . . ? C27 C28 N6 111.3(6) . . ? C27 C28 H28A 109.4 . . ? N6 C28 H28A 109.4 . . ? C27 C28 H28B 109.4 . . ? N6 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? N6 C29 H29A 109.5 . . ? N6 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N6 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N6 C30 C6 115.6(4) . . ? N6 C30 H30A 108.4 . . ? C6 C30 H30A 108.4 . . ? N6 C30 H30B 108.4 . . ? C6 C30 H30B 108.4 . . ? H30A C30 H30B 107.4 . . ? C33 C31 C4 113.3(5) . . ? C33 C31 C32 107.9(6) . . ? C4 C31 C32 109.6(5) . . ? C33 C31 C34 109.1(6) . . ? C4 C31 C34 108.1(5) . . ? C32 C31 C34 108.7(5) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C37 C35 C36 113.8(10) . . ? C37 C35 C20 114.0(7) . . ? C36 C35 C20 113.7(6) . . ? C37 C35 C38 105.5(12) . . ? C36 C35 C38 101.7(11) . . ? C20 C35 C38 106.7(7) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C201 B2 C401 108.4(4) . . ? C201 B2 C301 108.1(4) . . ? C401 B2 C301 112.0(5) . . ? C201 B2 C101 111.4(4) . . ? C401 B2 C101 108.3(4) . . ? C301 B2 C101 108.6(4) . . ? C106 C101 C102 114.4(5) . . ? C106 C101 B2 122.4(4) . . ? C102 C101 B2 122.9(4) . . ? C103 C102 C101 123.0(5) . . ? C103 C102 H102 118.5 . . ? C101 C102 H102 118.5 . . ? C102 C103 C104 119.8(5) . . ? C102 C103 H103 120.1 . . ? C104 C103 H103 120.1 . . ? C105 C104 C103 119.2(5) . . ? C105 C104 H104 120.4 . . ? C103 C104 H104 120.4 . . ? C104 C105 C106 121.1(6) . . ? C104 C105 H105 119.4 . . ? C106 C105 H105 119.4 . . ? C101 C106 C105 122.5(5) . . ? C101 C106 H106 118.7 . . ? C105 C106 H106 118.7 . . ? C202 C201 C203 115.0(5) . . ? C202 C201 B2 122.4(4) . . ? C203 C201 B2 122.4(4) . . ? C204 C202 C201 123.4(5) . . ? C204 C202 H202 118.3 . . ? C201 C202 H202 118.3 . . ? C206 C203 C201 121.6(5) . . ? C206 C203 H203 119.2 . . ? C201 C203 H203 119.2 . . ? C205 C204 C202 119.7(5) . . ? C205 C204 H204 120.1 . . ? C202 C204 H204 120.1 . . ? C206 C205 C204 119.8(6) . . ? C206 C205 H205 120.1 . . ? C204 C205 H205 120.1 . . ? C205 C206 C203 120.4(6) . . ? C205 C206 H206 119.8 . . ? C203 C206 H206 119.8 . . ? C302 C301 C306 114.2(6) . . ? C302 C301 B2 122.9(5) . . ? C306 C301 B2 122.8(6) . . ? C301 C302 C303 122.6(8) . . ? C301 C302 H302 118.7 . . ? C303 C302 H302 118.7 . . ? C304 C303 C302 119.6(9) . . ? C304 C303 H303 120.2 . . ? C302 C303 H303 120.2 . . ? C305 C304 C303 120.0(8) . . ? C305 C304 H304 120.0 . . ? C303 C304 H304 120.0 . . ? C304 C305 C306 120.7(9) . . ? C304 C305 H305 119.7 . . ? C306 C305 H305 119.7 . . ? C305 C306 C301 122.8(8) . . ? C305 C306 H306 118.6 . . ? C301 C306 H306 118.6 . . ? C406 C401 C402 115.2(6) . . ? C406 C401 B2 122.7(6) . . ? C402 C401 B2 122.0(6) . . ? C403 C402 C401 122.0(9) . . ? C403 C402 H402 119.0 . . ? C401 C402 H402 119.0 . . ? C404 C403 C402 122.2(11) . . ? C404 C403 H403 118.9 . . ? C402 C403 H403 118.9 . . ? C403 C404 C405 119.0(9) . . ? C403 C404 H404 120.5 . . ? C405 C404 H404 120.5 . . ? C404 C405 C406 121.5(10) . . ? C404 C405 H405 119.3 . . ? C406 C405 H405 119.3 . . ? C401 C406 C405 120.1(9) . . ? C401 C406 H406 120.0 . . ? C405 C406 H406 120.0 . . ? C39A N7A N7A 144(2) . 2_675 ? N7A C39A C40A 170.8(15) . . ? C39A C40A H40A 109.5 . . ? C39A C40A H40B 109.5 . . ? H40A C40A H40B 109.5 . . ? C39A C40A H40C 109.5 . . ? H40A C40A H40C 109.5 . . ? H40B C40A H40C 109.5 . . ? N7B C39B C40B 166.1(11) . . ? C39B C40B H40D 109.5 . . ? C39B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? C39B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? N8A C41A C42A 174(2) . . ? C41A C42A H42A 109.5 . . ? C41A C42A H42B 109.5 . . ? H42A C42A H42B 109.5 . . ? C41A C42A H42C 109.5 . . ? H42A C42A H42C 109.5 . . ? H42B C42A H42C 109.5 . . ? N8B C41B C42B 175(3) . . ? C41B C42B H42D 109.5 . . ? C41B C42B H42E 109.5 . . ? H42D C42B H42E 109.5 . . ? C41B C42B H42F 109.5 . . ? H42D C42B H42F 109.5 . . ? H42E C42B H42F 109.5 . . ? #===END #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 280005' _chemical_formula_structural ; [(L)Ni2(u-O2CH)]BPh4 ; _chemical_formula_sum 'C63 H85 B N6 Ni2 O2 S2' _chemical_formula_weight 1150.72 _chemical_melting_point ? _chemical_compound_source ; Crystals were grown by recrystallization from acetonitrile ; #CRYSTAL DATA _symmetry_cell_setting monoclinic _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 18.452(4) _cell_length_b 34.531(7) _cell_length_c 18.452(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.22(3) _cell_angle_gamma 90.00 _cell_volume 11748(4) _cell_formula_units_Z 8 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pale-green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_F_000 4912 _exptl_absorpt_coefficient_mu 0.761 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? #EXPERIMENTAL DATA _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'BRUKER AXS' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74914 _diffrn_reflns_av_R_equivalents 0.1561 _diffrn_reflns_av_sigmaI/netI 0.2740 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 28.34 #REFINEMENT DATA _reflns_number_total 28479 _reflns_number_gt 8710 _reflns_threshold_expression >2sigma(I) _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^)+(0.0818P)^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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 28479 _refine_ls_number_parameters 1369 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2361 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.2216 _refine_ls_wR_factor_gt 0.1651 _refine_ls_goodness_of_fit_ref 0.809 _refine_ls_restrained_S_all 0.809 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.897 _refine_diff_density_min -1.382 _refine_diff_density_rms 0.104 _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (FARRUGIA)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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' 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 Ni1A Ni 0.20005(4) 0.14121(2) 0.72151(5) 0.0343(2) Uani 1 1 d . . . Ni2A Ni 0.37472(5) 0.14715(2) 0.79905(5) 0.0338(2) Uani 1 1 d . . . S1A S 0.32194(9) 0.12193(5) 0.68289(9) 0.0377(4) Uani 1 1 d . . . S2A S 0.25720(9) 0.12208(5) 0.84107(9) 0.0376(4) Uani 1 1 d . . . O1A O 0.2251(2) 0.19698(12) 0.7338(2) 0.0400(12) Uani 1 1 d . . . O2A O 0.3380(2) 0.20115(12) 0.7854(2) 0.0383(12) Uani 1 1 d . . . N1A N 0.1640(3) 0.15555(17) 0.6058(3) 0.0454(16) Uani 1 1 d . . . N2A N 0.1491(3) 0.08685(16) 0.6954(3) 0.0461(15) Uani 1 1 d . . . N3A N 0.0940(3) 0.15384(16) 0.7736(3) 0.0382(14) Uani 1 1 d . . . N4A N 0.4085(3) 0.16373(18) 0.9174(3) 0.0465(15) Uani 1 1 d . . . N5A N 0.4384(3) 0.09730(17) 0.8269(4) 0.0514(17) Uani 1 1 d . . . N6A N 0.4761(3) 0.16567(15) 0.7453(3) 0.0357(13) Uani 1 1 d . . . C1A C 0.3441(4) 0.15855(17) 0.6224(3) 0.0338(16) Uani 1 1 d . . . C2A C 0.2915(4) 0.1726(2) 0.5702(4) 0.0380(17) Uani 1 1 d . . . C3A C 0.3063(4) 0.2060(2) 0.5327(4) 0.0418(18) Uani 1 1 d . . . H3A H 0.2709 0.2155 0.5000 0.050 Uiso 1 1 calc R . . C4A C 0.3713(4) 0.22660(19) 0.5411(4) 0.0387(17) Uani 1 1 d . . . C5A C 0.4253(4) 0.20893(18) 0.5856(3) 0.0374(17) Uani 1 1 d . . . H5A H 0.4709 0.2204 0.5897 0.045 Uiso 1 1 calc R . . C6A C 0.4134(4) 0.17512(18) 0.6238(4) 0.0353(16) Uani 1 1 d . . . C7A C 0.2240(3) 0.1491(2) 0.5549(4) 0.0413(18) Uani 1 1 d . . . H7A1 H 0.2059 0.1549 0.5060 0.050 Uiso 1 1 calc R . . H7A2 H 0.2370 0.1219 0.5562 0.050 Uiso 1 1 calc R . . C8A C 0.1355(4) 0.1950(2) 0.5899(4) 0.064(2) Uani 1 1 d . . . H8A1 H 0.1201 0.1966 0.5396 0.095 Uiso 1 1 calc R . . H8A2 H 0.1729 0.2138 0.6001 0.095 Uiso 1 1 calc R . . H8A3 H 0.0950 0.2001 0.6196 0.095 Uiso 1 1 calc R . . C9A C 0.1071(4) 0.1266(3) 0.5883(4) 0.064(2) Uani 1 1 d . . . H9A1 H 0.0995 0.1251 0.5361 0.077 Uiso 1 1 calc R . . H9A2 H 0.0620 0.1349 0.6087 0.077 Uiso 1 1 calc R . . C10A C 0.1261(5) 0.0875(2) 0.6168(4) 0.066(3) Uani 1 1 d . . . H10A H 0.1650 0.0770 0.5889 0.079 Uiso 1 1 calc R . . H10B H 0.0844 0.0707 0.6094 0.079 Uiso 1 1 calc R . . C11A C 0.1924(5) 0.0526(2) 0.7109(6) 0.083(3) Uani 1 1 d . . . H11A H 0.2084 0.0527 0.7610 0.124 Uiso 1 1 calc R . . H11B H 0.2337 0.0525 0.6809 0.124 Uiso 1 1 calc R . . H11C H 0.1636 0.0299 0.7010 0.124 Uiso 1 1 calc R . . C12A C 0.0837(4) 0.0841(2) 0.7407(4) 0.059(2) Uani 1 1 d . . . H12A H 0.0988 0.0752 0.7888 0.071 Uiso 1 1 calc R . . H12B H 0.0509 0.0649 0.7195 0.071 Uiso 1 1 calc R . . C13A C 0.0432(4) 0.1218(2) 0.7478(4) 0.056(2) Uani 1 1 d . . . H13A H 0.0051 0.1187 0.7820 0.067 Uiso 1 1 calc R . . H13B H 0.0208 0.1288 0.7012 0.067 Uiso 1 1 calc R . . C14A C 0.0606(4) 0.1911(2) 0.7588(4) 0.059(2) Uani 1 1 d . . . H14A H 0.0218 0.1950 0.7912 0.089 Uiso 1 1 calc R . . H14B H 0.0417 0.1916 0.7096 0.089 Uiso 1 1 calc R . . H14C H 0.0961 0.2112 0.7658 0.089 Uiso 1 1 calc R . . C15A C 0.1006(4) 0.14964(19) 0.8539(4) 0.0401(17) Uani 1 1 d . . . H15A H 0.1112 0.1228 0.8656 0.048 Uiso 1 1 calc R . . H15B H 0.0543 0.1559 0.8741 0.048 Uiso 1 1 calc R . . C16A C 0.1584(4) 0.17488(18) 0.8896(3) 0.0338(16) Uani 1 1 d . . . C17A C 0.2299(3) 0.16084(18) 0.8952(3) 0.0296(14) Uani 1 1 d . . . C18A C 0.2779(4) 0.17897(19) 0.9444(3) 0.0386(17) Uani 1 1 d . . . C19A C 0.2584(4) 0.2140(2) 0.9761(4) 0.0439(19) Uani 1 1 d . . . H19A H 0.2915 0.2260 1.0081 0.053 Uiso 1 1 calc R . . C20A C 0.1917(4) 0.23188(18) 0.9621(4) 0.0384(17) Uani 1 1 d . . . C21A C 0.1418(3) 0.20946(18) 0.9224(3) 0.0351(16) Uani 1 1 d . . . H21A H 0.0943 0.2183 0.9177 0.042 Uiso 1 1 calc R . . C22A C 0.3464(4) 0.1579(2) 0.9658(4) 0.051(2) Uani 1 1 d . . . H22A H 0.3615 0.1659 1.0145 0.061 Uiso 1 1 calc R . . H22B H 0.3357 0.1304 0.9676 0.061 Uiso 1 1 calc R . . C23A C 0.4358(4) 0.2034(2) 0.9287(4) 0.063(2) Uani 1 1 d . . . H23A H 0.4016 0.2215 0.9076 0.095 Uiso 1 1 calc R . . H23B H 0.4815 0.2061 0.9060 0.095 Uiso 1 1 calc R . . H23C H 0.4421 0.2084 0.9797 0.095 Uiso 1 1 calc R . . C24A C 0.4645(4) 0.1350(3) 0.9400(4) 0.064(2) Uani 1 1 d . . . H24A H 0.4667 0.1327 0.9925 0.076 Uiso 1 1 calc R . . H24B H 0.5116 0.1436 0.9248 0.076 Uiso 1 1 calc R . . C25A C 0.4473(5) 0.0965(3) 0.9072(5) 0.074(3) Uani 1 1 d . . . H25A H 0.4859 0.0785 0.9208 0.088 Uiso 1 1 calc R . . H25B H 0.4029 0.0869 0.9271 0.088 Uiso 1 1 calc R . . C26A C 0.4046(4) 0.0612(2) 0.8029(5) 0.071(3) Uani 1 1 d . . . H26A H 0.4412 0.0418 0.7978 0.106 Uiso 1 1 calc R . . H26B H 0.3793 0.0652 0.7570 0.106 Uiso 1 1 calc R . . H26C H 0.3709 0.0528 0.8380 0.106 Uiso 1 1 calc R . . C27A C 0.5102(4) 0.1009(2) 0.7915(4) 0.050(2) Uani 1 1 d . . . H27A H 0.5466 0.0870 0.8205 0.060 Uiso 1 1 calc R . . H27B H 0.5064 0.0886 0.7443 0.060 Uiso 1 1 calc R . . C28A C 0.5356(4) 0.1416(2) 0.7818(4) 0.049(2) Uani 1 1 d . . . H28A H 0.5781 0.1418 0.7524 0.059 Uiso 1 1 calc R . . H28B H 0.5491 0.1527 0.8287 0.059 Uiso 1 1 calc R . . C29A C 0.4968(4) 0.20680(19) 0.7521(4) 0.050(2) Uani 1 1 d . . . H29A H 0.5386 0.2116 0.7241 0.076 Uiso 1 1 calc R . . H29B H 0.5079 0.2128 0.8021 0.076 Uiso 1 1 calc R . . H29C H 0.4573 0.2227 0.7344 0.076 Uiso 1 1 calc R . . C30A C 0.4730(4) 0.15605(19) 0.6670(4) 0.0395(17) Uani 1 1 d . . . H30A H 0.4678 0.1282 0.6619 0.047 Uiso 1 1 calc R . . H30B H 0.5188 0.1633 0.6468 0.047 Uiso 1 1 calc R . . C31A C 0.3801(4) 0.2668(2) 0.5075(4) 0.046(2) Uani 1 1 d . . . C32A C 0.4501(6) 0.2869(3) 0.5334(7) 0.132(5) Uani 1 1 d . . . H32A H 0.4906 0.2702 0.5254 0.198 Uiso 1 1 calc R . . H32B H 0.4480 0.2925 0.5842 0.198 Uiso 1 1 calc R . . H32C H 0.4556 0.3106 0.5069 0.198 Uiso 1 1 calc R . . C33A C 0.3211(6) 0.2928(3) 0.5371(7) 0.121(5) Uani 1 1 d . . . H33A H 0.3110 0.3136 0.5037 0.181 Uiso 1 1 calc R . . H33B H 0.3375 0.3032 0.5831 0.181 Uiso 1 1 calc R . . H33C H 0.2778 0.2779 0.5431 0.181 Uiso 1 1 calc R . . C34A C 0.3688(9) 0.2660(3) 0.4292(5) 0.177(8) Uani 1 1 d . . . H34A H 0.3193 0.2724 0.4167 0.266 Uiso 1 1 calc R . . H34B H 0.3794 0.2405 0.4115 0.266 Uiso 1 1 calc R . . H34C H 0.4004 0.2844 0.4077 0.266 Uiso 1 1 calc R . . C35A C 0.1764(4) 0.2721(2) 0.9900(4) 0.0468(19) Uani 1 1 d . . . C36A C 0.2413(4) 0.2984(2) 0.9799(4) 0.057(2) Uani 1 1 d . . . H36A H 0.2831 0.2877 1.0054 0.085 Uiso 1 1 calc R . . H36B H 0.2313 0.3236 0.9988 0.085 Uiso 1 1 calc R . . H36C H 0.2507 0.3003 0.9292 0.085 Uiso 1 1 calc R . . C37A C 0.1599(5) 0.2699(2) 1.0703(4) 0.067(3) Uani 1 1 d . . . H37A H 0.1150 0.2563 1.0758 0.100 Uiso 1 1 calc R . . H37B H 0.1558 0.2956 1.0895 0.100 Uiso 1 1 calc R . . H37C H 0.1983 0.2564 1.0960 0.100 Uiso 1 1 calc R . . C38A C 0.1109(5) 0.2906(2) 0.9506(5) 0.075(3) Uani 1 1 d . . . H38A H 0.1178 0.2904 0.8993 0.113 Uiso 1 1 calc R . . H38B H 0.1057 0.3169 0.9668 0.113 Uiso 1 1 calc R . . H38C H 0.0680 0.2762 0.9609 0.113 Uiso 1 1 calc R . . C39A C 0.2806(4) 0.21482(19) 0.7597(4) 0.0399(18) Uani 1 1 d . . . H39A H 0.2776 0.2417 0.7593 0.048 Uiso 1 1 calc R . . Ni1B Ni 0.17513(5) 0.10889(2) 0.22492(5) 0.0372(2) Uani 1 1 d . . . Ni2B Ni 0.34989(5) 0.09469(2) 0.29762(5) 0.0348(2) Uani 1 1 d . . . S1B S 0.23692(10) 0.12184(5) 0.34550(9) 0.0385(4) Uani 1 1 d . . . S2B S 0.29745(10) 0.12591(5) 0.18597(10) 0.0406(4) Uani 1 1 d . . . O1B O 0.1944(2) 0.05190(11) 0.2269(2) 0.0389(12) Uani 1 1 d . . . O2B O 0.3068(2) 0.04254(11) 0.2769(2) 0.0390(12) Uani 1 1 d . . . N1B N 0.0702(3) 0.09625(16) 0.2770(3) 0.0409(14) Uani 1 1 d . . . N2B N 0.1254(4) 0.16527(16) 0.2091(3) 0.0504(17) Uani 1 1 d . . . N3B N 0.1343(3) 0.10174(16) 0.1056(3) 0.0462(16) Uani 1 1 d . . . N4B N 0.4480(3) 0.07480(16) 0.2392(3) 0.0389(14) Uani 1 1 d . . . N5B N 0.4204(3) 0.14090(17) 0.3310(3) 0.0501(16) Uani 1 1 d . . . N6B N 0.3851(3) 0.07210(17) 0.4120(3) 0.0433(15) Uani 1 1 d . . . C1B C 0.2057(4) 0.08340(18) 0.3961(3) 0.0353(16) Uani 1 1 d . . . C2B C 0.1320(4) 0.07217(18) 0.3922(3) 0.0344(16) Uani 1 1 d . . . C3B C 0.1111(4) 0.03715(19) 0.4221(3) 0.0363(16) Uani 1 1 d . . . H3B H 0.0626 0.0299 0.4175 0.044 Uiso 1 1 calc R . . C4B C 0.1595(4) 0.01247(17) 0.4587(3) 0.0315(15) Uani 1 1 d . . . C5B C 0.2293(4) 0.02697(19) 0.4713(3) 0.0377(17) Uani 1 1 d . . . H5B H 0.2616 0.0127 0.5005 0.045 Uiso 1 1 calc R . . C6B C 0.2530(4) 0.06140(18) 0.4426(3) 0.0341(16) Uani 1 1 d . . . C7B C 0.0774(4) 0.09972(18) 0.3573(4) 0.0423(18) Uani 1 1 d . . . H7B1 H 0.0304 0.0950 0.3774 0.051 Uiso 1 1 calc R . . H7B2 H 0.0915 0.1261 0.3696 0.051 Uiso 1 1 calc R . . C8B C 0.0375(4) 0.0582(2) 0.2610(4) 0.055(2) Uani 1 1 d . . . H8B1 H 0.0682 0.0382 0.2812 0.083 Uiso 1 1 calc R . . H8B2 H 0.0321 0.0549 0.2094 0.083 Uiso 1 1 calc R . . H8B3 H -0.0093 0.0568 0.2820 0.083 Uiso 1 1 calc R . . C9B C 0.0200(4) 0.1270(2) 0.2518(5) 0.071(3) Uani 1 1 d . . . H9B1 H -0.0200 0.1287 0.2843 0.085 Uiso 1 1 calc R . . H9B2 H 0.0001 0.1206 0.2038 0.085 Uiso 1 1 calc R . . C10B C 0.0581(5) 0.1654(2) 0.2491(5) 0.070(3) Uani 1 1 d . . . H10C H 0.0251 0.1842 0.2270 0.083 Uiso 1 1 calc R . . H10D H 0.0694 0.1739 0.2984 0.083 Uiso 1 1 calc R . . C11B C 0.1727(6) 0.1970(2) 0.2370(5) 0.088(3) Uani 1 1 d . . . H11D H 0.1438 0.2196 0.2451 0.133 Uiso 1 1 calc R . . H11E H 0.2085 0.2028 0.2023 0.133 Uiso 1 1 calc R . . H11F H 0.1964 0.1891 0.2819 0.133 Uiso 1 1 calc R . . C12B C 0.1111(4) 0.1705(2) 0.1303(4) 0.057(2) Uani 1 1 d . . . H12C H 0.1556 0.1785 0.1083 0.068 Uiso 1 1 calc R . . H12D H 0.0759 0.1911 0.1228 0.068 Uiso 1 1 calc R . . C13B C 0.0828(4) 0.1342(2) 0.0921(4) 0.057(2) Uani 1 1 d . . . H13C H 0.0357 0.1275 0.1099 0.068 Uiso 1 1 calc R . . H13D H 0.0772 0.1390 0.0404 0.068 Uiso 1 1 calc R . . C14B C 0.0975(4) 0.0653(2) 0.0861(4) 0.060(2) Uani 1 1 d . . . H14D H 0.0883 0.0643 0.0346 0.090 Uiso 1 1 calc R . . H14E H 0.0524 0.0638 0.1103 0.090 Uiso 1 1 calc R . . H14F H 0.1278 0.0438 0.1008 0.090 Uiso 1 1 calc R . . C15B C 0.1956(4) 0.10707(19) 0.0553(4) 0.0393(17) Uani 1 1 d . . . H15C H 0.2123 0.1336 0.0594 0.047 Uiso 1 1 calc R . . H15D H 0.1766 0.1034 0.0060 0.047 Uiso 1 1 calc R . . C16B C 0.2598(4) 0.08085(19) 0.0671(4) 0.0395(17) Uani 1 1 d . . . C17B C 0.3136(4) 0.09028(18) 0.1201(3) 0.0348(16) Uani 1 1 d . . . C18B C 0.3793(4) 0.07091(18) 0.1190(4) 0.0365(17) Uani 1 1 d . . . C19B C 0.3867(4) 0.03927(19) 0.0729(4) 0.0427(18) Uani 1 1 d . . . H19B H 0.4310 0.0264 0.0727 0.051 Uiso 1 1 calc R . . C20B C 0.3297(4) 0.02607(18) 0.0268(4) 0.0390(17) Uani 1 1 d . . . C21B C 0.2684(4) 0.04879(19) 0.0228(4) 0.0414(18) Uani 1 1 d . . . H21B H 0.2314 0.0424 -0.0108 0.050 Uiso 1 1 calc R . . C22B C 0.4428(4) 0.0869(2) 0.1617(3) 0.0431(18) Uani 1 1 d . . . H22C H 0.4868 0.0790 0.1386 0.052 Uiso 1 1 calc R . . H22D H 0.4405 0.1150 0.1597 0.052 Uiso 1 1 calc R . . C23B C 0.4627(4) 0.0329(2) 0.2398(4) 0.058(2) Uani 1 1 d . . . H23D H 0.5100 0.0282 0.2218 0.087 Uiso 1 1 calc R . . H23E H 0.4270 0.0199 0.2094 0.087 Uiso 1 1 calc R . . H23F H 0.4607 0.0233 0.2885 0.087 Uiso 1 1 calc R . . C24B C 0.5085(4) 0.0953(2) 0.2753(4) 0.063(2) Uani 1 1 d . . . H24C H 0.5498 0.0949 0.2444 0.075 Uiso 1 1 calc R . . H24D H 0.5222 0.0820 0.3201 0.075 Uiso 1 1 calc R . . C25B C 0.4893(5) 0.1365(2) 0.2919(4) 0.068(3) Uani 1 1 d . . . H25C H 0.5286 0.1479 0.3212 0.082 Uiso 1 1 calc R . . H25D H 0.4852 0.1509 0.2468 0.082 Uiso 1 1 calc R . . C26B C 0.3901(5) 0.1794(2) 0.3122(6) 0.089(4) Uani 1 1 d . . . H26D H 0.3519 0.1855 0.3441 0.133 Uiso 1 1 calc R . . H26E H 0.3712 0.1791 0.2630 0.133 Uiso 1 1 calc R . . H26F H 0.4276 0.1986 0.3172 0.133 Uiso 1 1 calc R . . C27B C 0.4335(5) 0.1388(2) 0.4096(4) 0.063(2) Uani 1 1 d . . . H27C H 0.3922 0.1498 0.4333 0.076 Uiso 1 1 calc R . . H27D H 0.4757 0.1544 0.4230 0.076 Uiso 1 1 calc R . . C28B C 0.4458(4) 0.0982(2) 0.4369(4) 0.059(2) Uani 1 1 d . . . H28C H 0.4912 0.0885 0.4192 0.070 Uiso 1 1 calc R . . H28D H 0.4495 0.0984 0.4895 0.070 Uiso 1 1 calc R . . C29B C 0.4064(4) 0.0320(2) 0.4181(4) 0.065(2) Uani 1 1 d . . . H29D H 0.4521 0.0283 0.3959 0.097 Uiso 1 1 calc R . . H29E H 0.3703 0.0160 0.3941 0.097 Uiso 1 1 calc R . . H29F H 0.4110 0.0249 0.4684 0.097 Uiso 1 1 calc R . . C30B C 0.3251(4) 0.0791(2) 0.4633(4) 0.0427(18) Uani 1 1 d . . . H30C H 0.3405 0.0692 0.5106 0.051 Uiso 1 1 calc R . . H30D H 0.3185 0.1068 0.4680 0.051 Uiso 1 1 calc R . . C31B C 0.1385(4) -0.02776(17) 0.4846(4) 0.0358(16) Uani 1 1 d . . . C32B C 0.1285(4) -0.02651(19) 0.5670(4) 0.051(2) Uani 1 1 d . . . H32D H 0.1681 -0.0126 0.5901 0.076 Uiso 1 1 calc R . . H32E H 0.1276 -0.0524 0.5857 0.076 Uiso 1 1 calc R . . H32F H 0.0837 -0.0138 0.5767 0.076 Uiso 1 1 calc R . . C33B C 0.0654(4) -0.0417(2) 0.4489(4) 0.054(2) Uani 1 1 d . . . H33D H 0.0302 -0.0213 0.4510 0.081 Uiso 1 1 calc R . . H33E H 0.0485 -0.0639 0.4744 0.081 Uiso 1 1 calc R . . H33F H 0.0724 -0.0484 0.3991 0.081 Uiso 1 1 calc R . . C34B C 0.1966(4) -0.05708(18) 0.4668(4) 0.0481(19) Uani 1 1 d . . . H34D H 0.2105 -0.0534 0.4177 0.072 Uiso 1 1 calc R . . H34E H 0.1778 -0.0828 0.4724 0.072 Uiso 1 1 calc R . . H34F H 0.2381 -0.0535 0.4991 0.072 Uiso 1 1 calc R . . C35B C 0.3331(4) -0.01304(19) -0.0126(4) 0.0429(18) Uani 1 1 d . . . C36B C 0.2892(5) -0.0122(2) -0.0826(4) 0.068(3) Uani 1 1 d . . . H36D H 0.3091 -0.0302 -0.1161 0.101 Uiso 1 1 calc R . . H36E H 0.2904 0.0134 -0.1028 0.101 Uiso 1 1 calc R . . H36F H 0.2400 -0.0192 -0.0739 0.101 Uiso 1 1 calc R . . C37B C 0.4097(5) -0.0238(2) -0.0304(5) 0.082(3) Uani 1 1 d . . . H37D H 0.4384 -0.0269 0.0137 0.124 Uiso 1 1 calc R . . H37E H 0.4301 -0.0036 -0.0591 0.124 Uiso 1 1 calc R . . H37F H 0.4093 -0.0476 -0.0571 0.124 Uiso 1 1 calc R . . C38B C 0.3025(7) -0.0430(3) 0.0369(5) 0.124(5) Uani 1 1 d . . . H38D H 0.2520 -0.0379 0.0430 0.187 Uiso 1 1 calc R . . H38E H 0.3280 -0.0421 0.0832 0.187 Uiso 1 1 calc R . . H38F H 0.3080 -0.0683 0.0160 0.187 Uiso 1 1 calc R . . C39B C 0.2464(4) 0.0312(2) 0.2496(4) 0.0401(18) Uani 1 1 d . . . H39B H 0.2399 0.0046 0.2461 0.048 Uiso 1 1 calc R . . B1 B 0.7910(4) 0.1375(2) 0.7652(4) 0.0333(18) Uani 1 1 d . . . C101 C 0.7403(4) 0.15998(19) 0.8241(4) 0.0362(16) Uani 1 1 d . . . C102 C 0.7054(4) 0.19526(19) 0.8124(4) 0.0414(17) Uani 1 1 d . . . H102 H 0.7121 0.2079 0.7686 0.050 Uiso 1 1 calc R . . C103 C 0.6611(4) 0.2129(2) 0.8619(4) 0.051(2) Uani 1 1 d . . . H103 H 0.6398 0.2367 0.8512 0.061 Uiso 1 1 calc R . . C104 C 0.6490(4) 0.1948(2) 0.9267(5) 0.056(2) Uani 1 1 d . . . H104 H 0.6210 0.2067 0.9612 0.067 Uiso 1 1 calc R . . C105 C 0.6793(4) 0.1588(2) 0.9394(4) 0.053(2) Uani 1 1 d . . . H105 H 0.6695 0.1457 0.9820 0.063 Uiso 1 1 calc R . . C106 C 0.7237(4) 0.1420(2) 0.8901(4) 0.0441(18) Uani 1 1 d . . . H106 H 0.7436 0.1178 0.9008 0.053 Uiso 1 1 calc R . . C201 C 0.8497(3) 0.10806(18) 0.8048(4) 0.0347(15) Uani 1 1 d . . . C202 C 0.8669(4) 0.0719(2) 0.7768(4) 0.051(2) Uani 1 1 d . . . H202 H 0.8442 0.0641 0.7335 0.061 Uiso 1 1 calc R . . C203 C 0.9165(5) 0.0473(2) 0.8110(5) 0.062(2) Uani 1 1 d . . . H203 H 0.9254 0.0232 0.7906 0.074 Uiso 1 1 calc R . . C204 C 0.9526(5) 0.0576(3) 0.8738(5) 0.066(3) Uani 1 1 d . . . H204 H 0.9860 0.0410 0.8966 0.080 Uiso 1 1 calc R . . C205 C 0.9377(4) 0.0940(2) 0.9029(4) 0.053(2) Uani 1 1 d . . . H205 H 0.9616 0.1020 0.9457 0.064 Uiso 1 1 calc R . . C206 C 0.8881(4) 0.1179(2) 0.8688(4) 0.0438(18) Uani 1 1 d . . . H206 H 0.8795 0.1420 0.8893 0.053 Uiso 1 1 calc R . . C301 C 0.7307(4) 0.11472(19) 0.7141(4) 0.0363(16) Uani 1 1 d . . . C302 C 0.6991(4) 0.07994(19) 0.7346(4) 0.0420(18) Uani 1 1 d . . . H302 H 0.7140 0.0690 0.7788 0.050 Uiso 1 1 calc R . . C303 C 0.6470(4) 0.0609(2) 0.6928(4) 0.050(2) Uani 1 1 d . . . H303 H 0.6306 0.0367 0.7072 0.059 Uiso 1 1 calc R . . C304 C 0.6191(4) 0.0773(2) 0.6297(4) 0.050(2) Uani 1 1 d . . . H304 H 0.5820 0.0651 0.6029 0.060 Uiso 1 1 calc R . . C305 C 0.6472(4) 0.1124(2) 0.6068(4) 0.0460(19) Uani 1 1 d . . . H305 H 0.6294 0.1239 0.5641 0.055 Uiso 1 1 calc R . . C306 C 0.7017(4) 0.1299(2) 0.6480(4) 0.0457(19) Uani 1 1 d . . . H306 H 0.7205 0.1532 0.6314 0.055 Uiso 1 1 calc R . . C401 C 0.8374(4) 0.16783(19) 0.7156(4) 0.0377(17) Uani 1 1 d . . . C402 C 0.8539(4) 0.2061(2) 0.7310(4) 0.0454(18) Uani 1 1 d . . . H402 H 0.8376 0.2165 0.7740 0.055 Uiso 1 1 calc R . . C403 C 0.8932(4) 0.2301(2) 0.6866(5) 0.055(2) Uani 1 1 d . . . H403 H 0.9018 0.2558 0.6996 0.067 Uiso 1 1 calc R . . C404 C 0.9193(4) 0.2157(2) 0.6235(4) 0.060(2) Uani 1 1 d . . . H404 H 0.9441 0.2316 0.5922 0.072 Uiso 1 1 calc R . . C405 C 0.9081(4) 0.1776(3) 0.6076(4) 0.056(2) Uani 1 1 d . . . H405 H 0.9274 0.1671 0.5661 0.068 Uiso 1 1 calc R . . C406 C 0.8690(4) 0.1546(2) 0.6518(4) 0.0457(19) Uani 1 1 d . . . H406 H 0.8628 0.1287 0.6391 0.055 Uiso 1 1 calc R . . B2 B 0.7544(4) 0.1157(2) 0.2526(4) 0.0308(18) Uani 1 1 d . . . C501 C 0.8130(4) 0.14171(18) 0.3021(4) 0.0366(16) Uani 1 1 d . . . C502 C 0.8402(4) 0.17653(19) 0.2772(4) 0.0442(19) Uani 1 1 d . . . H502 H 0.8239 0.1856 0.2320 0.053 Uiso 1 1 calc R . . C503 C 0.8915(4) 0.1986(2) 0.3178(5) 0.053(2) Uani 1 1 d . . . H503 H 0.9063 0.2226 0.3010 0.063 Uiso 1 1 calc R . . C504 C 0.9195(4) 0.1844(2) 0.3824(5) 0.056(2) Uani 1 1 d . . . H504 H 0.9542 0.1985 0.4093 0.068 Uiso 1 1 calc R . . C505 C 0.8957(4) 0.1492(2) 0.4071(4) 0.053(2) Uani 1 1 d . . . H505 H 0.9152 0.1391 0.4503 0.063 Uiso 1 1 calc R . . C506 C 0.8431(4) 0.12886(19) 0.3680(4) 0.0442(18) Uani 1 1 d . . . H506 H 0.8271 0.1055 0.3866 0.053 Uiso 1 1 calc R . . C601 C 0.7096(4) 0.08556(18) 0.3045(3) 0.0354(16) Uani 1 1 d . . . C602 C 0.6928(4) 0.04707(19) 0.2864(4) 0.0407(17) Uani 1 1 d . . . H602 H 0.7086 0.0373 0.2428 0.049 Uiso 1 1 calc R . . C603 C 0.6539(4) 0.0230(2) 0.3305(5) 0.057(2) Uani 1 1 d . . . H603 H 0.6446 -0.0025 0.3165 0.068 Uiso 1 1 calc R . . C604 C 0.6289(4) 0.0366(3) 0.3954(4) 0.058(2) Uani 1 1 d . . . H604 H 0.6032 0.0206 0.4257 0.069 Uiso 1 1 calc R . . C605 C 0.6429(4) 0.0744(3) 0.4137(4) 0.055(2) Uani 1 1 d . . . H605 H 0.6260 0.0842 0.4569 0.065 Uiso 1 1 calc R . . C606 C 0.6816(4) 0.0980(2) 0.3694(4) 0.0445(18) Uani 1 1 d . . . H606 H 0.6894 0.1236 0.3835 0.053 Uiso 1 1 calc R . . C701 C 0.8035(4) 0.09300(19) 0.1953(4) 0.0419(18) Uani 1 1 d . . . C702 C 0.8418(4) 0.0588(2) 0.2105(4) 0.0438(18) Uani 1 1 d . . . H702 H 0.8382 0.0479 0.2563 0.053 Uiso 1 1 calc R . . C703 C 0.8848(4) 0.0399(2) 0.1612(5) 0.058(2) Uani 1 1 d . . . H703 H 0.9074 0.0166 0.1736 0.070 Uiso 1 1 calc R . . C704 C 0.8936(4) 0.0563(3) 0.0928(5) 0.066(3) Uani 1 1 d . . . H704 H 0.9224 0.0445 0.0590 0.079 Uiso 1 1 calc R . . C705 C 0.8580(5) 0.0907(3) 0.0771(5) 0.071(3) Uani 1 1 d . . . H705 H 0.8637 0.1023 0.0321 0.086 Uiso 1 1 calc R . . C706 C 0.8150(5) 0.1082(2) 0.1255(4) 0.059(2) Uani 1 1 d . . . H706 H 0.7921 0.1312 0.1121 0.071 Uiso 1 1 calc R . . C801 C 0.6922(4) 0.14256(19) 0.2130(4) 0.0404(17) Uani 1 1 d . . . C802 C 0.6708(4) 0.1789(2) 0.2377(4) 0.049(2) Uani 1 1 d . . . H802 H 0.6945 0.1892 0.2787 0.059 Uiso 1 1 calc R . . C803 C 0.6146(5) 0.2005(2) 0.2028(6) 0.073(3) Uani 1 1 d . . . H803 H 0.6023 0.2247 0.2210 0.087 Uiso 1 1 calc R . . C804 C 0.5784(5) 0.1865(3) 0.1432(5) 0.069(3) Uani 1 1 d . . . H804 H 0.5420 0.2010 0.1198 0.082 Uiso 1 1 calc R . . C805 C 0.5963(5) 0.1511(3) 0.1184(4) 0.067(3) Uani 1 1 d . . . H805 H 0.5716 0.1412 0.0776 0.080 Uiso 1 1 calc R . . C806 C 0.6509(4) 0.1293(2) 0.1524(4) 0.052(2) Uani 1 1 d . . . H806 H 0.6606 0.1048 0.1343 0.062 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 Ni1A 0.0226(5) 0.0450(5) 0.0357(5) -0.0069(4) 0.0051(4) -0.0056(4) Ni2A 0.0233(5) 0.0416(5) 0.0369(5) 0.0053(4) 0.0048(4) 0.0019(4) S1A 0.0302(10) 0.0425(10) 0.0412(11) -0.0038(8) 0.0105(8) -0.0046(8) S2A 0.0307(10) 0.0441(10) 0.0384(10) 0.0019(8) 0.0071(8) -0.0005(8) O1A 0.023(3) 0.048(3) 0.049(3) 0.000(2) -0.004(2) -0.003(2) O2A 0.020(3) 0.045(3) 0.049(3) 0.002(2) -0.004(2) 0.004(2) N1A 0.030(4) 0.077(5) 0.030(3) -0.013(3) 0.006(3) -0.011(3) N2A 0.024(3) 0.057(4) 0.057(4) -0.016(3) 0.012(3) -0.012(3) N3A 0.018(3) 0.065(4) 0.032(3) -0.009(3) 0.004(2) 0.001(3) N4A 0.030(4) 0.076(4) 0.033(4) 0.005(3) 0.002(3) 0.004(3) N5A 0.031(4) 0.058(4) 0.066(5) 0.023(3) 0.015(3) 0.005(3) N6A 0.021(3) 0.045(3) 0.041(4) 0.008(3) 0.006(3) 0.004(2) C1A 0.031(4) 0.042(4) 0.029(4) -0.011(3) 0.010(3) 0.003(3) C2A 0.026(4) 0.058(5) 0.030(4) -0.008(3) 0.011(3) 0.001(3) C3A 0.032(4) 0.059(5) 0.034(4) -0.002(3) -0.006(3) 0.009(4) C4A 0.033(4) 0.048(4) 0.036(4) -0.003(3) 0.010(3) -0.003(3) C5A 0.024(4) 0.051(4) 0.038(4) 0.002(3) 0.002(3) -0.001(3) C6A 0.026(4) 0.041(4) 0.040(4) -0.002(3) 0.013(3) 0.000(3) C7A 0.024(4) 0.075(5) 0.025(4) -0.013(3) 0.005(3) -0.003(3) C8A 0.039(5) 0.100(7) 0.052(5) 0.005(4) 0.011(4) 0.025(5) C9A 0.033(5) 0.111(7) 0.049(5) -0.014(5) 0.008(4) -0.021(5) C10A 0.054(6) 0.078(6) 0.068(6) -0.033(5) 0.021(5) -0.041(5) C11A 0.065(7) 0.040(5) 0.144(10) -0.018(5) 0.003(6) 0.001(5) C12A 0.050(6) 0.073(6) 0.056(5) -0.019(4) 0.021(4) -0.032(4) C13A 0.023(4) 0.089(6) 0.055(5) -0.021(4) 0.007(4) -0.014(4) C14A 0.049(5) 0.089(6) 0.040(5) -0.004(4) 0.000(4) 0.036(5) C15A 0.023(4) 0.054(4) 0.044(5) -0.009(3) 0.009(3) -0.004(3) C16A 0.033(4) 0.042(4) 0.027(4) -0.001(3) 0.005(3) -0.007(3) C17A 0.016(4) 0.052(4) 0.021(3) 0.004(3) 0.006(3) -0.002(3) C18A 0.034(4) 0.055(5) 0.026(4) 0.009(3) 0.002(3) -0.008(3) C19A 0.041(5) 0.055(5) 0.036(4) -0.010(3) -0.001(4) -0.008(4) C20A 0.033(4) 0.044(4) 0.039(4) -0.001(3) 0.010(3) -0.006(3) C21A 0.019(4) 0.051(4) 0.036(4) -0.009(3) 0.007(3) -0.003(3) C22A 0.031(5) 0.092(6) 0.030(4) 0.011(4) 0.008(3) 0.005(4) C23A 0.037(5) 0.100(7) 0.052(6) -0.007(4) -0.001(4) -0.028(5) C24A 0.038(5) 0.114(8) 0.039(5) 0.010(5) -0.003(4) 0.011(5) C25A 0.060(6) 0.106(8) 0.055(6) 0.040(5) 0.015(5) 0.038(5) C26A 0.038(5) 0.041(5) 0.133(9) 0.023(5) -0.002(5) 0.005(4) C27A 0.037(5) 0.052(5) 0.061(5) 0.018(4) 0.006(4) 0.023(4) C28A 0.015(4) 0.066(5) 0.065(5) 0.013(4) 0.000(3) 0.011(3) C29A 0.036(5) 0.061(5) 0.055(5) -0.002(4) 0.007(4) -0.004(4) C30A 0.022(4) 0.055(4) 0.042(4) 0.006(3) 0.007(3) 0.003(3) C31A 0.051(5) 0.046(4) 0.041(5) 0.010(3) -0.008(4) 0.004(4) C32A 0.087(9) 0.092(8) 0.214(15) 0.077(8) -0.034(9) -0.039(7) C33A 0.115(10) 0.057(6) 0.193(14) -0.011(7) 0.030(9) 0.010(6) C34A 0.42(3) 0.056(7) 0.053(8) 0.019(5) -0.017(11) -0.010(10) C35A 0.049(5) 0.049(5) 0.043(5) 0.002(3) 0.006(4) -0.007(4) C36A 0.061(6) 0.049(5) 0.060(6) -0.008(4) 0.010(4) -0.012(4) C37A 0.092(7) 0.046(5) 0.065(6) -0.009(4) 0.035(5) -0.012(4) C38A 0.068(7) 0.057(5) 0.100(8) -0.013(5) 0.003(6) 0.016(5) C39A 0.039(5) 0.035(4) 0.046(5) 0.003(3) 0.002(4) -0.008(3) Ni1B 0.0344(6) 0.0391(5) 0.0387(5) 0.0035(4) 0.0096(4) 0.0070(4) Ni2B 0.0305(5) 0.0408(5) 0.0336(5) -0.0041(4) 0.0090(4) -0.0059(4) S1B 0.0384(11) 0.0409(10) 0.0369(10) -0.0017(7) 0.0124(8) 0.0002(8) S2B 0.0419(12) 0.0408(10) 0.0399(11) -0.0013(8) 0.0121(8) -0.0015(8) O1B 0.026(3) 0.037(3) 0.053(3) -0.002(2) -0.002(2) 0.004(2) O2B 0.028(3) 0.040(3) 0.049(3) 0.001(2) 0.000(2) 0.003(2) N1B 0.031(4) 0.055(4) 0.037(4) 0.011(3) 0.004(3) 0.013(3) N2B 0.051(5) 0.049(4) 0.052(4) 0.008(3) 0.008(3) 0.016(3) N3B 0.043(4) 0.056(4) 0.039(4) 0.003(3) 0.005(3) 0.014(3) N4B 0.030(3) 0.056(4) 0.031(3) -0.006(3) 0.007(3) -0.007(3) N5B 0.043(4) 0.054(4) 0.055(4) -0.007(3) 0.012(3) -0.012(3) N6B 0.035(4) 0.063(4) 0.033(4) -0.004(3) 0.011(3) -0.009(3) C1B 0.040(5) 0.045(4) 0.022(4) -0.008(3) 0.007(3) -0.002(3) C2B 0.034(4) 0.037(4) 0.032(4) 0.000(3) -0.001(3) 0.009(3) C3B 0.024(4) 0.054(4) 0.031(4) -0.001(3) 0.003(3) 0.000(3) C4B 0.031(4) 0.036(4) 0.028(4) 0.002(3) 0.003(3) 0.000(3) C5B 0.029(4) 0.055(4) 0.029(4) 0.004(3) 0.001(3) 0.006(3) C6B 0.029(4) 0.043(4) 0.030(4) -0.003(3) 0.007(3) 0.004(3) C7B 0.024(4) 0.045(4) 0.059(5) 0.008(3) 0.011(3) 0.013(3) C8B 0.026(4) 0.089(6) 0.049(5) 0.007(4) -0.009(4) -0.018(4) C9B 0.038(5) 0.095(7) 0.083(7) 0.047(5) 0.025(4) 0.025(5) C10B 0.073(7) 0.064(6) 0.074(6) 0.029(5) 0.033(5) 0.046(5) C11B 0.116(9) 0.036(5) 0.112(9) -0.004(5) -0.016(7) 0.021(5) C12B 0.064(6) 0.055(5) 0.052(5) 0.019(4) 0.015(4) 0.032(4) C13B 0.046(5) 0.066(5) 0.059(6) 0.002(4) 0.005(4) 0.022(4) C14B 0.042(5) 0.073(6) 0.067(6) -0.010(4) 0.007(4) -0.017(4) C15B 0.029(4) 0.055(4) 0.034(4) 0.004(3) 0.008(3) 0.006(3) C16B 0.036(5) 0.050(4) 0.032(4) 0.003(3) 0.008(3) 0.005(3) C17B 0.031(4) 0.047(4) 0.027(4) 0.006(3) 0.007(3) -0.005(3) C18B 0.031(4) 0.040(4) 0.039(4) 0.000(3) 0.001(3) -0.002(3) C19B 0.039(5) 0.048(4) 0.041(4) -0.002(3) 0.004(4) 0.006(3) C20B 0.042(5) 0.041(4) 0.034(4) 0.002(3) 0.002(3) -0.004(3) C21B 0.036(5) 0.055(5) 0.033(4) -0.004(3) 0.000(3) 0.005(4) C22B 0.033(4) 0.068(5) 0.029(4) -0.009(3) 0.016(3) -0.010(3) C23B 0.056(6) 0.076(6) 0.042(5) 0.003(4) 0.004(4) 0.026(4) C24B 0.031(5) 0.100(7) 0.058(6) -0.027(5) 0.008(4) -0.017(4) C25B 0.070(7) 0.095(7) 0.041(5) -0.019(4) 0.017(4) -0.052(5) C26B 0.091(8) 0.037(5) 0.136(10) -0.009(5) -0.025(7) -0.007(5) C27B 0.056(6) 0.082(6) 0.052(6) -0.021(4) 0.010(4) -0.035(5) C28B 0.027(5) 0.108(7) 0.041(5) 0.000(4) 0.002(4) -0.016(4) C29B 0.060(6) 0.070(6) 0.066(6) 0.019(4) 0.023(5) 0.024(4) C30B 0.034(4) 0.068(5) 0.027(4) 0.000(3) 0.012(3) -0.003(4) C31B 0.034(4) 0.034(4) 0.041(4) 0.001(3) 0.008(3) -0.003(3) C32B 0.055(6) 0.049(5) 0.049(5) 0.004(3) 0.015(4) 0.004(4) C33B 0.042(5) 0.053(5) 0.067(6) 0.006(4) 0.002(4) -0.001(4) C34B 0.051(5) 0.045(4) 0.049(5) -0.001(3) 0.006(4) 0.013(4) C35B 0.040(5) 0.045(4) 0.044(5) -0.005(3) 0.001(4) 0.002(3) C36B 0.079(7) 0.067(6) 0.057(6) -0.018(4) -0.007(5) -0.011(5) C37B 0.071(7) 0.080(6) 0.097(8) -0.038(5) 0.006(6) 0.014(5) C38B 0.245(16) 0.062(6) 0.069(8) 0.006(5) 0.044(8) -0.036(8) C39B 0.029(5) 0.039(4) 0.052(5) -0.005(3) 0.001(4) 0.000(3) B1 0.028(4) 0.040(4) 0.032(4) -0.002(3) 0.004(3) -0.002(4) C101 0.034(4) 0.045(4) 0.030(4) -0.005(3) 0.006(3) -0.005(3) C102 0.030(4) 0.053(5) 0.041(4) -0.002(3) 0.004(3) 0.004(3) C103 0.037(5) 0.056(5) 0.059(6) -0.007(4) -0.002(4) 0.019(4) C104 0.025(4) 0.084(6) 0.059(6) -0.024(4) 0.010(4) 0.005(4) C105 0.044(5) 0.067(5) 0.047(5) -0.008(4) 0.009(4) 0.002(4) C106 0.034(4) 0.053(5) 0.047(5) 0.005(3) 0.014(3) 0.004(3) C201 0.028(4) 0.040(4) 0.036(4) 0.000(3) 0.011(3) -0.007(3) C202 0.047(5) 0.048(5) 0.058(5) -0.005(4) 0.012(4) 0.001(4) C203 0.059(6) 0.040(5) 0.087(7) -0.005(4) 0.021(5) 0.009(4) C204 0.060(6) 0.075(6) 0.064(6) 0.024(5) 0.009(5) 0.023(5) C205 0.037(5) 0.078(6) 0.045(5) 0.007(4) 0.008(4) 0.010(4) C206 0.033(4) 0.056(5) 0.042(5) 0.001(3) 0.003(3) 0.007(3) C301 0.031(4) 0.043(4) 0.035(4) -0.003(3) 0.010(3) 0.004(3) C302 0.035(5) 0.049(4) 0.042(4) -0.001(3) -0.001(4) -0.009(3) C303 0.049(5) 0.046(4) 0.054(5) -0.009(4) 0.009(4) -0.002(4) C304 0.036(5) 0.065(5) 0.049(5) -0.013(4) -0.007(4) -0.007(4) C305 0.042(5) 0.058(5) 0.039(4) -0.003(4) 0.002(4) 0.007(4) C306 0.038(5) 0.053(5) 0.045(5) -0.003(3) 0.000(4) 0.002(4) C401 0.030(4) 0.053(5) 0.030(4) 0.005(3) -0.002(3) 0.000(3) C402 0.043(5) 0.057(5) 0.037(4) -0.002(3) 0.012(4) -0.004(4) C403 0.050(6) 0.056(5) 0.061(6) 0.005(4) 0.004(4) -0.018(4) C404 0.059(6) 0.073(6) 0.049(5) 0.018(4) 0.005(4) -0.024(5) C405 0.044(5) 0.096(7) 0.030(4) 0.000(4) 0.008(4) -0.008(5) C406 0.052(5) 0.049(5) 0.037(4) -0.006(3) 0.010(4) -0.009(4) B2 0.027(4) 0.032(4) 0.033(4) -0.004(3) 0.002(3) -0.003(3) C501 0.034(4) 0.035(4) 0.041(4) -0.005(3) 0.003(3) 0.006(3) C502 0.037(5) 0.043(4) 0.054(5) 0.004(3) 0.005(4) 0.003(3) C503 0.035(5) 0.040(4) 0.083(6) -0.013(4) 0.008(4) -0.003(3) C504 0.038(5) 0.064(6) 0.067(6) -0.027(4) -0.005(4) 0.001(4) C505 0.044(5) 0.068(6) 0.045(5) -0.008(4) -0.005(4) 0.003(4) C506 0.051(5) 0.043(4) 0.039(4) -0.002(3) 0.002(4) 0.009(4) C601 0.036(4) 0.044(4) 0.026(4) 0.001(3) 0.007(3) 0.002(3) C602 0.037(5) 0.046(4) 0.040(4) -0.001(3) 0.008(3) -0.002(3) C603 0.038(5) 0.055(5) 0.077(7) 0.014(4) 0.001(4) -0.008(4) C604 0.038(5) 0.093(7) 0.042(5) 0.016(4) 0.006(4) -0.008(4) C605 0.035(5) 0.092(7) 0.037(5) -0.004(4) 0.008(4) 0.000(4) C606 0.043(5) 0.055(5) 0.037(4) -0.007(3) 0.011(4) 0.001(4) C701 0.047(5) 0.043(4) 0.037(4) -0.005(3) 0.007(4) -0.007(4) C702 0.028(4) 0.054(5) 0.050(5) -0.011(4) 0.004(4) -0.003(3) C703 0.038(5) 0.069(6) 0.069(6) -0.024(4) 0.004(4) 0.000(4) C704 0.037(5) 0.108(8) 0.054(6) -0.033(5) 0.022(4) -0.013(5) C705 0.073(7) 0.089(7) 0.054(6) -0.002(5) 0.032(5) -0.009(5) C706 0.071(6) 0.057(5) 0.051(5) -0.003(4) 0.029(4) -0.012(4) C801 0.042(5) 0.044(4) 0.035(4) 0.002(3) 0.009(3) -0.010(3) C802 0.051(5) 0.049(5) 0.048(5) -0.001(4) 0.001(4) 0.001(4) C803 0.055(6) 0.066(6) 0.098(8) 0.018(5) 0.009(6) 0.010(5) C804 0.055(6) 0.086(7) 0.066(7) 0.032(5) 0.004(5) 0.012(5) C805 0.052(6) 0.109(8) 0.038(5) 0.017(5) -0.004(4) -0.018(5) C806 0.045(5) 0.066(5) 0.044(5) 0.001(4) 0.002(4) -0.008(4) #BOND LENGTHS AND ANGLES _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 Ni1A O1A 1.992(4) . ? Ni1A N2A 2.146(5) . ? Ni1A N3A 2.255(5) . ? Ni1A N1A 2.266(6) . ? Ni1A S1A 2.477(2) . ? Ni1A S2A 2.497(2) . ? Ni2A O2A 1.996(4) . ? Ni2A N5A 2.136(6) . ? Ni2A N6A 2.243(6) . ? Ni2A N4A 2.320(6) . ? Ni2A S1A 2.478(2) . ? Ni2A S2A 2.487(2) . ? S1A C1A 1.745(7) . ? S2A C17A 1.755(7) . ? O1A C39A 1.272(7) . ? O2A C39A 1.237(7) . ? N1A C9A 1.478(9) . ? N1A C8A 1.485(9) . ? N1A C7A 1.496(8) . ? N2A C11A 1.449(9) . ? N2A C10A 1.496(9) . ? N2A C12A 1.497(9) . ? N3A C14A 1.447(8) . ? N3A C15A 1.490(8) . ? N3A C13A 1.514(8) . ? N4A C23A 1.470(9) . ? N4A C24A 1.482(9) . ? N4A C22A 1.495(9) . ? N5A C26A 1.456(9) . ? N5A C25A 1.483(10) . ? N5A C27A 1.505(9) . ? N6A C29A 1.475(8) . ? N6A C30A 1.482(8) . ? N6A C28A 1.514(7) . ? C1A C6A 1.400(9) . ? C1A C2A 1.426(9) . ? C2A C3A 1.378(9) . ? C2A C7A 1.503(9) . ? C3A C4A 1.397(9) . ? C4A C5A 1.407(8) . ? C4A C31A 1.530(9) . ? C5A C6A 1.385(8) . ? C6A C30A 1.488(8) . ? C9A C10A 1.484(11) . ? C12A C13A 1.510(10) . ? C15A C16A 1.508(8) . ? C16A C21A 1.379(8) . ? C16A C17A 1.406(8) . ? C17A C18A 1.392(8) . ? C18A C19A 1.398(9) . ? C18A C22A 1.498(9) . ? C19A C20A 1.391(9) . ? C20A C21A 1.390(8) . ? C20A C35A 1.513(9) . ? C24A C25A 1.488(11) . ? C27A C28A 1.494(9) . ? C31A C34A 1.451(11) . ? C31A C33A 1.527(12) . ? C31A C32A 1.527(11) . ? C35A C36A 1.519(10) . ? C35A C37A 1.526(10) . ? C35A C38A 1.526(10) . ? Ni1B O1B 2.000(4) . ? Ni1B N2B 2.167(5) . ? Ni1B N1B 2.238(6) . ? Ni1B N3B 2.313(6) . ? Ni1B S2B 2.466(2) . ? Ni1B S1B 2.501(2) . ? Ni2B O2B 2.000(4) . ? Ni2B N5B 2.135(6) . ? Ni2B N4B 2.250(6) . ? Ni2B N6B 2.319(6) . ? Ni2B S1B 2.479(2) . ? Ni2B S2B 2.488(2) . ? S1B C1B 1.735(7) . ? S2B C17B 1.763(7) . ? O1B C39B 1.255(7) . ? O2B C39B 1.266(7) . ? N1B C8B 1.470(8) . ? N1B C9B 1.472(8) . ? N1B C7B 1.487(8) . ? N2B C10B 1.470(10) . ? N2B C12B 1.478(9) . ? N2B C11B 1.480(9) . ? N3B C14B 1.469(8) . ? N3B C13B 1.486(8) . ? N3B C15B 1.501(9) . ? N4B C24B 1.460(8) . ? N4B C23B 1.471(8) . ? N4B C22B 1.491(8) . ? N5B C27B 1.464(9) . ? N5B C26B 1.478(9) . ? N5B C25B 1.493(10) . ? N6B C29B 1.444(8) . ? N6B C28B 1.497(8) . ? N6B C30B 1.504(8) . ? C1B C2B 1.412(9) . ? C1B C6B 1.420(8) . ? C2B C3B 1.390(9) . ? C2B C7B 1.513(8) . ? C3B C4B 1.389(8) . ? C4B C5B 1.393(8) . ? C4B C31B 1.524(8) . ? C5B C6B 1.379(9) . ? C6B C30B 1.500(9) . ? C9B C10B 1.503(11) . ? C12B C13B 1.519(10) . ? C15B C16B 1.501(9) . ? C16B C21B 1.389(9) . ? C16B C17B 1.404(8) . ? C17B C18B 1.386(9) . ? C18B C19B 1.394(9) . ? C18B C22B 1.493(8) . ? C19B C20B 1.403(9) . ? C20B C21B 1.375(9) . ? C20B C35B 1.537(9) . ? C24B C25B 1.501(10) . ? C27B C28B 1.503(10) . ? C31B C34B 1.519(9) . ? C31B C32B 1.540(9) . ? C31B C33B 1.554(9) . ? C35B C36B 1.499(9) . ? C35B C38B 1.505(11) . ? C35B C37B 1.509(11) . ? B1 C301 1.632(9) . ? B1 C201 1.637(10) . ? B1 C401 1.651(10) . ? B1 C101 1.655(10) . ? C101 C102 1.391(9) . ? C101 C106 1.413(9) . ? C102 C103 1.389(10) . ? C103 C104 1.375(10) . ? C104 C105 1.379(10) . ? C105 C106 1.378(10) . ? C201 C202 1.391(9) . ? C201 C206 1.396(9) . ? C202 C203 1.385(10) . ? C203 C204 1.361(11) . ? C204 C205 1.398(10) . ? C205 C206 1.368(9) . ? C301 C302 1.393(9) . ? C301 C306 1.414(9) . ? C302 C303 1.377(9) . ? C303 C304 1.376(9) . ? C304 C305 1.391(10) . ? C305 C306 1.377(9) . ? C401 C402 1.385(9) . ? C401 C406 1.410(9) . ? C402 C403 1.390(10) . ? C403 C404 1.371(11) . ? C404 C405 1.363(10) . ? C405 C406 1.365(10) . ? B2 C701 1.620(10) . ? B2 C801 1.627(10) . ? B2 C501 1.654(9) . ? B2 C601 1.657(10) . ? C501 C502 1.388(9) . ? C501 C506 1.390(9) . ? C502 C503 1.409(9) . ? C503 C504 1.371(10) . ? C504 C505 1.378(10) . ? C505 C506 1.379(9) . ? C601 C606 1.389(9) . ? C601 C602 1.402(8) . ? C602 C603 1.384(10) . ? C603 C604 1.382(11) . ? C604 C605 1.369(10) . ? C605 C606 1.376(10) . ? C701 C702 1.400(9) . ? C701 C706 1.416(10) . ? C702 C703 1.392(10) . ? C703 C704 1.399(11) . ? C704 C705 1.383(11) . ? C705 C706 1.359(11) . ? C801 C802 1.397(9) . ? C801 C806 1.405(9) . ? C802 C803 1.412(10) . ? C803 C804 1.354(11) . ? C804 C805 1.351(11) . ? C805 C806 1.390(10) . ? 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 O1A Ni1A N2A 165.8(2) . . ? O1A Ni1A N3A 88.03(19) . . ? N2A Ni1A N3A 83.4(2) . . ? O1A Ni1A N1A 87.38(19) . . ? N2A Ni1A N1A 82.5(2) . . ? N3A Ni1A N1A 97.6(2) . . ? O1A Ni1A S1A 94.79(14) . . ? N2A Ni1A S1A 95.46(17) . . ? N3A Ni1A S1A 170.75(15) . . ? N1A Ni1A S1A 91.38(16) . . ? O1A Ni1A S2A 93.83(13) . . ? N2A Ni1A S2A 97.66(18) . . ? N3A Ni1A S2A 91.06(14) . . ? N1A Ni1A S2A 171.34(16) . . ? S1A Ni1A S2A 79.98(7) . . ? O2A Ni2A N5A 164.6(2) . . ? O2A Ni2A N6A 87.85(19) . . ? N5A Ni2A N6A 82.9(2) . . ? O2A Ni2A N4A 88.06(19) . . ? N5A Ni2A N4A 81.2(2) . . ? N6A Ni2A N4A 98.5(2) . . ? O2A Ni2A S1A 95.67(13) . . ? N5A Ni2A S1A 96.86(19) . . ? N6A Ni2A S1A 91.41(15) . . ? N4A Ni2A S1A 169.59(16) . . ? O2A Ni2A S2A 93.95(14) . . ? N5A Ni2A S2A 97.05(17) . . ? N6A Ni2A S2A 171.50(15) . . ? N4A Ni2A S2A 89.91(16) . . ? S1A Ni2A S2A 80.15(7) . . ? C1A S1A Ni1A 103.1(2) . . ? C1A S1A Ni2A 101.8(2) . . ? Ni1A S1A Ni2A 89.28(7) . . ? C17A S2A Ni2A 100.6(2) . . ? C17A S2A Ni1A 100.4(2) . . ? Ni2A S2A Ni1A 88.62(7) . . ? C39A O1A Ni1A 133.7(4) . . ? C39A O2A Ni2A 133.3(4) . . ? C9A N1A C8A 109.5(6) . . ? C9A N1A C7A 107.4(5) . . ? C8A N1A C7A 106.1(6) . . ? C9A N1A Ni1A 103.7(4) . . ? C8A N1A Ni1A 118.4(4) . . ? C7A N1A Ni1A 111.2(4) . . ? C11A N2A C10A 109.7(6) . . ? C11A N2A C12A 106.8(6) . . ? C10A N2A C12A 109.7(6) . . ? C11A N2A Ni1A 115.9(5) . . ? C10A N2A Ni1A 108.0(4) . . ? C12A N2A Ni1A 106.5(4) . . ? C14A N3A C15A 106.9(5) . . ? C14A N3A C13A 109.6(6) . . ? C15A N3A C13A 105.5(5) . . ? C14A N3A Ni1A 117.5(5) . . ? C15A N3A Ni1A 111.5(4) . . ? C13A N3A Ni1A 105.2(4) . . ? C23A N4A C24A 110.7(6) . . ? C23A N4A C22A 107.9(6) . . ? C24A N4A C22A 106.5(6) . . ? C23A N4A Ni2A 116.1(4) . . ? C24A N4A Ni2A 105.0(4) . . ? C22A N4A Ni2A 110.1(4) . . ? C26A N5A C25A 108.6(6) . . ? C26A N5A C27A 108.2(6) . . ? C25A N5A C27A 111.7(6) . . ? C26A N5A Ni2A 113.0(4) . . ? C25A N5A Ni2A 107.1(5) . . ? C27A N5A Ni2A 108.3(4) . . ? C29A N6A C30A 107.3(5) . . ? C29A N6A C28A 108.0(5) . . ? C30A N6A C28A 108.1(5) . . ? C29A N6A Ni2A 117.1(4) . . ? C30A N6A Ni2A 111.5(4) . . ? C28A N6A Ni2A 104.5(4) . . ? C6A C1A C2A 118.1(6) . . ? C6A C1A S1A 121.4(5) . . ? C2A C1A S1A 120.6(5) . . ? C3A C2A C1A 118.7(6) . . ? C3A C2A C7A 122.4(6) . . ? C1A C2A C7A 118.7(6) . . ? C2A C3A C4A 123.8(6) . . ? C3A C4A C5A 115.5(6) . . ? C3A C4A C31A 121.3(6) . . ? C5A C4A C31A 123.1(6) . . ? C6A C5A C4A 122.6(6) . . ? C5A C6A C1A 119.9(6) . . ? C5A C6A C30A 121.1(6) . . ? C1A C6A C30A 119.0(6) . . ? N1A C7A C2A 115.4(5) . . ? N1A C9A C10A 112.5(6) . . ? C9A C10A N2A 114.3(6) . . ? N2A C12A C13A 114.0(6) . . ? C12A C13A N3A 110.7(6) . . ? N3A C15A C16A 114.0(5) . . ? C21A C16A C17A 119.3(6) . . ? C21A C16A C15A 121.8(6) . . ? C17A C16A C15A 118.6(6) . . ? C18A C17A C16A 117.7(6) . . ? C18A C17A S2A 121.6(5) . . ? C16A C17A S2A 120.7(5) . . ? C17A C18A C19A 119.7(6) . . ? C17A C18A C22A 117.5(6) . . ? C19A C18A C22A 122.6(6) . . ? C20A C19A C18A 123.1(6) . . ? C21A C20A C19A 114.5(6) . . ? C21A C20A C35A 124.2(6) . . ? C19A C20A C35A 121.3(6) . . ? C16A C21A C20A 124.1(6) . . ? N4A C22A C18A 115.8(6) . . ? N4A C24A C25A 110.4(6) . . ? N5A C25A C24A 113.8(7) . . ? C28A C27A N5A 114.5(6) . . ? C27A C28A N6A 110.1(5) . . ? N6A C30A C6A 115.1(5) . . ? C34A C31A C33A 106.9(9) . . ? C34A C31A C32A 114.0(10) . . ? C33A C31A C32A 103.0(8) . . ? C34A C31A C4A 111.9(6) . . ? C33A C31A C4A 107.4(7) . . ? C32A C31A C4A 112.8(6) . . ? C20A C35A C36A 110.3(7) . . ? C20A C35A C37A 109.3(6) . . ? C36A C35A C37A 109.7(6) . . ? C20A C35A C38A 112.2(6) . . ? C36A C35A C38A 107.8(6) . . ? C37A C35A C38A 107.4(7) . . ? O2A C39A O1A 128.6(6) . . ? O1B Ni1B N2B 163.9(2) . . ? O1B Ni1B N1B 87.52(19) . . ? N2B Ni1B N1B 82.2(2) . . ? O1B Ni1B N3B 87.92(19) . . ? N2B Ni1B N3B 81.2(2) . . ? N1B Ni1B N3B 97.6(2) . . ? O1B Ni1B S2B 94.33(14) . . ? N2B Ni1B S2B 97.70(19) . . ? N1B Ni1B S2B 171.35(16) . . ? N3B Ni1B S2B 90.90(17) . . ? O1B Ni1B S1B 94.85(13) . . ? N2B Ni1B S1B 97.79(17) . . ? N1B Ni1B S1B 91.46(15) . . ? N3B Ni1B S1B 170.63(17) . . ? S2B Ni1B S1B 79.97(7) . . ? O2B Ni2B N5B 164.1(2) . . ? O2B Ni2B N4B 87.39(19) . . ? N5B Ni2B N4B 82.7(2) . . ? O2B Ni2B N6B 88.09(19) . . ? N5B Ni2B N6B 81.0(2) . . ? N4B Ni2B N6B 97.5(2) . . ? O2B Ni2B S1B 94.33(14) . . ? N5B Ni2B S1B 97.27(18) . . ? N4B Ni2B S1B 171.63(15) . . ? N6B Ni2B S1B 90.74(16) . . ? O2B Ni2B S2B 95.32(13) . . ? N5B Ni2B S2B 97.36(18) . . ? N4B Ni2B S2B 91.72(15) . . ? N6B Ni2B S2B 170.31(16) . . ? S1B Ni2B S2B 79.97(7) . . ? C1B S1B Ni2B 101.8(2) . . ? C1B S1B Ni1B 101.1(2) . . ? Ni2B S1B Ni1B 88.62(7) . . ? C17B S2B Ni1B 102.4(2) . . ? C17B S2B Ni2B 101.4(2) . . ? Ni1B S2B Ni2B 89.22(7) . . ? C39B O1B Ni1B 134.4(4) . . ? C39B O2B Ni2B 133.8(4) . . ? C8B N1B C9B 109.4(6) . . ? C8B N1B C7B 107.0(5) . . ? C9B N1B C7B 106.7(6) . . ? C8B N1B Ni1B 116.3(4) . . ? C9B N1B Ni1B 105.6(4) . . ? C7B N1B Ni1B 111.5(4) . . ? C10B N2B C12B 111.8(6) . . ? C10B N2B C11B 108.7(7) . . ? C12B N2B C11B 109.5(6) . . ? C10B N2B Ni1B 107.2(4) . . ? C12B N2B Ni1B 107.5(4) . . ? C11B N2B Ni1B 112.1(5) . . ? C14B N3B C13B 108.6(6) . . ? C14B N3B C15B 107.8(6) . . ? C13B N3B C15B 107.2(5) . . ? C14B N3B Ni1B 117.0(4) . . ? C13B N3B Ni1B 105.2(4) . . ? C15B N3B Ni1B 110.5(4) . . ? C24B N4B C23B 109.6(6) . . ? C24B N4B C22B 108.7(6) . . ? C23B N4B C22B 106.8(5) . . ? C24B N4B Ni2B 104.4(4) . . ? C23B N4B Ni2B 116.6(4) . . ? C22B N4B Ni2B 110.5(4) . . ? C27B N5B C26B 108.9(6) . . ? C27B N5B C25B 111.3(6) . . ? C26B N5B C25B 107.4(7) . . ? C27B N5B Ni2B 108.9(4) . . ? C26B N5B Ni2B 112.5(5) . . ? C25B N5B Ni2B 107.9(4) . . ? C29B N6B C28B 110.9(6) . . ? C29B N6B C30B 108.0(6) . . ? C28B N6B C30B 105.7(5) . . ? C29B N6B Ni2B 117.4(4) . . ? C28B N6B Ni2B 104.9(4) . . ? C30B N6B Ni2B 109.3(4) . . ? C2B C1B C6B 116.8(6) . . ? C2B C1B S1B 121.5(5) . . ? C6B C1B S1B 121.7(5) . . ? C3B C2B C1B 120.0(6) . . ? C3B C2B C7B 121.7(6) . . ? C1B C2B C7B 118.3(6) . . ? C4B C3B C2B 122.9(6) . . ? C3B C4B C5B 115.6(6) . . ? C3B C4B C31B 123.1(6) . . ? C5B C4B C31B 121.3(6) . . ? C6B C5B C4B 123.4(6) . . ? C5B C6B C1B 119.7(6) . . ? C5B C6B C30B 123.0(6) . . ? C1B C6B C30B 117.0(6) . . ? N1B C7B C2B 114.0(5) . . ? N1B C9B C10B 110.9(7) . . ? N2B C10B C9B 114.8(7) . . ? N2B C12B C13B 113.7(6) . . ? N3B C13B C12B 109.7(6) . . ? N3B C15B C16B 116.5(5) . . ? C21B C16B C17B 120.1(6) . . ? C21B C16B C15B 120.2(6) . . ? C17B C16B C15B 119.6(6) . . ? C18B C17B C16B 118.2(6) . . ? C18B C17B S2B 121.2(5) . . ? C16B C17B S2B 120.6(5) . . ? C17B C18B C19B 119.6(6) . . ? C17B C18B C22B 118.9(6) . . ? C19B C18B C22B 121.2(6) . . ? C18B C19B C20B 122.4(7) . . ? C21B C20B C19B 116.3(6) . . ? C21B C20B C35B 121.7(6) . . ? C19B C20B C35B 121.9(6) . . ? C20B C21B C16B 122.3(6) . . ? N4B C22B C18B 115.0(6) . . ? N4B C24B C25B 111.8(7) . . ? N5B C25B C24B 113.9(6) . . ? N5B C27B C28B 113.2(6) . . ? N6B C28B C27B 111.0(6) . . ? C6B C30B N6B 116.2(5) . . ? C34B C31B C4B 110.5(6) . . ? C34B C31B C32B 110.1(5) . . ? C4B C31B C32B 109.0(5) . . ? C34B C31B C33B 108.1(5) . . ? C4B C31B C33B 112.0(5) . . ? C32B C31B C33B 107.0(6) . . ? C36B C35B C38B 109.5(7) . . ? C36B C35B C37B 107.3(7) . . ? C38B C35B C37B 109.9(8) . . ? C36B C35B C20B 111.1(6) . . ? C38B C35B C20B 107.1(7) . . ? C37B C35B C20B 112.1(6) . . ? O1B C39B O2B 127.3(6) . . ? C301 B1 C201 112.5(5) . . ? C301 B1 C401 110.0(5) . . ? C201 B1 C401 107.0(6) . . ? C301 B1 C101 102.4(5) . . ? C201 B1 C101 112.3(5) . . ? C401 B1 C101 112.6(5) . . ? C102 C101 C106 113.9(6) . . ? C102 C101 B1 125.4(6) . . ? C106 C101 B1 120.5(6) . . ? C103 C102 C101 124.3(7) . . ? C104 C103 C102 119.5(7) . . ? C103 C104 C105 118.6(7) . . ? C106 C105 C104 121.1(8) . . ? C105 C106 C101 122.5(7) . . ? C202 C201 C206 114.5(6) . . ? C202 C201 B1 123.2(6) . . ? C206 C201 B1 122.2(6) . . ? C203 C202 C201 122.7(7) . . ? C204 C203 C202 121.3(8) . . ? C203 C204 C205 117.8(7) . . ? C206 C205 C204 120.2(7) . . ? C205 C206 C201 123.5(7) . . ? C302 C301 C306 114.0(6) . . ? C302 C301 B1 122.8(6) . . ? C306 C301 B1 123.1(6) . . ? C303 C302 C301 123.4(7) . . ? C304 C303 C302 120.5(7) . . ? C303 C304 C305 119.0(6) . . ? C306 C305 C304 119.2(7) . . ? C305 C306 C301 123.9(7) . . ? C402 C401 C406 112.8(6) . . ? C402 C401 B1 127.3(6) . . ? C406 C401 B1 119.8(6) . . ? C401 C402 C403 124.4(7) . . ? C404 C403 C402 119.5(7) . . ? C405 C404 C403 118.6(7) . . ? C404 C405 C406 120.9(8) . . ? C405 C406 C401 123.7(7) . . ? C701 B2 C801 112.6(5) . . ? C701 B2 C501 104.6(5) . . ? C801 B2 C501 111.9(5) . . ? C701 B2 C601 112.2(5) . . ? C801 B2 C601 105.0(5) . . ? C501 B2 C601 110.6(5) . . ? C502 C501 C506 115.4(6) . . ? C502 C501 B2 121.7(6) . . ? C506 C501 B2 122.7(6) . . ? C501 C502 C503 122.5(7) . . ? C504 C503 C502 119.4(7) . . ? C503 C504 C505 119.3(7) . . ? C504 C505 C506 120.2(7) . . ? C505 C506 C501 123.0(7) . . ? C606 C601 C602 114.4(6) . . ? C606 C601 B2 120.9(6) . . ? C602 C601 B2 124.6(6) . . ? C603 C602 C601 123.0(7) . . ? C604 C603 C602 120.2(8) . . ? C605 C604 C603 118.2(8) . . ? C604 C605 C606 121.0(8) . . ? C605 C606 C601 123.2(7) . . ? C702 C701 C706 113.7(7) . . ? C702 C701 B2 124.7(6) . . ? C706 C701 B2 121.5(6) . . ? C703 C702 C701 124.2(8) . . ? C702 C703 C704 119.2(8) . . ? C705 C704 C703 117.9(8) . . ? C706 C705 C704 121.8(9) . . ? C705 C706 C701 123.1(8) . . ? C802 C801 C806 113.7(7) . . ? C802 C801 B2 124.7(6) . . ? C806 C801 B2 121.5(6) . . ? C801 C802 C803 122.6(7) . . ? C804 C803 C802 120.8(9) . . ? C805 C804 C803 118.6(8) . . ? C804 C805 C806 121.4(8) . . ? C805 C806 C801 122.9(8) . . ?