# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Yan-wei Ren' _publ_contact_author_email renyw@scut.edu.cn loop_ _publ_author_name 'Huanfeng Jiang.' 'Yan-wei Ren.' 'Bowei Cai.' 'Dabin Shi.' 'Jiaxian Lu.' ; Jun Chen ; 'De Zheng.' 'Bin Liu.' # Attachment 'complex-2.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 789253' #TrackingRef 'complex-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H58 B Br N10 Ni2 O13' _chemical_formula_weight 1359.32 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.222(3) _cell_length_b 25.914(5) _cell_length_c 19.506(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.11(3) _cell_angle_gamma 90.00 _cell_volume 6387(2) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2800 _exptl_absorpt_coefficient_mu 1.285 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6992 _exptl_absorpt_correction_T_max 0.7832 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48779 _diffrn_reflns_av_R_equivalents 0.0837 _diffrn_reflns_av_sigmaI/netI 0.0695 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11227 _reflns_number_gt 5727 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1061P)^2^+1.2798P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0021(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11227 _refine_ls_number_parameters 803 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1333 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.2095 _refine_ls_wR_factor_gt 0.1705 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.13860(6) 0.65564(3) 0.28097(4) 0.0673(3) Uani 1 1 d . . . Ni2 Ni -0.03778(6) 0.56274(3) 0.19197(4) 0.0722(3) Uani 1 1 d . . . Br1 Br 0.42023(7) 0.52886(4) 0.06493(5) 0.1181(4) Uani 1 1 d . . . O2 O -0.0036(3) 0.69202(14) 0.2287(2) 0.0793(11) Uani 1 1 d . . . O1 O 0.1023(3) 0.59747(13) 0.2110(2) 0.0691(10) Uani 1 1 d . . . O3 O -0.1205(3) 0.62686(15) 0.1989(2) 0.0806(11) Uani 1 1 d . . . C6 C 0.1960(5) 0.5305(2) 0.1760(3) 0.0761(16) Uani 1 1 d . . . C1 C 0.1705(5) 0.5827(2) 0.1766(3) 0.0685(15) Uani 1 1 d . . . C2 C 0.2162(5) 0.6181(2) 0.1405(3) 0.0701(15) Uani 1 1 d . . . C5 C 0.2690(5) 0.5145(3) 0.1409(4) 0.0859(18) Uani 1 1 d . . . H5A H 0.2871 0.4798 0.1407 0.103 Uiso 1 1 calc R . . C3 C 0.2874(5) 0.6017(3) 0.1059(3) 0.0814(17) Uani 1 1 d . . . H3A H 0.3178 0.6253 0.0820 0.098 Uiso 1 1 calc R . . C4 C 0.3134(5) 0.5502(3) 0.1069(3) 0.0835(18) Uani 1 1 d . . . N1 N 0.2219(4) 0.69146(16) 0.2185(3) 0.0731(13) Uani 1 1 d . . . H1A H 0.2911 0.6826 0.2377 0.088 Uiso 1 1 calc R . . O5 O -0.0221(3) 0.55358(15) 0.3013(2) 0.0821(12) Uani 1 1 d . . . N3 N 0.0299(4) 0.49077(18) 0.1857(3) 0.0797(14) Uani 1 1 d . . . O4 O 0.0634(3) 0.62622(15) 0.3486(2) 0.0822(12) Uani 1 1 d . . . N2 N 0.1726(4) 0.72576(18) 0.3384(3) 0.0762(13) Uani 1 1 d . . . H2A H 0.1100 0.7431 0.3255 0.091 Uiso 1 1 calc R . . N4 N -0.1681(5) 0.5093(2) 0.1659(4) 0.1016(18) Uani 1 1 d . . . N5 N 0.2724(5) 0.6170(2) 0.3438(3) 0.0804(14) Uani 1 1 d . . . C9 C 0.2430(5) 0.7573(2) 0.3078(4) 0.0792(17) Uani 1 1 d . . . H9A H 0.3154 0.7447 0.3291 0.095 Uiso 1 1 calc R . . C8 C 0.2147(5) 0.7472(2) 0.2290(3) 0.0804(17) Uani 1 1 d . . . H8A H 0.1434 0.7592 0.2055 0.096 Uiso 1 1 calc R . . H8B H 0.2631 0.7654 0.2085 0.096 Uiso 1 1 calc R . . C10 C 0.2410(6) 0.8128(2) 0.3300(4) 0.099(2) Uani 1 1 d . . . H10A H 0.1697 0.8264 0.3115 0.119 Uiso 1 1 calc R . . H10B H 0.2871 0.8332 0.3101 0.119 Uiso 1 1 calc R . . C11 C 0.2775(6) 0.8171(3) 0.4118(5) 0.114(3) Uani 1 1 d . . . H11A H 0.3510 0.8068 0.4299 0.137 Uiso 1 1 calc R . . H11B H 0.2718 0.8526 0.4258 0.137 Uiso 1 1 calc R . . N6 N -0.0708(5) 0.5868(2) 0.0818(3) 0.0960(18) Uani 1 1 d . . . C7 C 0.1904(5) 0.6741(2) 0.1439(3) 0.0800(17) Uani 1 1 d . . . H7A H 0.2275 0.6942 0.1168 0.096 Uiso 1 1 calc R . . H7B H 0.1151 0.6794 0.1227 0.096 Uiso 1 1 calc R . . C14 C 0.1480(5) 0.4938(2) 0.2160(3) 0.0802(17) Uani 1 1 d . . . H14A H 0.1658 0.5045 0.2658 0.096 Uiso 1 1 calc R . . H14B H 0.1779 0.4597 0.2147 0.096 Uiso 1 1 calc R . . C19 C -0.1319(7) 0.4660(3) 0.2187(4) 0.108(2) Uani 1 1 d . . . H19A H -0.1720 0.4351 0.2005 0.129 Uiso 1 1 calc R . . H19B H -0.1443 0.4751 0.2638 0.129 Uiso 1 1 calc R . . C15 C 0.0028(6) 0.4711(3) 0.1104(4) 0.101(2) Uani 1 1 d . . . H15A H 0.0133 0.4987 0.0797 0.122 Uiso 1 1 calc R . . H15B H 0.0517 0.4436 0.1085 0.122 Uiso 1 1 calc R . . C16 C -0.1058(7) 0.4515(3) 0.0814(5) 0.119(3) Uani 1 1 d . . . H16A H -0.1108 0.4184 0.1034 0.142 Uiso 1 1 calc R . . H16B H -0.1201 0.4458 0.0303 0.142 Uiso 1 1 calc R . . C18 C -0.0121(6) 0.4558(2) 0.2310(4) 0.092(2) Uani 1 1 d . . . H18A H 0.0260 0.4614 0.2812 0.110 Uiso 1 1 calc R . . H18B H -0.0017 0.4202 0.2193 0.110 Uiso 1 1 calc R . . C17 C -0.1893(8) 0.4866(3) 0.0930(5) 0.122(3) Uani 1 1 d . . . H17A H -0.1998 0.5147 0.0587 0.146 Uiso 1 1 calc R . . H17B H -0.2552 0.4675 0.0823 0.146 Uiso 1 1 calc R . . C27 C -0.2892(5) 0.6950(2) 0.1850(3) 0.0737(16) Uani 1 1 d . . . H27A H -0.3064 0.6620 0.1666 0.088 Uiso 1 1 calc R . . C24 C -0.2418(6) 0.7919(2) 0.2393(3) 0.0769(17) Uani 1 1 d . . . C22 C -0.1834(5) 0.7099(2) 0.2122(3) 0.0678(15) Uani 1 1 d . . . C23 C -0.1599(5) 0.7597(2) 0.2392(3) 0.0725(16) Uani 1 1 d . . . H23A H -0.0901 0.7708 0.2567 0.087 Uiso 1 1 calc R . . C21 C -0.0951(5) 0.6726(3) 0.2133(3) 0.0741(16) Uani 1 1 d . . . C25 C -0.3453(6) 0.7780(3) 0.2121(3) 0.0812(17) Uani 1 1 d . . . H25A H -0.3993 0.8011 0.2116 0.097 Uiso 1 1 calc R . . C26 C -0.3672(5) 0.7296(2) 0.1858(3) 0.0728(16) Uani 1 1 d . . . C13 C 0.2066(6) 0.7279(2) 0.4169(4) 0.093(2) Uani 1 1 d . . . H13A H 0.2760 0.7123 0.4351 0.111 Uiso 1 1 calc R . . H13B H 0.1576 0.7084 0.4352 0.111 Uiso 1 1 calc R . . C12 C 0.2112(7) 0.7834(3) 0.4435(4) 0.115(3) Uani 1 1 d . . . H12A H 0.1400 0.7973 0.4314 0.138 Uiso 1 1 calc R . . H12B H 0.2401 0.7838 0.4954 0.138 Uiso 1 1 calc R . . C20 C -0.2626(7) 0.5316(3) 0.1755(6) 0.148(4) Uani 1 1 d . . . H20A H -0.3187 0.5066 0.1632 0.221 Uiso 1 1 calc R . . H20B H -0.2827 0.5613 0.1450 0.221 Uiso 1 1 calc R . . H20C H -0.2496 0.5418 0.2246 0.221 Uiso 1 1 calc R . . O8 O -0.4966(4) 0.6753(2) 0.1218(3) 0.1157(17) Uani 1 1 d . . . N9 N -0.2134(7) 0.8425(2) 0.2733(4) 0.1011(18) Uani 1 1 d . . . O9 O -0.5449(4) 0.7411(2) 0.1705(3) 0.1154(17) Uani 1 1 d . . . O7 O -0.2855(5) 0.87199(19) 0.2748(3) 0.1239(19) Uani 1 1 d . . . N10 N -0.4791(5) 0.7146(3) 0.1565(3) 0.0934(16) Uani 1 1 d . . . O6 O -0.1198(6) 0.8519(2) 0.3018(4) 0.130(2) Uani 1 1 d . . . C30 C 0.0115(5) 0.5863(3) 0.3497(3) 0.0750(16) Uani 1 1 d . . . C31 C -0.0128(5) 0.5773(2) 0.4206(4) 0.0794(17) Uani 1 1 d . . . C36 C -0.0920(5) 0.5437(2) 0.4256(4) 0.0838(18) Uani 1 1 d . . . H36A H -0.1296 0.5241 0.3865 0.101 Uiso 1 1 calc R . . C34 C -0.0598(8) 0.5677(3) 0.5501(5) 0.113(3) Uani 1 1 d . . . H34A H -0.0765 0.5655 0.5931 0.136 Uiso 1 1 calc R . . C32 C 0.0422(6) 0.6042(2) 0.4804(4) 0.091(2) Uani 1 1 d . . . H32A H 0.0958 0.6267 0.4779 0.110 Uiso 1 1 calc R . . C35 C -0.1134(6) 0.5404(3) 0.4912(5) 0.096(2) Uani 1 1 d . . . C33 C 0.0193(8) 0.5983(3) 0.5428(4) 0.110(3) Uani 1 1 d . . . B1 B 0.6433(6) 0.7045(3) 0.4476(4) 0.0769(19) Uani 1 1 d . . . C39 C 0.6122(5) 0.6639(2) 0.3792(3) 0.0764(16) Uani 1 1 d . . . C40 C 0.5173(5) 0.6632(3) 0.3266(4) 0.0901(19) Uani 1 1 d . . . H40A H 0.4689 0.6893 0.3265 0.108 Uiso 1 1 calc R . . C45 C 0.7713(5) 0.7133(2) 0.4732(3) 0.0806(17) Uani 1 1 d . . . C41 C 0.4893(6) 0.6265(3) 0.2742(4) 0.107(2) Uani 1 1 d . . . H41A H 0.4235 0.6282 0.2399 0.128 Uiso 1 1 calc R . . C50 C 0.8302(6) 0.7219(3) 0.5438(4) 0.0881(19) Uani 1 1 d . . . H50A H 0.7966 0.7196 0.5794 0.106 Uiso 1 1 calc R . . C42 C 0.5552(7) 0.5883(4) 0.2719(4) 0.121(3) Uani 1 1 d . . . H42A H 0.5362 0.5637 0.2356 0.145 Uiso 1 1 calc R . . C47 C 0.9338(6) 0.7301(3) 0.4408(4) 0.112(3) Uani 1 1 d . . . H47A H 0.9682 0.7325 0.4056 0.135 Uiso 1 1 calc R . . C46 C 0.8288(6) 0.7187(3) 0.4230(4) 0.100(2) Uani 1 1 d . . . H46A H 0.7926 0.7143 0.3747 0.121 Uiso 1 1 calc R . . C48 C 0.9889(6) 0.7380(3) 0.5129(5) 0.104(2) Uani 1 1 d . . . H48A H 1.0606 0.7462 0.5262 0.125 Uiso 1 1 calc R . . C44 C 0.6766(6) 0.6230(3) 0.3762(4) 0.119(3) Uani 1 1 d . . . H44A H 0.7411 0.6201 0.4117 0.142 Uiso 1 1 calc R . . C43 C 0.6501(7) 0.5854(4) 0.3226(5) 0.149(4) Uani 1 1 d . . . H43A H 0.6969 0.5588 0.3218 0.178 Uiso 1 1 calc R . . C51 C 0.5951(5) 0.7623(3) 0.4286(4) 0.0857(19) Uani 1 1 d . . . C52 C 0.5641(7) 0.7847(3) 0.3612(4) 0.107(2) Uani 1 1 d . . . H52A H 0.5642 0.7645 0.3218 0.129 Uiso 1 1 calc R . . C49 C 0.9376(6) 0.7338(3) 0.5636(4) 0.099(2) Uani 1 1 d . . . H49A H 0.9744 0.7389 0.6117 0.119 Uiso 1 1 calc R . . C56 C 0.5936(6) 0.7971(3) 0.4830(4) 0.104(2) Uani 1 1 d . . . H56A H 0.6140 0.7844 0.5297 0.125 Uiso 1 1 calc R . . C54 C 0.5344(8) 0.8677(3) 0.4063(7) 0.128(3) Uani 1 1 d . . . H54A H 0.5150 0.9022 0.3986 0.153 Uiso 1 1 calc R . . C53 C 0.5329(8) 0.8358(4) 0.3495(6) 0.130(3) Uani 1 1 d . . . H53A H 0.5107 0.8487 0.3030 0.156 Uiso 1 1 calc R . . C57 C 0.6021(6) 0.6757(3) 0.5080(3) 0.0816(17) Uani 1 1 d . . . C58 C 0.5027(6) 0.6856(3) 0.5182(4) 0.100(2) Uani 1 1 d . . . H58A H 0.4628 0.7125 0.4922 0.119 Uiso 1 1 calc R . . C38 C 0.4281(6) 0.5598(3) 0.4201(4) 0.111(2) Uani 1 1 d . . . C28 C -0.1088(6) 0.6117(3) 0.0327(4) 0.093(2) Uani 1 1 d . . . C37 C 0.3393(6) 0.5920(3) 0.3769(4) 0.0828(18) Uani 1 1 d . . . C55 C 0.5650(8) 0.8478(4) 0.4743(6) 0.127(3) Uani 1 1 d . . . H55A H 0.5662 0.8683 0.5136 0.152 Uiso 1 1 calc R . . C29 C -0.1618(8) 0.6423(3) -0.0318(4) 0.127(3) Uani 1 1 d . . . O10 O -0.2419(7) 0.4788(3) 0.4423(5) 0.170(3) Uani 1 1 d U . . O12 O 0.1525(8) 0.6485(3) 0.6031(4) 0.166(3) Uani 1 1 d U . . N8 N -0.1980(8) 0.5047(4) 0.4936(6) 0.140(3) Uani 1 1 d U . . N7 N 0.0761(11) 0.6255(3) 0.6073(6) 0.166(4) Uani 1 1 d U . . O11 O -0.2173(6) 0.5021(3) 0.5523(5) 0.177(3) Uani 1 1 d U . . C62 C 0.6576(7) 0.6348(3) 0.5492(4) 0.102(2) Uani 1 1 d . . . H62A H 0.7244 0.6270 0.5455 0.123 Uiso 1 1 calc R . . O13 O 0.0471(10) 0.6258(3) 0.6599(4) 0.246(6) Uani 1 1 d U . . C59 C 0.4610(8) 0.6588(4) 0.5630(5) 0.125(3) Uani 1 1 d . . . H59A H 0.3949 0.6673 0.5675 0.150 Uiso 1 1 calc R . . C60 C 0.5196(11) 0.6181(5) 0.6023(6) 0.142(4) Uani 1 1 d . . . H60A H 0.4925 0.5991 0.6334 0.171 Uiso 1 1 calc R . . C61 C 0.6192(9) 0.6056(3) 0.5950(5) 0.126(3) Uani 1 1 d . . . H61A H 0.6582 0.5782 0.6204 0.151 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0541(5) 0.0672(4) 0.0758(5) 0.0023(4) 0.0115(4) -0.0064(3) Ni2 0.0609(5) 0.0695(5) 0.0807(5) -0.0007(4) 0.0122(4) -0.0085(4) Br1 0.0928(6) 0.1518(8) 0.1178(6) -0.0374(5) 0.0435(5) -0.0094(5) O2 0.056(3) 0.075(2) 0.098(3) 0.002(2) 0.008(2) -0.005(2) O1 0.057(2) 0.069(2) 0.080(3) -0.0003(19) 0.019(2) -0.0052(19) O3 0.062(3) 0.072(3) 0.100(3) -0.008(2) 0.013(2) -0.012(2) C6 0.068(4) 0.074(4) 0.078(4) -0.001(3) 0.009(3) -0.007(3) C1 0.056(4) 0.071(4) 0.072(4) -0.003(3) 0.009(3) -0.006(3) C2 0.062(4) 0.073(4) 0.064(3) -0.004(3) 0.002(3) -0.005(3) C5 0.073(5) 0.091(4) 0.092(5) -0.019(4) 0.021(4) -0.001(4) C3 0.061(4) 0.107(5) 0.071(4) -0.008(4) 0.012(3) -0.015(4) C4 0.065(4) 0.099(5) 0.082(4) -0.013(4) 0.015(3) -0.008(4) N1 0.062(3) 0.068(3) 0.082(3) 0.001(2) 0.010(3) -0.003(2) O5 0.081(3) 0.077(3) 0.088(3) -0.002(2) 0.024(2) -0.016(2) N3 0.085(4) 0.070(3) 0.079(3) -0.004(3) 0.016(3) -0.013(3) O4 0.082(3) 0.081(3) 0.088(3) -0.006(2) 0.032(2) -0.020(2) N2 0.061(3) 0.079(3) 0.087(4) -0.006(3) 0.019(3) -0.006(2) N4 0.069(4) 0.095(4) 0.132(5) -0.015(4) 0.016(4) -0.010(3) N5 0.067(4) 0.083(3) 0.085(4) 0.003(3) 0.014(3) -0.006(3) C9 0.060(4) 0.069(4) 0.107(5) 0.002(3) 0.022(4) -0.009(3) C8 0.077(5) 0.072(4) 0.087(4) 0.004(3) 0.017(4) -0.008(3) C10 0.089(5) 0.071(4) 0.132(6) -0.012(4) 0.026(5) -0.010(4) C11 0.092(6) 0.101(5) 0.150(8) -0.042(5) 0.036(6) -0.022(5) N6 0.091(5) 0.088(4) 0.095(4) 0.001(3) 0.005(4) -0.004(3) C7 0.066(4) 0.092(4) 0.075(4) 0.013(3) 0.010(3) -0.005(3) C14 0.076(5) 0.070(4) 0.089(4) 0.002(3) 0.015(4) 0.006(3) C19 0.116(7) 0.099(5) 0.112(6) -0.010(5) 0.041(5) -0.023(5) C15 0.096(6) 0.089(5) 0.106(5) -0.004(4) 0.009(4) -0.016(4) C16 0.116(7) 0.111(6) 0.121(6) -0.020(5) 0.022(6) -0.036(6) C18 0.090(6) 0.072(4) 0.119(6) 0.005(4) 0.040(4) -0.011(4) C17 0.121(8) 0.103(6) 0.116(6) -0.017(5) -0.006(5) -0.027(5) C27 0.059(4) 0.075(4) 0.084(4) 0.003(3) 0.016(3) -0.003(3) C24 0.077(5) 0.066(4) 0.089(4) 0.008(3) 0.026(4) -0.003(3) C22 0.060(4) 0.069(4) 0.070(4) 0.009(3) 0.012(3) 0.002(3) C23 0.063(4) 0.080(4) 0.067(4) 0.007(3) 0.008(3) -0.008(3) C21 0.051(4) 0.086(4) 0.077(4) 0.009(3) 0.006(3) -0.001(3) C25 0.069(5) 0.087(4) 0.089(4) 0.013(4) 0.025(4) 0.008(4) C26 0.057(4) 0.085(4) 0.076(4) 0.005(3) 0.020(3) 0.000(3) C13 0.085(5) 0.092(5) 0.106(5) -0.019(4) 0.035(4) -0.019(4) C12 0.118(7) 0.107(5) 0.126(6) -0.037(5) 0.047(5) -0.028(5) C20 0.089(7) 0.129(7) 0.233(12) -0.007(7) 0.061(7) -0.016(6) O8 0.071(4) 0.131(4) 0.137(4) -0.027(4) 0.018(3) -0.030(3) N9 0.105(6) 0.076(4) 0.128(5) -0.005(4) 0.043(5) -0.009(4) O9 0.063(3) 0.133(4) 0.151(5) 0.008(3) 0.034(3) 0.014(3) O7 0.118(5) 0.082(3) 0.175(5) -0.017(3) 0.050(4) 0.008(3) N10 0.060(4) 0.110(5) 0.104(4) 0.008(4) 0.015(3) -0.010(4) O6 0.106(5) 0.103(4) 0.180(6) -0.038(4) 0.039(4) -0.029(4) C30 0.067(4) 0.077(4) 0.077(4) 0.001(4) 0.014(3) -0.002(3) C31 0.082(5) 0.063(3) 0.092(5) 0.005(3) 0.023(4) 0.000(3) C36 0.078(5) 0.070(4) 0.102(5) 0.013(3) 0.024(4) 0.005(3) C34 0.156(9) 0.100(6) 0.099(6) 0.013(5) 0.062(6) 0.023(6) C32 0.115(6) 0.079(4) 0.082(5) 0.011(4) 0.032(4) -0.009(4) C35 0.095(6) 0.088(5) 0.118(6) 0.034(5) 0.050(5) 0.014(4) C33 0.170(9) 0.078(5) 0.083(5) -0.001(4) 0.036(6) -0.022(5) B1 0.059(5) 0.097(5) 0.070(4) -0.008(4) 0.011(4) -0.006(4) C39 0.059(4) 0.098(4) 0.068(4) -0.006(3) 0.013(3) -0.003(3) C40 0.058(4) 0.117(5) 0.085(4) -0.019(4) 0.006(4) 0.003(4) C45 0.063(4) 0.099(4) 0.071(4) -0.002(3) 0.007(3) -0.009(3) C41 0.069(5) 0.142(7) 0.092(5) -0.029(5) -0.004(4) 0.006(5) C50 0.070(5) 0.109(5) 0.080(4) -0.016(4) 0.013(4) -0.013(4) C42 0.089(6) 0.154(7) 0.102(6) -0.045(5) 0.000(5) 0.012(6) C47 0.074(6) 0.159(7) 0.102(6) -0.011(5) 0.025(5) -0.021(5) C46 0.065(5) 0.147(6) 0.083(5) 0.006(4) 0.011(4) -0.018(4) C48 0.064(5) 0.123(6) 0.117(6) -0.013(5) 0.014(5) -0.022(4) C44 0.074(5) 0.146(7) 0.108(6) -0.052(5) -0.018(4) 0.027(5) C43 0.099(7) 0.171(8) 0.141(7) -0.068(7) -0.020(6) 0.045(6) C51 0.060(4) 0.095(5) 0.100(5) -0.020(4) 0.021(4) -0.008(3) C52 0.123(7) 0.103(6) 0.105(6) 0.015(5) 0.047(5) 0.009(5) C49 0.076(5) 0.128(6) 0.082(5) -0.018(4) 0.004(4) -0.015(4) C56 0.093(6) 0.106(6) 0.107(6) -0.009(5) 0.017(4) 0.001(5) C54 0.122(8) 0.095(6) 0.184(10) -0.004(7) 0.073(8) -0.004(5) C53 0.146(9) 0.117(7) 0.149(8) 0.031(6) 0.077(7) 0.018(6) C57 0.071(5) 0.092(4) 0.079(4) -0.014(4) 0.017(4) -0.011(4) C58 0.081(5) 0.127(6) 0.091(5) -0.002(4) 0.026(4) -0.023(5) C38 0.083(6) 0.103(5) 0.127(6) 0.027(5) -0.003(5) 0.013(4) C28 0.085(6) 0.088(5) 0.103(6) -0.022(4) 0.024(5) -0.003(4) C37 0.072(5) 0.081(4) 0.092(5) 0.000(4) 0.018(4) -0.008(4) C55 0.122(8) 0.105(7) 0.154(9) -0.016(6) 0.040(7) -0.004(6) C29 0.156(9) 0.121(6) 0.089(5) 0.024(5) 0.010(5) 0.044(6) O10 0.147(7) 0.174(7) 0.198(8) 0.040(6) 0.064(6) -0.064(5) O12 0.226(10) 0.148(6) 0.099(5) -0.017(4) 0.006(5) -0.015(6) N8 0.129(8) 0.135(7) 0.177(10) 0.052(6) 0.074(7) 0.006(6) N7 0.274(15) 0.105(6) 0.113(7) 0.005(5) 0.046(9) -0.041(7) O11 0.183(7) 0.193(6) 0.201(7) 0.066(6) 0.127(6) 0.007(5) C62 0.100(6) 0.109(5) 0.101(5) -0.005(5) 0.037(5) -0.019(5) O13 0.479(18) 0.183(7) 0.096(5) 0.000(5) 0.117(8) -0.073(8) C59 0.119(8) 0.147(8) 0.120(7) -0.008(6) 0.054(6) -0.030(7) C60 0.172(12) 0.153(9) 0.121(8) -0.025(7) 0.071(8) -0.066(8) C61 0.153(10) 0.112(6) 0.111(6) -0.002(5) 0.039(7) -0.017(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 O1 1.995(4) . ? Ni1 O4 2.020(4) . ? Ni1 O2 2.082(4) . ? Ni1 N5 2.088(6) . ? Ni1 N1 2.085(5) . ? Ni1 N2 2.112(5) . ? Ni2 O1 1.993(4) . ? Ni2 O3 2.016(4) . ? Ni2 N3 2.088(5) . ? Ni2 O5 2.094(4) . ? Ni2 N4 2.152(6) . ? Ni2 N6 2.155(7) . ? Br1 C4 1.911(7) . ? O2 C21 1.262(7) . ? O1 C1 1.327(6) . ? O3 C21 1.242(7) . ? C6 C1 1.396(8) . ? C6 C5 1.399(8) . ? C6 C14 1.486(8) . ? C1 C2 1.398(8) . ? C2 C3 1.377(8) . ? C2 C7 1.497(8) . ? C5 C4 1.367(9) . ? C5 H5A 0.9300 . ? C3 C4 1.377(9) . ? C3 H3A 0.9300 . ? N1 C7 1.461(7) . ? N1 C8 1.466(7) . ? N1 H1A 0.9100 . ? O5 C30 1.249(7) . ? N3 C18 1.484(7) . ? N3 C15 1.496(8) . ? N3 C14 1.500(8) . ? O4 C30 1.246(7) . ? N2 C13 1.466(8) . ? N2 C9 1.488(7) . ? N2 H2A 0.9100 . ? N4 C20 1.438(9) . ? N4 C17 1.487(9) . ? N4 C19 1.502(9) . ? N5 C37 1.132(8) . ? C9 C8 1.494(8) . ? C9 C10 1.507(8) . ? C9 H9A 0.9800 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C10 C11 1.527(10) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.494(10) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? N6 C28 1.142(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C19 C18 1.553(10) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C15 C16 1.471(10) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.499(11) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C27 C26 1.370(8) . ? C27 C22 1.397(8) . ? C27 H27A 0.9300 . ? C24 C25 1.362(9) . ? C24 C23 1.367(8) . ? C24 N9 1.468(8) . ? C22 C23 1.395(8) . ? C22 C21 1.510(8) . ? C23 H23A 0.9300 . ? C25 C26 1.355(8) . ? C25 H25A 0.9300 . ? C26 N10 1.472(8) . ? C13 C12 1.523(9) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? O8 N10 1.207(7) . ? N9 O6 1.224(8) . ? N9 O7 1.230(7) . ? O9 N10 1.201(7) . ? C30 C31 1.526(8) . ? C31 C32 1.371(9) . ? C31 C36 1.387(8) . ? C36 C35 1.392(9) . ? C36 H36A 0.9300 . ? C34 C33 1.353(11) . ? C34 C35 1.358(11) . ? C34 H34A 0.9300 . ? C32 C33 1.346(9) . ? C32 H32A 0.9300 . ? C35 N8 1.463(11) . ? C33 N7 1.445(12) . ? B1 C51 1.628(10) . ? B1 C57 1.618(10) . ? B1 C45 1.634(9) . ? B1 C39 1.653(9) . ? C39 C40 1.368(9) . ? C39 C44 1.372(9) . ? C40 C41 1.366(9) . ? C40 H40A 0.9300 . ? C45 C50 1.387(8) . ? C45 C46 1.412(9) . ? C41 C42 1.327(10) . ? C41 H41A 0.9300 . ? C50 C49 1.392(9) . ? C50 H50A 0.9300 . ? C42 C43 1.352(11) . ? C42 H42A 0.9300 . ? C47 C46 1.360(9) . ? C47 C48 1.397(10) . ? C47 H47A 0.9300 . ? C46 H46A 0.9300 . ? C48 C49 1.358(9) . ? C48 H48A 0.9300 . ? C44 C43 1.395(10) . ? C44 H44A 0.9300 . ? C43 H43A 0.9300 . ? C51 C52 1.383(9) . ? C51 C56 1.397(9) . ? C52 C53 1.386(10) . ? C52 H52A 0.9300 . ? C49 H49A 0.9300 . ? C56 C55 1.364(10) . ? C56 H56A 0.9300 . ? C54 C55 1.369(12) . ? C54 C53 1.377(12) . ? C54 H54A 0.9300 . ? C53 H53A 0.9300 . ? C57 C62 1.399(10) . ? C57 C58 1.409(9) . ? C58 C59 1.354(10) . ? C58 H58A 0.9300 . ? C38 C37 1.484(10) . ? C28 C29 1.477(11) . ? C55 H55A 0.9300 . ? O10 N8 1.203(11) . ? O12 N7 1.198(12) . ? N8 O11 1.246(10) . ? N7 O13 1.195(11) . ? C62 C61 1.378(10) . ? C62 H62A 0.9300 . ? C59 C60 1.398(13) . ? C59 H59A 0.9300 . ? C60 C61 1.403(13) . ? C60 H60A 0.9300 . ? C61 H61A 0.9300 . ? 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 O1 Ni1 O4 95.52(16) . . ? O1 Ni1 O2 90.36(16) . . ? O4 Ni1 O2 86.76(17) . . ? O1 Ni1 N5 91.76(18) . . ? O4 Ni1 N5 86.02(19) . . ? O2 Ni1 N5 172.64(18) . . ? O1 Ni1 N1 89.92(16) . . ? O4 Ni1 N1 174.52(18) . . ? O2 Ni1 N1 93.92(18) . . ? N5 Ni1 N1 93.1(2) . . ? O1 Ni1 N2 169.56(17) . . ? O4 Ni1 N2 92.74(17) . . ? O2 Ni1 N2 83.73(18) . . ? N5 Ni1 N2 95.2(2) . . ? N1 Ni1 N2 81.94(18) . . ? O1 Ni2 O3 96.21(16) . . ? O1 Ni2 N3 91.33(18) . . ? O3 Ni2 N3 172.23(19) . . ? O1 Ni2 O5 93.08(16) . . ? O3 Ni2 O5 85.32(17) . . ? N3 Ni2 O5 92.45(18) . . ? O1 Ni2 N4 166.0(2) . . ? O3 Ni2 N4 97.7(2) . . ? N3 Ni2 N4 74.8(2) . . ? O5 Ni2 N4 90.0(2) . . ? O1 Ni2 N6 87.6(2) . . ? O3 Ni2 N6 82.7(2) . . ? N3 Ni2 N6 99.5(2) . . ? O5 Ni2 N6 168.0(2) . . ? N4 Ni2 N6 92.2(2) . . ? C21 O2 Ni1 126.9(4) . . ? C1 O1 Ni2 120.5(3) . . ? C1 O1 Ni1 120.0(3) . . ? Ni2 O1 Ni1 119.45(19) . . ? C21 O3 Ni2 133.3(4) . . ? C1 C6 C5 119.7(6) . . ? C1 C6 C14 118.2(6) . . ? C5 C6 C14 122.0(6) . . ? O1 C1 C6 119.1(5) . . ? O1 C1 C2 121.6(5) . . ? C6 C1 C2 119.3(6) . . ? C3 C2 C1 120.2(6) . . ? C3 C2 C7 121.3(6) . . ? C1 C2 C7 118.5(5) . . ? C4 C5 C6 119.5(6) . . ? C4 C5 H5A 120.2 . . ? C6 C5 H5A 120.2 . . ? C4 C3 C2 119.8(6) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C5 C4 C3 121.4(6) . . ? C5 C4 Br1 119.3(5) . . ? C3 C4 Br1 119.1(5) . . ? C7 N1 C8 115.5(5) . . ? C7 N1 Ni1 113.6(4) . . ? C8 N1 Ni1 106.9(4) . . ? C7 N1 H1A 106.8 . . ? C8 N1 H1A 106.8 . . ? Ni1 N1 H1A 106.8 . . ? C30 O5 Ni2 126.8(4) . . ? C18 N3 C15 110.7(5) . . ? C18 N3 C14 109.0(5) . . ? C15 N3 C14 109.0(5) . . ? C18 N3 Ni2 105.5(4) . . ? C15 N3 Ni2 112.3(4) . . ? C14 N3 Ni2 110.2(3) . . ? C30 O4 Ni1 134.8(4) . . ? C13 N2 C9 111.2(5) . . ? C13 N2 Ni1 122.6(4) . . ? C9 N2 Ni1 108.7(3) . . ? C13 N2 H2A 104.1 . . ? C9 N2 H2A 104.1 . . ? Ni1 N2 H2A 104.1 . . ? C20 N4 C17 110.9(7) . . ? C20 N4 C19 108.9(7) . . ? C17 N4 C19 107.1(6) . . ? C20 N4 Ni2 112.1(5) . . ? C17 N4 Ni2 113.1(5) . . ? C19 N4 Ni2 104.3(5) . . ? C37 N5 Ni1 173.6(5) . . ? N2 C9 C8 108.6(5) . . ? N2 C9 C10 110.0(5) . . ? C8 C9 C10 116.3(5) . . ? N2 C9 H9A 107.2 . . ? C8 C9 H9A 107.2 . . ? C10 C9 H9A 107.2 . . ? N1 C8 C9 107.9(5) . . ? N1 C8 H8A 110.1 . . ? C9 C8 H8A 110.1 . . ? N1 C8 H8B 110.1 . . ? C9 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? C9 C10 C11 110.0(6) . . ? C9 C10 H10A 109.7 . . ? C11 C10 H10A 109.7 . . ? C9 C10 H10B 109.7 . . ? C11 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? C12 C11 C10 110.3(6) . . ? C12 C11 H11A 109.6 . . ? C10 C11 H11A 109.6 . . ? C12 C11 H11B 109.6 . . ? C10 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? C28 N6 Ni2 155.6(6) . . ? N1 C7 C2 109.9(5) . . ? N1 C7 H7A 109.7 . . ? C2 C7 H7A 109.7 . . ? N1 C7 H7B 109.7 . . ? C2 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C6 C14 N3 112.5(5) . . ? C6 C14 H14A 109.1 . . ? N3 C14 H14A 109.1 . . ? C6 C14 H14B 109.1 . . ? N3 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? N4 C19 C18 109.8(6) . . ? N4 C19 H19A 109.7 . . ? C18 C19 H19A 109.7 . . ? N4 C19 H19B 109.7 . . ? C18 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? C16 C15 N3 114.9(7) . . ? C16 C15 H15A 108.5 . . ? N3 C15 H15A 108.6 . . ? C16 C15 H15B 108.6 . . ? N3 C15 H15B 108.6 . . ? H15A C15 H15B 107.5 . . ? C15 C16 C17 114.3(7) . . ? C15 C16 H16A 108.7 . . ? C17 C16 H16A 108.7 . . ? C15 C16 H16B 108.7 . . ? C17 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? N3 C18 C19 110.3(6) . . ? N3 C18 H18A 109.6 . . ? C19 C18 H18A 109.6 . . ? N3 C18 H18B 109.6 . . ? C19 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? N4 C17 C16 116.4(7) . . ? N4 C17 H17A 108.2 . . ? C16 C17 H17A 108.2 . . ? N4 C17 H17B 108.2 . . ? C16 C17 H17B 108.2 . . ? H17A C17 H17B 107.3 . . ? C26 C27 C22 119.2(6) . . ? C26 C27 H27A 120.4 . . ? C22 C27 H27A 120.4 . . ? C25 C24 C23 123.0(6) . . ? C25 C24 N9 120.4(7) . . ? C23 C24 N9 116.6(6) . . ? C27 C22 C23 119.1(6) . . ? C27 C22 C21 120.8(5) . . ? C23 C22 C21 120.1(6) . . ? C24 C23 C22 118.4(6) . . ? C24 C23 H23A 120.8 . . ? C22 C23 H23A 120.8 . . ? O3 C21 O2 127.6(6) . . ? O3 C21 C22 116.8(6) . . ? O2 C21 C22 115.6(6) . . ? C26 C25 C24 118.0(6) . . ? C26 C25 H25A 121.0 . . ? C24 C25 H25A 121.0 . . ? C25 C26 C27 122.2(6) . . ? C25 C26 N10 118.0(6) . . ? C27 C26 N10 119.8(6) . . ? N2 C13 C12 111.2(6) . . ? N2 C13 H13A 109.4 . . ? C12 C13 H13A 109.4 . . ? N2 C13 H13B 109.4 . . ? C12 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C11 C12 C13 112.3(6) . . ? C11 C12 H12A 109.1 . . ? C13 C12 H12A 109.1 . . ? C11 C12 H12B 109.1 . . ? C13 C12 H12B 109.1 . . ? H12A C12 H12B 107.9 . . ? N4 C20 H20A 109.5 . . ? N4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O6 N9 O7 123.5(7) . . ? O6 N9 C24 118.3(7) . . ? O7 N9 C24 118.0(7) . . ? O9 N10 O8 125.2(7) . . ? O9 N10 C26 118.3(7) . . ? O8 N10 C26 116.4(6) . . ? O4 C30 O5 128.7(6) . . ? O4 C30 C31 114.0(6) . . ? O5 C30 C31 117.3(6) . . ? C32 C31 C36 118.7(6) . . ? C32 C31 C30 119.6(6) . . ? C36 C31 C30 121.7(6) . . ? C31 C36 C35 117.8(7) . . ? C31 C36 H36A 121.1 . . ? C35 C36 H36A 121.1 . . ? C33 C34 C35 116.3(7) . . ? C33 C34 H34A 121.8 . . ? C35 C34 H34A 121.8 . . ? C33 C32 C31 120.5(7) . . ? C33 C32 H32A 119.7 . . ? C31 C32 H32A 119.7 . . ? C34 C35 C36 123.3(7) . . ? C34 C35 N8 121.1(8) . . ? C36 C35 N8 115.6(9) . . ? C32 C33 C34 123.3(8) . . ? C32 C33 N7 122.4(9) . . ? C34 C33 N7 114.4(9) . . ? C51 B1 C57 113.5(6) . . ? C51 B1 C45 104.0(5) . . ? C57 B1 C45 112.5(5) . . ? C51 B1 C39 114.4(5) . . ? C57 B1 C39 103.7(5) . . ? C45 B1 C39 108.9(5) . . ? C40 C39 C44 113.7(6) . . ? C40 C39 B1 124.7(6) . . ? C44 C39 B1 121.1(6) . . ? C39 C40 C41 123.8(7) . . ? C39 C40 H40A 118.1 . . ? C41 C40 H40A 118.1 . . ? C50 C45 C46 114.4(6) . . ? C50 C45 B1 123.6(6) . . ? C46 C45 B1 121.6(6) . . ? C42 C41 C40 120.7(7) . . ? C42 C41 H41A 119.7 . . ? C40 C41 H41A 119.7 . . ? C45 C50 C49 122.6(6) . . ? C45 C50 H50A 118.7 . . ? C49 C50 H50A 118.7 . . ? C41 C42 C43 119.5(8) . . ? C41 C42 H42A 120.3 . . ? C43 C42 H42A 120.3 . . ? C46 C47 C48 118.6(7) . . ? C46 C47 H47A 120.7 . . ? C48 C47 H47A 120.7 . . ? C47 C46 C45 124.2(7) . . ? C47 C46 H46A 117.9 . . ? C45 C46 H46A 117.9 . . ? C49 C48 C47 119.9(7) . . ? C49 C48 H48A 120.1 . . ? C47 C48 H48A 120.1 . . ? C39 C44 C43 123.3(7) . . ? C39 C44 H44A 118.4 . . ? C43 C44 H44A 118.4 . . ? C42 C43 C44 119.0(8) . . ? C42 C43 H43A 120.5 . . ? C44 C43 H43A 120.5 . . ? C52 C51 C56 112.7(7) . . ? C52 C51 B1 126.1(6) . . ? C56 C51 B1 120.8(7) . . ? C51 C52 C53 123.2(8) . . ? C51 C52 H52A 118.4 . . ? C53 C52 H52A 118.4 . . ? C48 C49 C50 120.2(7) . . ? C48 C49 H49A 119.9 . . ? C50 C49 H49A 119.9 . . ? C55 C56 C51 126.2(8) . . ? C55 C56 H56A 116.9 . . ? C51 C56 H56A 116.9 . . ? C55 C54 C53 118.8(9) . . ? C55 C54 H54A 120.6 . . ? C53 C54 H54A 120.6 . . ? C54 C53 C52 120.5(9) . . ? C54 C53 H53A 119.7 . . ? C52 C53 H53A 119.7 . . ? C62 C57 C58 114.2(7) . . ? C62 C57 B1 122.4(6) . . ? C58 C57 B1 123.1(7) . . ? C59 C58 C57 124.8(9) . . ? C59 C58 H58A 117.6 . . ? C57 C58 H58A 117.6 . . ? N6 C28 C29 177.5(9) . . ? N5 C37 C38 179.1(8) . . ? C56 C55 C54 118.5(9) . . ? C56 C55 H55A 120.8 . . ? C54 C55 H55A 120.8 . . ? O10 N8 O11 123.8(10) . . ? O10 N8 C35 120.8(10) . . ? O11 N8 C35 115.3(11) . . ? O12 N7 O13 123.0(12) . . ? O12 N7 C33 114.5(10) . . ? O13 N7 C33 122.4(12) . . ? C61 C62 C57 123.9(8) . . ? C61 C62 H62A 118.1 . . ? C57 C62 H62A 118.1 . . ? C58 C59 C60 118.4(10) . . ? C58 C59 H59A 120.8 . . ? C60 C59 H59A 120.8 . . ? C61 C60 C59 120.2(9) . . ? C61 C60 H60A 119.9 . . ? C59 C60 H60A 119.9 . . ? C62 C61 C60 118.4(10) . . ? C62 C61 H61A 120.8 . . ? C60 C61 H61A 120.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ni1 O2 C21 52.4(5) . . . . ? O4 Ni1 O2 C21 -43.1(5) . . . . ? N5 Ni1 O2 C21 -54.3(16) . . . . ? N1 Ni1 O2 C21 142.3(5) . . . . ? N2 Ni1 O2 C21 -136.2(5) . . . . ? O3 Ni2 O1 C1 -142.4(4) . . . . ? N3 Ni2 O1 C1 39.4(4) . . . . ? O5 Ni2 O1 C1 131.9(4) . . . . ? N4 Ni2 O1 C1 29.5(11) . . . . ? N6 Ni2 O1 C1 -60.0(4) . . . . ? O3 Ni2 O1 Ni1 36.5(2) . . . . ? N3 Ni2 O1 Ni1 -141.6(2) . . . . ? O5 Ni2 O1 Ni1 -49.1(2) . . . . ? N4 Ni2 O1 Ni1 -151.6(8) . . . . ? N6 Ni2 O1 Ni1 118.9(2) . . . . ? O4 Ni1 O1 C1 -145.5(4) . . . . ? O2 Ni1 O1 C1 127.7(4) . . . . ? N5 Ni1 O1 C1 -59.3(4) . . . . ? N1 Ni1 O1 C1 33.8(4) . . . . ? N2 Ni1 O1 C1 72.4(11) . . . . ? O4 Ni1 O1 Ni2 35.6(2) . . . . ? O2 Ni1 O1 Ni2 -51.2(2) . . . . ? N5 Ni1 O1 Ni2 121.7(2) . . . . ? N1 Ni1 O1 Ni2 -145.2(2) . . . . ? N2 Ni1 O1 Ni2 -106.6(9) . . . . ? O1 Ni2 O3 C21 -3.1(6) . . . . ? N3 Ni2 O3 C21 163.1(12) . . . . ? O5 Ni2 O3 C21 89.5(6) . . . . ? N4 Ni2 O3 C21 178.9(6) . . . . ? N6 Ni2 O3 C21 -89.9(6) . . . . ? Ni2 O1 C1 C6 -51.2(7) . . . . ? Ni1 O1 C1 C6 129.9(5) . . . . ? Ni2 O1 C1 C2 128.1(5) . . . . ? Ni1 O1 C1 C2 -50.8(7) . . . . ? C5 C6 C1 O1 -179.0(5) . . . . ? C14 C6 C1 O1 -1.9(8) . . . . ? C5 C6 C1 C2 1.7(9) . . . . ? C14 C6 C1 C2 178.8(5) . . . . ? O1 C1 C2 C3 179.4(5) . . . . ? C6 C1 C2 C3 -1.3(9) . . . . ? O1 C1 C2 C7 2.7(8) . . . . ? C6 C1 C2 C7 -178.0(5) . . . . ? C1 C6 C5 C4 -0.8(9) . . . . ? C14 C6 C5 C4 -177.8(6) . . . . ? C1 C2 C3 C4 0.1(9) . . . . ? C7 C2 C3 C4 176.7(6) . . . . ? C6 C5 C4 C3 -0.5(10) . . . . ? C6 C5 C4 Br1 175.6(5) . . . . ? C2 C3 C4 C5 0.8(10) . . . . ? C2 C3 C4 Br1 -175.2(4) . . . . ? O1 Ni1 N1 C7 21.3(4) . . . . ? O4 Ni1 N1 C7 -166.1(18) . . . . ? O2 Ni1 N1 C7 -69.0(4) . . . . ? N5 Ni1 N1 C7 113.1(4) . . . . ? N2 Ni1 N1 C7 -152.1(4) . . . . ? O1 Ni1 N1 C8 149.9(4) . . . . ? O4 Ni1 N1 C8 -37(2) . . . . ? O2 Ni1 N1 C8 59.5(4) . . . . ? N5 Ni1 N1 C8 -118.4(4) . . . . ? N2 Ni1 N1 C8 -23.6(4) . . . . ? O1 Ni2 O5 C30 43.1(5) . . . . ? O3 Ni2 O5 C30 -52.8(5) . . . . ? N3 Ni2 O5 C30 134.6(5) . . . . ? N4 Ni2 O5 C30 -150.6(5) . . . . ? N6 Ni2 O5 C30 -50.0(12) . . . . ? O1 Ni2 N3 C18 132.4(4) . . . . ? O3 Ni2 N3 C18 -33.9(16) . . . . ? O5 Ni2 N3 C18 39.2(4) . . . . ? N4 Ni2 N3 C18 -50.1(4) . . . . ? N6 Ni2 N3 C18 -139.8(4) . . . . ? O1 Ni2 N3 C15 -106.9(4) . . . . ? O3 Ni2 N3 C15 86.8(14) . . . . ? O5 Ni2 N3 C15 159.9(4) . . . . ? N4 Ni2 N3 C15 70.6(5) . . . . ? N6 Ni2 N3 C15 -19.1(5) . . . . ? O1 Ni2 N3 C14 14.8(4) . . . . ? O3 Ni2 N3 C14 -151.4(13) . . . . ? O5 Ni2 N3 C14 -78.3(4) . . . . ? N4 Ni2 N3 C14 -167.6(4) . . . . ? N6 Ni2 N3 C14 102.7(4) . . . . ? O1 Ni1 O4 C30 0.1(6) . . . . ? O2 Ni1 O4 C30 90.1(6) . . . . ? N5 Ni1 O4 C30 -91.3(6) . . . . ? N1 Ni1 O4 C30 -172.5(18) . . . . ? N2 Ni1 O4 C30 173.7(6) . . . . ? O1 Ni1 N2 C13 -176.8(8) . . . . ? O4 Ni1 N2 C13 40.9(5) . . . . ? O2 Ni1 N2 C13 127.4(5) . . . . ? N5 Ni1 N2 C13 -45.3(5) . . . . ? N1 Ni1 N2 C13 -137.7(5) . . . . ? O1 Ni1 N2 C9 -44.7(12) . . . . ? O4 Ni1 N2 C9 173.1(4) . . . . ? O2 Ni1 N2 C9 -100.5(4) . . . . ? N5 Ni1 N2 C9 86.8(4) . . . . ? N1 Ni1 N2 C9 -5.6(4) . . . . ? O1 Ni2 N4 C20 176.7(8) . . . . ? O3 Ni2 N4 C20 -11.4(6) . . . . ? N3 Ni2 N4 C20 166.4(7) . . . . ? O5 Ni2 N4 C20 73.9(6) . . . . ? N6 Ni2 N4 C20 -94.3(6) . . . . ? O1 Ni2 N4 C17 -57.0(12) . . . . ? O3 Ni2 N4 C17 114.9(5) . . . . ? N3 Ni2 N4 C17 -67.3(5) . . . . ? O5 Ni2 N4 C17 -159.8(5) . . . . ? N6 Ni2 N4 C17 32.0(6) . . . . ? O1 Ni2 N4 C19 59.0(11) . . . . ? O3 Ni2 N4 C19 -129.1(4) . . . . ? N3 Ni2 N4 C19 48.7(4) . . . . ? O5 Ni2 N4 C19 -43.8(4) . . . . ? N6 Ni2 N4 C19 148.0(5) . . . . ? O1 Ni1 N5 C37 -43(5) . . . . ? O4 Ni1 N5 C37 52(5) . . . . ? O2 Ni1 N5 C37 63(6) . . . . ? N1 Ni1 N5 C37 -133(5) . . . . ? N2 Ni1 N5 C37 145(5) . . . . ? C13 N2 C9 C8 171.5(5) . . . . ? Ni1 N2 C9 C8 33.6(6) . . . . ? C13 N2 C9 C10 -60.1(7) . . . . ? Ni1 N2 C9 C10 161.9(5) . . . . ? C7 N1 C8 C9 176.4(5) . . . . ? Ni1 N1 C8 C9 49.0(5) . . . . ? N2 C9 C8 N1 -55.6(6) . . . . ? C10 C9 C8 N1 179.7(6) . . . . ? N2 C9 C10 C11 59.1(8) . . . . ? C8 C9 C10 C11 -176.9(6) . . . . ? C9 C10 C11 C12 -55.8(8) . . . . ? O1 Ni2 N6 C28 -103.1(15) . . . . ? O3 Ni2 N6 C28 -6.5(15) . . . . ? N3 Ni2 N6 C28 165.9(15) . . . . ? O5 Ni2 N6 C28 -9(2) . . . . ? N4 Ni2 N6 C28 90.9(15) . . . . ? C8 N1 C7 C2 171.8(5) . . . . ? Ni1 N1 C7 C2 -64.1(6) . . . . ? C3 C2 C7 N1 -117.5(6) . . . . ? C1 C2 C7 N1 59.2(7) . . . . ? C1 C6 C14 N3 64.3(7) . . . . ? C5 C6 C14 N3 -118.7(6) . . . . ? C18 N3 C14 C6 -176.8(5) . . . . ? C15 N3 C14 C6 62.3(6) . . . . ? Ni2 N3 C14 C6 -61.4(6) . . . . ? C20 N4 C19 C18 -157.8(7) . . . . ? C17 N4 C19 C18 82.2(7) . . . . ? Ni2 N4 C19 C18 -37.9(6) . . . . ? C18 N3 C15 C16 42.6(8) . . . . ? C14 N3 C15 C16 162.5(6) . . . . ? Ni2 N3 C15 C16 -75.1(7) . . . . ? N3 C15 C16 C17 47.9(10) . . . . ? C15 N3 C18 C19 -79.8(7) . . . . ? C14 N3 C18 C19 160.3(5) . . . . ? Ni2 N3 C18 C19 42.0(6) . . . . ? N4 C19 C18 N3 -1.5(8) . . . . ? C20 N4 C17 C16 -166.1(7) . . . . ? C19 N4 C17 C16 -47.4(9) . . . . ? Ni2 N4 C17 C16 66.9(8) . . . . ? C15 C16 C17 N4 -45.2(10) . . . . ? C26 C27 C22 C23 -0.3(8) . . . . ? C26 C27 C22 C21 179.1(5) . . . . ? C25 C24 C23 C22 -2.2(9) . . . . ? N9 C24 C23 C22 175.3(5) . . . . ? C27 C22 C23 C24 1.3(8) . . . . ? C21 C22 C23 C24 -178.1(5) . . . . ? Ni2 O3 C21 O2 -0.1(10) . . . . ? Ni2 O3 C21 C22 179.5(4) . . . . ? Ni1 O2 C21 O3 -31.1(9) . . . . ? Ni1 O2 C21 C22 149.3(4) . . . . ? C27 C22 C21 O3 -10.0(8) . . . . ? C23 C22 C21 O3 169.4(5) . . . . ? C27 C22 C21 O2 169.7(5) . . . . ? C23 C22 C21 O2 -10.9(8) . . . . ? C23 C24 C25 C26 1.9(9) . . . . ? N9 C24 C25 C26 -175.5(5) . . . . ? C24 C25 C26 C27 -0.8(9) . . . . ? C24 C25 C26 N10 179.9(5) . . . . ? C22 C27 C26 C25 0.0(9) . . . . ? C22 C27 C26 N10 179.3(5) . . . . ? C9 N2 C13 C12 56.5(7) . . . . ? Ni1 N2 C13 C12 -172.4(5) . . . . ? C10 C11 C12 C13 52.9(9) . . . . ? N2 C13 C12 C11 -53.6(9) . . . . ? C25 C24 N9 O6 174.5(7) . . . . ? C23 C24 N9 O6 -3.0(9) . . . . ? C25 C24 N9 O7 -1.7(9) . . . . ? C23 C24 N9 O7 -179.2(6) . . . . ? C25 C26 N10 O9 -15.4(9) . . . . ? C27 C26 N10 O9 165.3(6) . . . . ? C25 C26 N10 O8 166.7(6) . . . . ? C27 C26 N10 O8 -12.6(9) . . . . ? Ni1 O4 C30 O5 -10.3(11) . . . . ? Ni1 O4 C30 C31 169.6(4) . . . . ? Ni2 O5 C30 O4 -17.1(10) . . . . ? Ni2 O5 C30 C31 163.1(4) . . . . ? O4 C30 C31 C32 -15.5(9) . . . . ? O5 C30 C31 C32 164.4(6) . . . . ? O4 C30 C31 C36 162.2(6) . . . . ? O5 C30 C31 C36 -17.9(9) . . . . ? C32 C31 C36 C35 1.9(9) . . . . ? C30 C31 C36 C35 -175.9(6) . . . . ? C36 C31 C32 C33 -0.4(10) . . . . ? C30 C31 C32 C33 177.4(7) . . . . ? C33 C34 C35 C36 -1.5(12) . . . . ? C33 C34 C35 N8 177.8(7) . . . . ? C31 C36 C35 C34 -1.0(10) . . . . ? C31 C36 C35 N8 179.7(6) . . . . ? C31 C32 C33 C34 -2.3(12) . . . . ? C31 C32 C33 N7 179.3(8) . . . . ? C35 C34 C33 C32 3.2(12) . . . . ? C35 C34 C33 N7 -178.3(8) . . . . ? C51 B1 C39 C40 -36.0(9) . . . . ? C57 B1 C39 C40 88.1(8) . . . . ? C45 B1 C39 C40 -151.8(6) . . . . ? C51 B1 C39 C44 153.0(7) . . . . ? C57 B1 C39 C44 -82.9(8) . . . . ? C45 B1 C39 C44 37.1(9) . . . . ? C44 C39 C40 C41 -2.0(11) . . . . ? B1 C39 C40 C41 -173.7(7) . . . . ? C51 B1 C45 C50 91.0(7) . . . . ? C57 B1 C45 C50 -32.2(9) . . . . ? C39 B1 C45 C50 -146.7(6) . . . . ? C51 B1 C45 C46 -81.5(8) . . . . ? C57 B1 C45 C46 155.3(6) . . . . ? C39 B1 C45 C46 40.9(9) . . . . ? C39 C40 C41 C42 0.1(12) . . . . ? C46 C45 C50 C49 -1.3(10) . . . . ? B1 C45 C50 C49 -174.2(7) . . . . ? C40 C41 C42 C43 1.1(14) . . . . ? C48 C47 C46 C45 -1.4(13) . . . . ? C50 C45 C46 C47 1.6(11) . . . . ? B1 C45 C46 C47 174.7(8) . . . . ? C46 C47 C48 C49 0.7(13) . . . . ? C40 C39 C44 C43 2.9(13) . . . . ? B1 C39 C44 C43 174.9(8) . . . . ? C41 C42 C43 C44 -0.3(16) . . . . ? C39 C44 C43 C42 -1.9(16) . . . . ? C57 B1 C51 C52 -141.6(7) . . . . ? C45 B1 C51 C52 95.8(8) . . . . ? C39 B1 C51 C52 -22.9(9) . . . . ? C57 B1 C51 C56 46.5(9) . . . . ? C45 B1 C51 C56 -76.1(7) . . . . ? C39 B1 C51 C56 165.2(6) . . . . ? C56 C51 C52 C53 -1.3(11) . . . . ? B1 C51 C52 C53 -173.8(8) . . . . ? C47 C48 C49 C50 -0.4(12) . . . . ? C45 C50 C49 C48 0.7(12) . . . . ? C52 C51 C56 C55 0.3(12) . . . . ? B1 C51 C56 C55 173.3(8) . . . . ? C55 C54 C53 C52 -1.5(14) . . . . ? C51 C52 C53 C54 1.9(14) . . . . ? C51 B1 C57 C62 -158.0(6) . . . . ? C45 B1 C57 C62 -40.2(8) . . . . ? C39 B1 C57 C62 77.3(7) . . . . ? C51 B1 C57 C58 29.1(9) . . . . ? C45 B1 C57 C58 146.8(6) . . . . ? C39 B1 C57 C58 -95.6(7) . . . . ? C62 C57 C58 C59 -0.4(11) . . . . ? B1 C57 C58 C59 173.1(7) . . . . ? Ni2 N6 C28 C29 -92(19) . . . . ? Ni1 N5 C37 C38 153(54) . . . . ? C51 C56 C55 C54 0.0(14) . . . . ? C53 C54 C55 C56 0.5(14) . . . . ? C34 C35 N8 O10 -176.5(10) . . . . ? C36 C35 N8 O10 2.9(13) . . . . ? C34 C35 N8 O11 1.1(12) . . . . ? C36 C35 N8 O11 -179.6(7) . . . . ? C32 C33 N7 O12 -8.5(16) . . . . ? C34 C33 N7 O12 173.0(10) . . . . ? C32 C33 N7 O13 169.6(10) . . . . ? C34 C33 N7 O13 -8.9(15) . . . . ? C58 C57 C62 C61 1.4(10) . . . . ? B1 C57 C62 C61 -172.2(7) . . . . ? C57 C58 C59 C60 -0.2(13) . . . . ? C58 C59 C60 C61 0.0(14) . . . . ? C57 C62 C61 C60 -1.7(12) . . . . ? C59 C60 C61 C62 0.9(14) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.537 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.066 # Attachment 'complex-3.cif' data_shelxl3 _database_code_depnum_ccdc_archive 'CCDC 789254' #TrackingRef 'complex-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H71 B Br N6 Ni2 O9 P2' _chemical_formula_weight 1434.43 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' P P 0.1023 0.0942 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.913(3) _cell_length_b 15.245(3) _cell_length_c 15.720(3) _cell_angle_alpha 93.31(3) _cell_angle_beta 99.98(3) _cell_angle_gamma 90.46(3) _cell_volume 3513.5(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1486 _exptl_absorpt_coefficient_mu 1.210 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7130 _exptl_absorpt_correction_T_max 0.8886 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27514 _diffrn_reflns_av_R_equivalents 0.1194 _diffrn_reflns_av_sigmaI/netI 0.1798 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12269 _reflns_number_gt 4228 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1239P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0066(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12269 _refine_ls_number_parameters 737 _refine_ls_number_restraints 174 _refine_ls_R_factor_all 0.2450 _refine_ls_R_factor_gt 0.0942 _refine_ls_wR_factor_ref 0.2942 _refine_ls_wR_factor_gt 0.2153 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.674 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.36474(12) 0.59442(13) 0.26218(14) 0.0644(7) Uani 1 1 d . . . Ni2 Ni 0.28287(13) 0.81831(13) 0.24943(15) 0.0691(8) Uani 1 1 d . . . Br1 Br 0.26449(16) 0.64929(15) -0.19211(14) 0.1074(9) Uani 1 1 d . . . P1 P 0.4562(3) 0.7575(3) 0.3848(3) 0.0740(14) Uani 1 1 d . . . P2 P 0.1967(3) 0.6645(3) 0.3486(3) 0.0734(14) Uani 1 1 d . . . O1 O 0.3199(7) 0.7042(7) 0.1963(8) 0.068(3) Uani 1 1 d . . . C2 C 0.2217(11) 0.7135(10) 0.0588(12) 0.068(5) Uani 1 1 d . . . C6 C 0.3774(11) 0.6589(11) 0.0682(13) 0.070(5) Uani 1 1 d . . . C1 C 0.3076(10) 0.6911(10) 0.1100(12) 0.065(4) Uani 1 1 d . . . C4 C 0.2841(13) 0.6650(12) -0.0705(11) 0.076(5) Uani 1 1 d . . . C5 C 0.3633(12) 0.6458(11) -0.0212(13) 0.073(5) Uani 1 1 d . . . H5A H 0.4100 0.6231 -0.0476 0.087 Uiso 1 1 calc R . . C3 C 0.2123(12) 0.6991(10) -0.0308(13) 0.074(5) Uani 1 1 d . . . H3A H 0.1575 0.7122 -0.0654 0.089 Uiso 1 1 calc R . . O6 O 0.2798(7) 0.6111(7) 0.3526(7) 0.073(3) Uani 1 1 d . . . O2 O 0.4603(7) 0.6674(7) 0.3455(8) 0.080(4) Uani 1 1 d . . . O3 O 0.3790(7) 0.8145(7) 0.3564(7) 0.078(3) Uani 1 1 d . . . O7 O 0.1891(7) 0.7478(7) 0.3020(8) 0.084(4) Uani 1 1 d . . . N1 N 0.4573(7) 0.5643(8) 0.1804(8) 0.062(3) Uani 1 1 d . . . O9 O 0.1076(7) 0.6071(8) 0.3073(7) 0.081(3) Uani 1 1 d . . . O5 O 0.4692(7) 0.7492(8) 0.4877(7) 0.079(3) Uani 1 1 d . . . O8 O 0.1830(8) 0.6845(9) 0.4455(8) 0.099(4) Uani 1 1 d . . . O4 O 0.5441(7) 0.8117(8) 0.3725(8) 0.085(4) Uani 1 1 d . . . N2 N 0.4313(10) 0.4816(9) 0.3125(10) 0.077(4) Uani 1 1 d . . . C9 C 0.5303(14) 0.4999(13) 0.3180(13) 0.099(7) Uani 1 1 d . . . H9A H 0.5631 0.4452 0.3196 0.119 Uiso 1 1 calc R . . H9B H 0.5533 0.5354 0.3706 0.119 Uiso 1 1 calc R . . C11 C 0.4391(13) 0.4018(11) 0.1752(14) 0.088(6) Uani 1 1 d . . . H11A H 0.4080 0.3539 0.1380 0.106 Uiso 1 1 calc R . . H11B H 0.5031 0.3874 0.1875 0.106 Uiso 1 1 calc R . . C8 C 0.5455(11) 0.5491(13) 0.2389(14) 0.097(7) Uani 1 1 d . . . H8A H 0.5757 0.6051 0.2581 0.116 Uiso 1 1 calc R . . H8B H 0.5849 0.5151 0.2071 0.116 Uiso 1 1 calc R . . C12 C 0.4048(14) 0.4036(14) 0.2565(15) 0.102(7) Uani 1 1 d . . . H12A H 0.3389 0.3993 0.2439 0.122 Uiso 1 1 calc R . . H12B H 0.4267 0.3524 0.2872 0.122 Uiso 1 1 calc R . . C10 C 0.4307(12) 0.4830(10) 0.1244(12) 0.078(5) Uani 1 1 d . . . H10A H 0.4692 0.4775 0.0806 0.094 Uiso 1 1 calc R . . H10B H 0.3683 0.4877 0.0951 0.094 Uiso 1 1 calc R . . C7 C 0.4667(10) 0.6387(11) 0.1229(12) 0.075(5) Uani 1 1 d . . . H7A H 0.5103 0.6229 0.0856 0.090 Uiso 1 1 calc R . . H7B H 0.4900 0.6907 0.1585 0.090 Uiso 1 1 calc R . . N3 N 0.1806(8) 0.8382(9) 0.1454(9) 0.070(4) Uani 1 1 d . . . N4 N 0.2248(9) 0.9257(9) 0.3038(10) 0.084(4) Uani 1 1 d . . . H4A H 0.1926 0.9015 0.3410 0.101 Uiso 1 1 calc R . . C14 C 0.1475(10) 0.7519(12) 0.0988(12) 0.078(5) Uani 1 1 d . . . H14A H 0.1297 0.7123 0.1393 0.094 Uiso 1 1 calc R . . H14B H 0.0949 0.7611 0.0546 0.094 Uiso 1 1 calc R . . C16 C 0.1543(12) 0.9598(12) 0.2384(13) 0.083(5) Uani 1 1 d . . . H16A H 0.1850 0.9966 0.2028 0.100 Uiso 1 1 calc R . . C15 C 0.1101(12) 0.8861(12) 0.1813(12) 0.086(6) Uani 1 1 d . . . H15A H 0.0786 0.8475 0.2138 0.103 Uiso 1 1 calc R . . H15B H 0.0659 0.9081 0.1350 0.103 Uiso 1 1 calc R . . C13 C 0.4179(15) 0.4669(14) 0.3989(14) 0.117(8) Uani 1 1 d . . . H13A H 0.4494 0.4150 0.4182 0.175 Uiso 1 1 calc R . . H13B H 0.3540 0.4593 0.3995 0.175 Uiso 1 1 calc R . . H13C H 0.4413 0.5165 0.4369 0.175 Uiso 1 1 calc R . . C17 C 0.0920(16) 1.0206(16) 0.2840(16) 0.121(8) Uani 1 1 d . . . H17A H 0.0454 1.0445 0.2410 0.145 Uiso 1 1 calc R . . H17B H 0.0621 0.9870 0.3219 0.145 Uiso 1 1 calc R . . C18 C 0.1480(17) 1.0948(15) 0.3360(18) 0.124(8) Uani 1 1 d . . . H18A H 0.1742 1.1306 0.2972 0.149 Uiso 1 1 calc R . . H18B H 0.1087 1.1317 0.3653 0.149 Uiso 1 1 calc R . . C19 C 0.2229(17) 1.0610(16) 0.4017(19) 0.150(11) Uani 1 1 d . . . H19A H 0.1971 1.0332 0.4461 0.180 Uiso 1 1 calc R . . H19B H 0.2620 1.1094 0.4291 0.180 Uiso 1 1 calc R . . C20 C 0.2782(15) 0.9947(15) 0.3572(18) 0.132(9) Uani 1 1 d . . . H20A H 0.3129 1.0259 0.3213 0.158 Uiso 1 1 calc R . . H20B H 0.3213 0.9678 0.4011 0.158 Uiso 1 1 calc R . . C27 C 0.4417(18) 0.819(2) 0.5382(19) 0.157(3) Uani 1 1 d DU . . C21 C 0.6268(19) 0.773(2) 0.3704(18) 0.157(3) Uani 1 1 d DU . . C28 C 0.4954(18) 0.8929(18) 0.5550(18) 0.157(3) Uani 1 1 d DU . . H28A H 0.5486 0.8962 0.5318 0.188 Uiso 1 1 calc R . . C29 C 0.4720(17) 0.9627(19) 0.6055(17) 0.157(3) Uani 1 1 d DU . . H29A H 0.5086 1.0131 0.6169 0.188 Uiso 1 1 calc R . . C22 C 0.6623(16) 0.7763(19) 0.2955(18) 0.157(3) Uani 1 1 d DU . . H22A H 0.6326 0.8089 0.2512 0.188 Uiso 1 1 calc R . . B1 B 0.2203(12) 0.1806(11) 0.0043(14) 0.066(5) Uani 1 1 d . . . C30 C 0.3946(16) 0.9562(19) 0.6382(18) 0.157(3) Uani 1 1 d DU . . H30A H 0.3703 1.0063 0.6615 0.188 Uiso 1 1 calc R . . C23 C 0.7403(16) 0.7333(19) 0.284(2) 0.157(3) Uani 1 1 d DU . . H23A H 0.7651 0.7376 0.2342 0.188 Uiso 1 1 calc R . . C25 C 0.7438(16) 0.6691(19) 0.4228(18) 0.157(3) Uani 1 1 d DU . . H25A H 0.7699 0.6309 0.4637 0.188 Uiso 1 1 calc R . . C24 C 0.7799(18) 0.684(2) 0.3503(18) 0.157(3) Uani 1 1 d DU . . H24A H 0.8353 0.6583 0.3455 0.188 Uiso 1 1 calc R . . C26 C 0.6658(17) 0.7153(18) 0.4308(19) 0.157(3) Uani 1 1 d DU . . H26A H 0.6385 0.7074 0.4787 0.188 Uiso 1 1 calc R . . C31 C 0.3510(18) 0.8757(17) 0.6373(18) 0.157(3) Uani 1 1 d DU . . H31A H 0.3080 0.8680 0.6727 0.188 Uiso 1 1 calc R . . C45 C 0.1398(10) 0.1783(12) 0.0619(11) 0.065(4) Uani 1 1 d . . . C62 C 0.2542(11) 0.0146(12) -0.0144(15) 0.090(6) Uani 1 1 d . . . H62A H 0.2689 0.0158 0.0456 0.108 Uiso 1 1 calc R . . C53 C 0.4307(16) 0.1760(12) 0.2030(16) 0.101(7) Uani 1 1 d . . . H53A H 0.4412 0.1699 0.2624 0.121 Uiso 1 1 calc R . . C50 C 0.0705(10) 0.1155(12) 0.0462(11) 0.071(5) Uani 1 1 d . . . H50A H 0.0746 0.0678 0.0076 0.085 Uiso 1 1 calc R . . C56 C 0.3986(12) 0.1974(11) 0.0297(15) 0.093(6) Uani 1 1 d . . . H56A H 0.3900 0.2078 -0.0288 0.111 Uiso 1 1 calc R . . C47 C 0.0552(15) 0.2537(14) 0.1663(13) 0.093(6) Uani 1 1 d . . . H47A H 0.0519 0.3014 0.2053 0.111 Uiso 1 1 calc R . . C51 C 0.3234(11) 0.1856(10) 0.0674(14) 0.074(5) Uani 1 1 d . . . C63 C 0.1999(11) 0.2683(11) -0.0501(11) 0.066(4) Uani 1 1 d . . . C64 C 0.2575(12) 0.3417(12) -0.0450(12) 0.081(5) Uani 1 1 d . . . H64A H 0.3148 0.3400 -0.0106 0.097 Uiso 1 1 calc R . . C68 C 0.1151(11) 0.2750(12) -0.1015(11) 0.075(5) Uani 1 1 d . . . H68A H 0.0733 0.2285 -0.1068 0.090 Uiso 1 1 calc R . . C58 C 0.2011(14) 0.0812(13) -0.1436(16) 0.096(6) Uani 1 1 d . . . H58A H 0.1781 0.1289 -0.1743 0.115 Uiso 1 1 calc R . . C48 C -0.0140(13) 0.1896(16) 0.1483(15) 0.093(6) Uani 1 1 d . . . H48A H -0.0638 0.1924 0.1767 0.112 Uiso 1 1 calc R . . C57 C 0.2242(10) 0.0913(12) -0.0537(13) 0.073(5) Uani 1 1 d . . . C52 C 0.3411(13) 0.1758(11) 0.1569(14) 0.084(6) Uani 1 1 d . . . H52A H 0.2927 0.1691 0.1863 0.101 Uiso 1 1 calc R . . C54 C 0.5013(18) 0.1850(15) 0.161(2) 0.117(9) Uani 1 1 d . . . H54A H 0.5601 0.1848 0.1926 0.140 Uiso 1 1 calc R . . C49 C -0.0071(12) 0.1222(14) 0.0877(14) 0.084(6) Uani 1 1 d . . . H49A H -0.0538 0.0803 0.0736 0.101 Uiso 1 1 calc R . . C46 C 0.1289(12) 0.2438(13) 0.1239(13) 0.085(5) Uani 1 1 d . . . H46A H 0.1759 0.2854 0.1386 0.102 Uiso 1 1 calc R . . C59 C 0.2116(16) 0.0018(17) -0.1886(16) 0.116(7) Uani 1 1 d . . . H59A H 0.1962 -0.0006 -0.2486 0.139 Uiso 1 1 calc R . . C67 C 0.0921(12) 0.3501(14) -0.1447(12) 0.087(6) Uani 1 1 d . . . H67A H 0.0354 0.3521 -0.1801 0.104 Uiso 1 1 calc R . . C66 C 0.1495(14) 0.4220(14) -0.1376(14) 0.094(6) Uani 1 1 d . . . H66A H 0.1322 0.4731 -0.1652 0.112 Uiso 1 1 calc R . . C65 C 0.2347(14) 0.4143(14) -0.0869(14) 0.099(6) Uani 1 1 d . . . H65A H 0.2767 0.4605 -0.0821 0.118 Uiso 1 1 calc R . . C55 C 0.4903(14) 0.1942(11) 0.077(2) 0.102(8) Uani 1 1 d . . . H55A H 0.5401 0.1985 0.0487 0.123 Uiso 1 1 calc R . . C61 C 0.2629(12) -0.0651(16) -0.063(2) 0.110(8) Uani 1 1 d . . . H61A H 0.2832 -0.1147 -0.0340 0.132 Uiso 1 1 calc R . . C60 C 0.2420(16) -0.0707(17) -0.152(2) 0.116(8) Uani 1 1 d . . . H60A H 0.2488 -0.1225 -0.1839 0.140 Uiso 1 1 calc R . . C39 C 0.0868(15) 0.5288(15) 0.3397(12) 0.096(6) Uani 1 1 d DU . . C40 C 0.1412(17) 0.4570(14) 0.3466(14) 0.142(9) Uani 1 1 d DU . . H40A H 0.1991 0.4599 0.3323 0.170 Uiso 1 1 calc R . . C44 C 0.0013(19) 0.528(2) 0.359(2) 0.174(11) Uani 1 1 d DU . . H44A H -0.0344 0.5774 0.3567 0.209 Uiso 1 1 calc R . . C42 C 0.026(2) 0.378(2) 0.397(2) 0.174(13) Uani 1 1 d DU . . H42A H 0.0061 0.3285 0.4207 0.209 Uiso 1 1 calc R . . C41 C 0.111(2) 0.3804(17) 0.3744(16) 0.161(11) Uani 1 1 d DU . . H41A H 0.1468 0.3309 0.3782 0.193 Uiso 1 1 calc R . . C32 C 0.3720(17) 0.8061(19) 0.5829(17) 0.157(3) Uani 1 1 d DU . . H32A H 0.3397 0.7530 0.5772 0.188 Uiso 1 1 calc R . . C75 C 0.1252(17) 0.7514(19) 0.4747(17) 0.157(3) Uani 1 1 d DU . . C76 C 0.0509(15) 0.7786(16) 0.4204(19) 0.157(3) Uani 1 1 d DU . . H76A H 0.0423 0.7533 0.3642 0.188 Uiso 1 1 calc R . . C43 C -0.029(3) 0.449(2) 0.383(3) 0.216(15) Uani 1 1 d DU . . H43A H -0.0897 0.4433 0.3895 0.260 Uiso 1 1 calc R . . N6 N 0.3750(11) 0.8884(10) 0.1890(12) 0.087(5) Uani 1 1 d . . . C83 C 0.4295(15) 0.9207(13) 0.1608(15) 0.087(6) Uani 1 1 d . . . C84 C 0.5007(17) 0.9622(14) 0.1201(18) 0.128(9) Uani 1 1 d . . . N5 N 0.2518(9) 0.5267(9) 0.1812(9) 0.074(4) Uani 1 1 d . . . C81 C 0.1847(13) 0.5088(12) 0.1374(12) 0.077(5) Uani 1 1 d . . . C82 C 0.0970(12) 0.4826(15) 0.0814(15) 0.112(7) Uani 1 1 d . . . C78 C 0.0256(16) 0.873(2) 0.5178(17) 0.157(3) Uani 1 1 d DU . . H78A H 0.0127 0.9317 0.5282 0.188 Uiso 1 1 calc R . . C77 C -0.0137(17) 0.8387(17) 0.4370(18) 0.157(3) Uani 1 1 d DU . . H77A H -0.0687 0.8522 0.4029 0.188 Uiso 1 1 calc R . . C79 C 0.0808(16) 0.8369(17) 0.5869(19) 0.157(3) Uani 1 1 d DU . . H79A H 0.0790 0.8550 0.6441 0.188 Uiso 1 1 calc R . . C80 C 0.1400(17) 0.7708(18) 0.5643(18) 0.157(3) Uani 1 1 d DU . . H80A H 0.1831 0.7437 0.6038 0.188 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0654(12) 0.0520(13) 0.0703(15) -0.0128(11) 0.0012(10) 0.0099(9) Ni2 0.0697(13) 0.0521(14) 0.0841(17) -0.0036(11) 0.0115(11) 0.0124(10) Br1 0.1475(19) 0.0964(18) 0.0786(16) -0.0019(12) 0.0223(13) 0.0173(14) P1 0.069(3) 0.061(3) 0.086(4) -0.017(3) 0.004(2) 0.008(2) P2 0.074(3) 0.072(3) 0.073(3) -0.007(3) 0.014(2) 0.014(2) O1 0.076(7) 0.053(7) 0.071(8) -0.007(6) 0.004(6) 0.006(5) C2 0.076(11) 0.054(11) 0.072(13) -0.003(9) 0.011(9) -0.002(8) C6 0.068(10) 0.058(11) 0.089(14) -0.002(10) 0.030(10) -0.004(8) C1 0.067(10) 0.053(10) 0.076(13) -0.012(9) 0.018(9) 0.008(8) C4 0.099(13) 0.078(13) 0.054(11) 0.006(10) 0.022(10) -0.001(10) C5 0.083(12) 0.062(11) 0.074(14) -0.013(10) 0.021(10) -0.006(9) C3 0.083(12) 0.047(10) 0.089(15) 0.011(10) 0.005(11) -0.004(8) O6 0.078(7) 0.069(8) 0.070(8) -0.003(6) 0.009(6) 0.029(6) O2 0.076(7) 0.049(7) 0.103(9) -0.038(6) -0.001(6) 0.018(5) O3 0.087(7) 0.057(7) 0.084(8) 0.001(6) -0.002(6) 0.015(6) O7 0.075(7) 0.061(8) 0.122(10) 0.015(7) 0.033(7) 0.010(6) N1 0.063(7) 0.049(8) 0.071(9) -0.019(7) 0.012(7) 0.005(6) O9 0.080(7) 0.079(9) 0.078(8) 0.019(7) -0.001(6) -0.001(6) O5 0.096(8) 0.076(8) 0.063(8) 0.002(6) 0.006(6) 0.020(6) O8 0.099(8) 0.123(12) 0.075(9) -0.024(8) 0.019(7) 0.009(8) O4 0.083(7) 0.074(8) 0.097(9) -0.022(7) 0.020(7) -0.003(6) N2 0.098(11) 0.068(10) 0.058(10) -0.016(8) -0.005(8) 0.018(8) C9 0.123(17) 0.069(13) 0.086(15) -0.007(11) -0.037(12) 0.024(11) C11 0.104(13) 0.056(12) 0.094(16) -0.022(11) -0.002(12) 0.005(10) C8 0.062(10) 0.086(14) 0.126(18) -0.033(13) -0.019(11) 0.028(10) C12 0.115(15) 0.090(17) 0.091(17) -0.009(13) -0.004(13) 0.015(12) C10 0.093(12) 0.051(11) 0.091(14) -0.011(10) 0.020(10) 0.015(9) C7 0.055(9) 0.064(12) 0.108(15) -0.006(11) 0.019(9) 0.002(8) N3 0.067(8) 0.062(9) 0.084(10) -0.001(8) 0.021(7) 0.029(7) N4 0.083(9) 0.064(10) 0.100(12) -0.014(9) 0.005(9) 0.013(8) C14 0.064(10) 0.087(14) 0.084(13) 0.000(11) 0.014(9) 0.028(9) C16 0.103(13) 0.054(12) 0.095(15) -0.005(11) 0.025(12) 0.033(10) C15 0.091(12) 0.077(14) 0.087(14) -0.006(11) 0.015(11) 0.044(10) C13 0.155(19) 0.102(17) 0.087(17) 0.005(13) 0.001(14) 0.042(14) C17 0.143(19) 0.102(19) 0.12(2) 0.002(16) 0.026(16) 0.051(16) C18 0.141(19) 0.076(17) 0.16(2) -0.011(16) 0.038(18) 0.026(15) C19 0.15(2) 0.101(19) 0.19(3) -0.056(18) 0.01(2) 0.049(16) C20 0.121(17) 0.078(16) 0.18(3) -0.036(16) 0.000(17) 0.034(13) C27 0.139(5) 0.175(7) 0.162(6) -0.025(5) 0.052(5) 0.016(4) C21 0.139(5) 0.175(7) 0.162(6) -0.025(5) 0.052(5) 0.016(4) C28 0.139(5) 0.175(7) 0.162(6) -0.025(5) 0.052(5) 0.016(4) C29 0.139(5) 0.175(7) 0.162(6) -0.025(5) 0.052(5) 0.016(4) C22 0.139(5) 0.175(7) 0.162(6) -0.025(5) 0.052(5) 0.016(4) B1 0.069(11) 0.033(10) 0.094(16) -0.005(10) 0.010(11) -0.008(8) C30 0.139(5) 0.175(7) 0.162(6) -0.025(5) 0.052(5) 0.016(4) C23 0.139(5) 0.175(7) 0.162(6) -0.025(5) 0.052(5) 0.016(4) C25 0.139(5) 0.175(7) 0.162(6) -0.025(5) 0.052(5) 0.016(4) C24 0.139(5) 0.175(7) 0.162(6) -0.025(5) 0.052(5) 0.016(4) C26 0.139(5) 0.175(7) 0.162(6) -0.025(5) 0.052(5) 0.016(4) C31 0.139(5) 0.175(7) 0.162(6) -0.025(5) 0.052(5) 0.016(4) C45 0.064(10) 0.068(12) 0.059(11) -0.002(9) 0.004(8) -0.016(9) C62 0.083(12) 0.053(12) 0.134(18) -0.014(12) 0.025(12) 0.003(9) C53 0.108(16) 0.058(13) 0.125(19) 0.002(12) -0.014(16) 0.014(12) C50 0.063(10) 0.085(13) 0.065(12) 0.004(10) 0.012(9) 0.003(9) C56 0.071(12) 0.051(11) 0.15(2) -0.007(12) 0.007(13) -0.009(9) C47 0.122(16) 0.079(15) 0.085(15) -0.004(12) 0.043(13) 0.023(13) C51 0.070(11) 0.040(10) 0.112(17) -0.014(10) 0.024(11) 0.006(8) C63 0.078(11) 0.059(11) 0.061(11) -0.008(9) 0.022(9) -0.002(9) C64 0.098(13) 0.061(12) 0.085(14) 0.008(11) 0.022(10) -0.004(10) C68 0.074(11) 0.069(12) 0.082(13) -0.001(10) 0.013(10) 0.001(9) C58 0.126(16) 0.065(14) 0.101(18) -0.009(12) 0.036(14) 0.005(11) C48 0.084(13) 0.106(18) 0.096(17) 0.022(14) 0.027(12) 0.013(13) C57 0.062(10) 0.067(13) 0.089(15) 0.001(11) 0.016(9) -0.007(8) C52 0.093(14) 0.059(12) 0.100(17) 0.005(11) 0.017(12) -0.008(9) C54 0.094(17) 0.079(16) 0.17(3) 0.018(18) 0.002(19) -0.005(13) C49 0.079(12) 0.084(15) 0.090(15) 0.010(12) 0.015(11) -0.012(10) C46 0.081(12) 0.090(15) 0.081(14) -0.006(12) 0.013(11) -0.006(10) C59 0.15(2) 0.085(18) 0.109(19) -0.030(15) 0.034(15) -0.001(15) C67 0.079(11) 0.095(16) 0.087(14) 0.005(12) 0.014(10) 0.005(11) C66 0.110(15) 0.072(14) 0.106(17) 0.019(12) 0.033(13) 0.005(12) C65 0.105(15) 0.077(15) 0.105(17) -0.003(13) -0.001(13) -0.020(12) C55 0.088(15) 0.033(11) 0.19(3) -0.002(14) 0.046(17) -0.001(9) C61 0.074(12) 0.093(19) 0.17(3) -0.009(18) 0.037(15) -0.006(11) C60 0.132(19) 0.078(18) 0.15(3) -0.039(18) 0.060(18) -0.009(14) C39 0.104(15) 0.103(17) 0.074(13) 0.013(12) -0.001(11) -0.005(13) C40 0.18(2) 0.098(18) 0.15(2) 0.037(17) 0.016(17) 0.013(17) C44 0.19(2) 0.13(2) 0.21(3) 0.05(2) 0.05(2) -0.04(2) C42 0.23(3) 0.14(3) 0.17(2) 0.03(2) 0.07(2) -0.06(2) C41 0.23(3) 0.096(19) 0.15(2) 0.030(17) 0.02(2) -0.04(2) C32 0.139(5) 0.175(7) 0.162(6) -0.025(5) 0.052(5) 0.016(4) C75 0.139(5) 0.175(7) 0.162(6) -0.025(5) 0.052(5) 0.016(4) C76 0.139(5) 0.175(7) 0.162(6) -0.025(5) 0.052(5) 0.016(4) C43 0.24(3) 0.18(3) 0.24(3) 0.02(3) 0.07(3) -0.03(3) N6 0.089(11) 0.062(11) 0.114(14) 0.002(10) 0.026(10) 0.001(9) C83 0.100(15) 0.053(13) 0.102(17) -0.010(11) 0.007(13) 0.008(11) C84 0.155(19) 0.071(15) 0.18(2) 0.021(16) 0.078(19) -0.014(14) N5 0.075(9) 0.073(10) 0.071(10) 0.006(8) 0.007(8) 0.017(8) C81 0.083(12) 0.085(14) 0.061(12) -0.003(10) 0.006(10) 0.023(11) C82 0.075(12) 0.123(19) 0.122(18) -0.018(14) -0.017(12) 0.005(12) C78 0.139(5) 0.175(7) 0.162(6) -0.025(5) 0.052(5) 0.016(4) C77 0.139(5) 0.175(7) 0.162(6) -0.025(5) 0.052(5) 0.016(4) C79 0.139(5) 0.175(7) 0.162(6) -0.025(5) 0.052(5) 0.016(4) C80 0.139(5) 0.175(7) 0.162(6) -0.025(5) 0.052(5) 0.016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O2 2.036(10) . ? Ni1 O6 2.069(11) . ? Ni1 O1 2.073(10) . ? Ni1 N1 2.080(13) . ? Ni1 N2 2.117(13) . ? Ni1 N5 2.144(15) . ? Ni2 O1 2.010(11) . ? Ni2 O3 2.015(10) . ? Ni2 N3 2.072(12) . ? Ni2 O7 2.067(11) . ? Ni2 N4 2.069(14) . ? Ni2 N6 2.115(18) . ? Br1 C4 1.884(17) . ? P1 O3 1.471(10) . ? P1 O2 1.480(11) . ? P1 O4 1.589(12) . ? P1 O5 1.608(12) . ? P2 O6 1.482(10) . ? P2 O7 1.496(11) . ? P2 O8 1.585(13) . ? P2 O9 1.604(12) . ? O1 C1 1.339(19) . ? C2 C3 1.40(2) . ? C2 C1 1.45(2) . ? C2 C14 1.47(2) . ? C6 C5 1.39(2) . ? C6 C1 1.40(2) . ? C6 C7 1.50(2) . ? C4 C5 1.34(2) . ? C4 C3 1.42(2) . ? C5 H5A 0.9300 . ? C3 H3A 0.9300 . ? N1 C10 1.488(19) . ? N1 C7 1.51(2) . ? N1 C8 1.496(18) . ? O9 C39 1.38(2) . ? O5 C27 1.39(3) . ? O8 C75 1.44(3) . ? O4 C21 1.38(3) . ? N2 C12 1.45(2) . ? N2 C13 1.44(2) . ? N2 C9 1.49(2) . ? C9 C8 1.54(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C11 C12 1.45(3) . ? C11 C10 1.51(2) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? N3 C15 1.459(19) . ? N3 C14 1.50(2) . ? N4 C20 1.45(2) . ? N4 C16 1.46(2) . ? N4 H4A 0.9100 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C16 C15 1.47(2) . ? C16 C17 1.55(3) . ? C16 H16A 0.9800 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C17 C18 1.51(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.50(3) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.52(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C27 C32 1.369(15) . ? C27 C28 1.369(15) . ? C21 C26 1.385(15) . ? C21 C22 1.375(15) . ? C28 C29 1.375(15) . ? C28 H28A 0.9300 . ? C29 C30 1.347(15) . ? C29 H29A 0.9300 . ? C22 C23 1.373(14) . ? C22 H22A 0.9300 . ? B1 C45 1.63(3) . ? B1 C57 1.60(3) . ? B1 C63 1.63(2) . ? B1 C51 1.68(2) . ? C30 C31 1.383(15) . ? C30 H30A 0.9300 . ? C23 C24 1.37(3) . ? C23 H23A 0.9300 . ? C25 C24 1.370(15) . ? C25 C26 1.385(14) . ? C25 H25A 0.9300 . ? C24 H24A 0.9300 . ? C26 H26A 0.9300 . ? C31 C32 1.397(15) . ? C31 H31A 0.9300 . ? C45 C46 1.38(2) . ? C45 C50 1.38(2) . ? C62 C57 1.40(2) . ? C62 C61 1.41(3) . ? C62 H62A 0.9300 . ? C53 C54 1.35(3) . ? C53 C52 1.41(2) . ? C53 H53A 0.9300 . ? C50 C49 1.42(2) . ? C50 H50A 0.9300 . ? C56 C51 1.37(2) . ? C56 C55 1.44(3) . ? C56 H56A 0.9300 . ? C47 C46 1.39(2) . ? C47 C48 1.40(3) . ? C47 H47A 0.9300 . ? C51 C52 1.40(2) . ? C63 C68 1.39(2) . ? C63 C64 1.39(2) . ? C64 C65 1.34(2) . ? C64 H64A 0.9300 . ? C68 C67 1.38(2) . ? C68 H68A 0.9300 . ? C58 C57 1.40(3) . ? C58 C59 1.39(3) . ? C58 H58A 0.9300 . ? C48 C49 1.38(3) . ? C48 H48A 0.9300 . ? C52 H52A 0.9300 . ? C54 C55 1.32(3) . ? C54 H54A 0.9300 . ? C49 H49A 0.9300 . ? C46 H46A 0.9300 . ? C59 C60 1.33(3) . ? C59 H59A 0.9300 . ? C67 C66 1.37(2) . ? C67 H67A 0.9300 . ? C66 C65 1.39(2) . ? C66 H66A 0.9300 . ? C65 H65A 0.9300 . ? C55 H55A 0.9300 . ? C61 C60 1.37(3) . ? C61 H61A 0.9300 . ? C60 H60A 0.9300 . ? C39 C44 1.361(15) . ? C39 C40 1.366(14) . ? C40 C41 1.373(15) . ? C40 H40A 0.9300 . ? C44 C43 1.377(15) . ? C44 H44A 0.9300 . ? C42 C43 1.367(15) . ? C42 C41 1.366(15) . ? C42 H42A 0.9300 . ? C41 H41A 0.9300 . ? C32 H32A 0.9300 . ? C75 C76 1.361(15) . ? C75 C80 1.402(15) . ? C76 C77 1.381(15) . ? C76 H76A 0.9300 . ? C43 H43A 0.9300 . ? N6 C83 1.12(2) . ? C83 C84 1.49(3) . ? N5 C81 1.134(19) . ? C81 C82 1.48(3) . ? C78 C77 1.375(15) . ? C78 C79 1.387(15) . ? C78 H78A 0.9300 . ? C77 H77A 0.9300 . ? C79 C80 1.415(15) . ? C79 H79A 0.9300 . ? C80 H80A 0.9300 . ? 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 O2 Ni1 O6 87.6(5) . . ? O2 Ni1 O1 91.5(4) . . ? O6 Ni1 O1 94.9(4) . . ? O2 Ni1 N1 91.5(5) . . ? O6 Ni1 N1 172.6(4) . . ? O1 Ni1 N1 92.4(5) . . ? O2 Ni1 N2 87.3(5) . . ? O6 Ni1 N2 97.0(5) . . ? O1 Ni1 N2 168.0(6) . . ? N1 Ni1 N2 75.6(6) . . ? O2 Ni1 N5 172.9(5) . . ? O6 Ni1 N5 86.2(5) . . ? O1 Ni1 N5 85.5(4) . . ? N1 Ni1 N5 95.0(5) . . ? N2 Ni1 N5 96.9(5) . . ? O1 Ni2 O3 94.0(4) . . ? O1 Ni2 N3 93.3(5) . . ? O3 Ni2 N3 172.7(5) . . ? O1 Ni2 O7 88.0(5) . . ? O3 Ni2 O7 93.2(5) . . ? N3 Ni2 O7 88.0(5) . . ? O1 Ni2 N4 170.8(5) . . ? O3 Ni2 N4 90.4(5) . . ? N3 Ni2 N4 82.5(5) . . ? O7 Ni2 N4 83.7(5) . . ? O1 Ni2 N6 90.6(6) . . ? O3 Ni2 N6 89.6(6) . . ? N3 Ni2 N6 89.4(6) . . ? O7 Ni2 N6 177.0(6) . . ? N4 Ni2 N6 97.5(6) . . ? O3 P1 O2 121.1(7) . . ? O3 P1 O4 105.2(7) . . ? O2 P1 O4 108.9(7) . . ? O3 P1 O5 109.9(7) . . ? O2 P1 O5 106.7(7) . . ? O4 P1 O5 103.7(6) . . ? O6 P2 O7 120.2(7) . . ? O6 P2 O8 106.4(7) . . ? O7 P2 O8 109.7(8) . . ? O6 P2 O9 110.9(7) . . ? O7 P2 O9 105.6(6) . . ? O8 P2 O9 102.8(7) . . ? C1 O1 Ni2 119.7(9) . . ? C1 O1 Ni1 113.9(9) . . ? Ni2 O1 Ni1 126.1(6) . . ? C3 C2 C1 117.2(16) . . ? C3 C2 C14 121.1(15) . . ? C1 C2 C14 121.7(16) . . ? C5 C6 C1 120.5(16) . . ? C5 C6 C7 121.4(16) . . ? C1 C6 C7 118.1(17) . . ? O1 C1 C6 121.4(15) . . ? O1 C1 C2 119.3(15) . . ? C6 C1 C2 119.2(17) . . ? C5 C4 C3 119.6(17) . . ? C5 C4 Br1 122.3(15) . . ? C3 C4 Br1 118.2(14) . . ? C4 C5 C6 121.7(17) . . ? C4 C5 H5A 119.1 . . ? C6 C5 H5A 119.1 . . ? C2 C3 C4 121.7(15) . . ? C2 C3 H3A 119.1 . . ? C4 C3 H3A 119.1 . . ? P2 O6 Ni1 128.8(6) . . ? P1 O2 Ni1 130.4(6) . . ? P1 O3 Ni2 135.2(8) . . ? P2 O7 Ni2 131.9(6) . . ? C10 N1 C7 108.4(13) . . ? C10 N1 C8 108.7(12) . . ? C7 N1 C8 111.0(13) . . ? C10 N1 Ni1 112.2(10) . . ? C7 N1 Ni1 111.1(9) . . ? C8 N1 Ni1 105.4(11) . . ? C39 O9 P2 122.1(10) . . ? C27 O5 P1 118.3(14) . . ? C75 O8 P2 125.7(14) . . ? C21 O4 P1 122.4(15) . . ? C12 N2 C13 109.9(18) . . ? C12 N2 C9 109.7(15) . . ? C13 N2 C9 106.4(15) . . ? C12 N2 Ni1 111.7(11) . . ? C13 N2 Ni1 113.2(12) . . ? C9 N2 Ni1 105.7(11) . . ? N2 C9 C8 109.4(13) . . ? N2 C9 H9A 109.8 . . ? C8 C9 H9A 109.8 . . ? N2 C9 H9B 109.8 . . ? C8 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? C12 C11 C10 118.7(17) . . ? C12 C11 H11A 107.6 . . ? C10 C11 H11A 107.6 . . ? C12 C11 H11B 107.6 . . ? C10 C11 H11B 107.6 . . ? H11A C11 H11B 107.1 . . ? N1 C8 C9 111.3(15) . . ? N1 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? N1 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? N2 C12 C11 114.1(19) . . ? N2 C12 H12A 108.7 . . ? C11 C12 H12A 108.7 . . ? N2 C12 H12B 108.7 . . ? C11 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? N1 C10 C11 112.2(15) . . ? N1 C10 H10A 109.2 . . ? C11 C10 H10A 109.2 . . ? N1 C10 H10B 109.2 . . ? C11 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? N1 C7 C6 111.7(12) . . ? N1 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? N1 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? C15 N3 C14 113.5(13) . . ? C15 N3 Ni2 105.8(10) . . ? C14 N3 Ni2 110.5(9) . . ? C20 N4 C16 112.8(15) . . ? C20 N4 Ni2 122.8(11) . . ? C16 N4 Ni2 108.8(11) . . ? C20 N4 H4A 103.4 . . ? C16 N4 H4A 103.4 . . ? Ni2 N4 H4A 103.4 . . ? C2 C14 N3 108.6(14) . . ? C2 C14 H14A 110.0 . . ? N3 C14 H14A 110.0 . . ? C2 C14 H14B 110.0 . . ? N3 C14 H14B 110.0 . . ? H14A C14 H14B 108.3 . . ? C15 C16 N4 109.2(14) . . ? C15 C16 C17 117.2(17) . . ? N4 C16 C17 108.9(16) . . ? C15 C16 H16A 107.0 . . ? N4 C16 H16A 107.0 . . ? C17 C16 H16A 107.0 . . ? N3 C15 C16 108.0(15) . . ? N3 C15 H15A 110.1 . . ? C16 C15 H15A 110.1 . . ? N3 C15 H15B 110.1 . . ? C16 C15 H15B 110.1 . . ? H15A C15 H15B 108.4 . . ? N2 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C18 C17 C16 109.9(19) . . ? C18 C17 H17A 109.7 . . ? C16 C17 H17A 109.7 . . ? C18 C17 H17B 109.7 . . ? C16 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? C19 C18 C17 111.6(19) . . ? C19 C18 H18A 109.3 . . ? C17 C18 H18A 109.3 . . ? C19 C18 H18B 109.3 . . ? C17 C18 H18B 109.3 . . ? H18A C18 H18B 108.0 . . ? C18 C19 C20 109(2) . . ? C18 C19 H19A 109.8 . . ? C20 C19 H19A 109.8 . . ? C18 C19 H19B 109.8 . . ? C20 C19 H19B 109.8 . . ? H19A C19 H19B 108.2 . . ? N4 C20 C19 114.8(18) . . ? N4 C20 H20A 108.6 . . ? C19 C20 H20A 108.6 . . ? N4 C20 H20B 108.6 . . ? C19 C20 H20B 108.6 . . ? H20A C20 H20B 107.6 . . ? C32 C27 C28 120(3) . . ? C32 C27 O5 120(2) . . ? C28 C27 O5 119(2) . . ? C26 C21 C22 118(3) . . ? C26 C21 O4 123(2) . . ? C22 C21 O4 117(2) . . ? C27 C28 C29 121(3) . . ? C27 C28 H28A 119.5 . . ? C29 C28 H28A 119.5 . . ? C30 C29 C28 118(3) . . ? C30 C29 H29A 120.8 . . ? C28 C29 H29A 120.8 . . ? C23 C22 C21 122(3) . . ? C23 C22 H22A 119.0 . . ? C21 C22 H22A 119.0 . . ? C45 B1 C57 112.4(14) . . ? C45 B1 C63 104.1(13) . . ? C57 B1 C63 114.9(16) . . ? C45 B1 C51 111.2(15) . . ? C57 B1 C51 102.6(13) . . ? C63 B1 C51 112.0(13) . . ? C29 C30 C31 120(3) . . ? C29 C30 H30A 119.8 . . ? C31 C30 H30A 119.8 . . ? C24 C23 C22 117(3) . . ? C24 C23 H23A 121.6 . . ? C22 C23 H23A 121.6 . . ? C24 C25 C26 115(3) . . ? C24 C25 H25A 122.4 . . ? C26 C25 H25A 122.4 . . ? C23 C24 C25 125(3) . . ? C23 C24 H24A 117.5 . . ? C25 C24 H24A 117.5 . . ? C21 C26 C25 123(3) . . ? C21 C26 H26A 118.6 . . ? C25 C26 H26A 118.6 . . ? C30 C31 C32 120(3) . . ? C30 C31 H31A 120.2 . . ? C32 C31 H31A 120.2 . . ? C46 C45 C50 114.2(17) . . ? C46 C45 B1 123.1(15) . . ? C50 C45 B1 122.3(16) . . ? C57 C62 C61 122(2) . . ? C57 C62 H62A 118.9 . . ? C61 C62 H62A 118.9 . . ? C54 C53 C52 120(2) . . ? C54 C53 H53A 120.1 . . ? C52 C53 H53A 120.1 . . ? C45 C50 C49 121.6(18) . . ? C45 C50 H50A 119.2 . . ? C49 C50 H50A 119.2 . . ? C51 C56 C55 123(2) . . ? C51 C56 H56A 118.5 . . ? C55 C56 H56A 118.5 . . ? C46 C47 C48 118(2) . . ? C46 C47 H47A 121.2 . . ? C48 C47 H47A 121.2 . . ? C56 C51 C52 115.5(17) . . ? C56 C51 B1 118.6(18) . . ? C52 C51 B1 125.8(17) . . ? C68 C63 C64 115.7(15) . . ? C68 C63 B1 118.0(14) . . ? C64 C63 B1 126.1(14) . . ? C65 C64 C63 123.5(17) . . ? C65 C64 H64A 118.3 . . ? C63 C64 H64A 118.3 . . ? C63 C68 C67 120.5(16) . . ? C63 C68 H68A 119.8 . . ? C67 C68 H68A 119.8 . . ? C57 C58 C59 122(2) . . ? C57 C58 H58A 119.1 . . ? C59 C58 H58A 119.1 . . ? C49 C48 C47 119(2) . . ? C49 C48 H48A 120.7 . . ? C47 C48 H48A 120.7 . . ? C62 C57 C58 114.0(19) . . ? C62 C57 B1 119.9(18) . . ? C58 C57 B1 126.1(17) . . ? C51 C52 C53 121(2) . . ? C51 C52 H52A 119.4 . . ? C53 C52 H52A 119.4 . . ? C53 C54 C55 123(3) . . ? C53 C54 H54A 118.7 . . ? C55 C54 H54A 118.7 . . ? C48 C49 C50 121.1(18) . . ? C48 C49 H49A 119.4 . . ? C50 C49 H49A 119.4 . . ? C47 C46 C45 126.6(18) . . ? C47 C46 H46A 116.7 . . ? C45 C46 H46A 116.7 . . ? C60 C59 C58 124(3) . . ? C60 C59 H59A 117.8 . . ? C58 C59 H59A 117.8 . . ? C66 C67 C68 122.7(17) . . ? C66 C67 H67A 118.7 . . ? C68 C67 H67A 118.7 . . ? C67 C66 C65 116.4(18) . . ? C67 C66 H66A 121.8 . . ? C65 C66 H66A 121.8 . . ? C64 C65 C66 121.2(19) . . ? C64 C65 H65A 119.4 . . ? C66 C65 H65A 119.4 . . ? C54 C55 C56 118(2) . . ? C54 C55 H55A 121.1 . . ? C56 C55 H55A 121.1 . . ? C60 C61 C62 121(2) . . ? C60 C61 H61A 119.3 . . ? C62 C61 H61A 119.3 . . ? C59 C60 C61 116(2) . . ? C59 C60 H60A 121.9 . . ? C61 C60 H60A 121.9 . . ? C44 C39 C40 122(2) . . ? C44 C39 O9 112(2) . . ? C40 C39 O9 125(2) . . ? C39 C40 C41 120(3) . . ? C39 C40 H40A 120.0 . . ? C41 C40 H40A 120.0 . . ? C39 C44 C43 116(3) . . ? C39 C44 H44A 121.9 . . ? C43 C44 H44A 121.9 . . ? C43 C42 C41 119(3) . . ? C43 C42 H42A 120.4 . . ? C41 C42 H42A 120.4 . . ? C42 C41 C40 119(3) . . ? C42 C41 H41A 120.5 . . ? C40 C41 H41A 120.5 . . ? C27 C32 C31 118(3) . . ? C27 C32 H32A 121.1 . . ? C31 C32 H32A 121.1 . . ? C76 C75 C80 123(3) . . ? C76 C75 O8 121(2) . . ? C80 C75 O8 115(2) . . ? C75 C76 C77 129(3) . . ? C75 C76 H76A 115.5 . . ? C77 C76 H76A 115.5 . . ? C42 C43 C44 123(4) . . ? C42 C43 H43A 118.7 . . ? C44 C43 H43A 118.7 . . ? C83 N6 Ni2 173.8(16) . . ? N6 C83 C84 178(2) . . ? C81 N5 Ni1 165.1(14) . . ? N5 C81 C82 178(2) . . ? C77 C78 C79 133(3) . . ? C77 C78 H78A 113.7 . . ? C79 C78 H78A 113.7 . . ? C76 C77 C78 101(3) . . ? C76 C77 H77A 129.6 . . ? C78 C77 H77A 129.6 . . ? C78 C79 C80 115(3) . . ? C78 C79 H79A 122.3 . . ? C80 C79 H79A 122.3 . . ? C75 C80 C79 111(3) . . ? C75 C80 H80A 124.4 . . ? C79 C80 H80A 124.4 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.947 _refine_diff_density_min -0.736 _refine_diff_density_rms 0.094