data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Fondo, Matilde' 'Ocampo, Noelia' 'Garcia-Deibe, Ana' 'Cano, Joan' 'Sanmartin, Jesus' _publ_contact_author_name 'Fondo, Matilde' _publ_contact_author_email matilde.fondo@usc.es _publ_section_title ; ne pot-synthesis of chiral Ni6 clusters involving Ni3 subunits: a combined structural, magnetic and DFT study ; # Attachment '- cif.cif' data_1.7.5H2O _database_code_depnum_ccdc_archive 'CCDC 781532' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H69 Cl N8 Ni6 O16, 4(H2 O), 3.5 O' _chemical_formula_sum 'C60 H77 Cl N8 Ni6 O23.50' _chemical_formula_weight 1674.01 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.863(4) _cell_length_b 17.737(4) _cell_length_c 22.319(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.681(3) _cell_angle_gamma 90.00 _cell_volume 7452(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1489 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 27.05 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3464 _exptl_absorpt_coefficient_mu 1.597 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4150 _exptl_absorpt_correction_T_max 0.5993 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker CCD SMART1000 ' _diffrn_measurement_method 'omega/phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63329 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6947 _reflns_number_gt 6138 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'Wingx 1.70.01 (Farrugia, 1999)' _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^)+(0.0534P)^2^+29.9619P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6947 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.1007 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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 Ni11 Ni 0.711845(18) 0.14576(2) 0.753267(15) 0.01484(10) Uani 1 1 d . . . Ni12 Ni 0.600912(19) 0.03590(2) 0.701436(15) 0.01535(10) Uani 1 1 d . . . Ni13 Ni 0.582110(18) 0.236964(19) 0.762282(15) 0.01208(10) Uani 1 1 d . . . Cl1 Cl 0.5000 -0.02109(6) 0.7500 0.0206(2) Uani 1 2 d S . . O101 O 0.67596(10) 0.24553(11) 0.72137(9) 0.0158(4) Uani 1 1 d . . . O102 O 0.53464(11) 0.09366(11) 0.64210(9) 0.0176(4) Uani 1 1 d . . . O103 O 0.68506(10) 0.09371(11) 0.67110(8) 0.0165(4) Uani 1 1 d . . . N101 N 0.80898(13) 0.17013(14) 0.72775(11) 0.0197(5) Uani 1 1 d . . . N102 N 0.59492(14) -0.05249(14) 0.64364(11) 0.0207(5) Uani 1 1 d . . . N103 N 0.76142(13) 0.04647(15) 0.78660(11) 0.0206(5) Uani 1 1 d . . . N104 N 0.67768(14) -0.03922(14) 0.75082(11) 0.0208(5) Uani 1 1 d . . . O3W O 0.51095(10) 0.21935(12) 0.68946(9) 0.0134(4) Uani 1 1 d . . . O1H O 0.60744(10) 0.12356(11) 0.76367(9) 0.0151(4) Uani 1 1 d . . . O13 O 0.63503(10) 0.26110(11) 0.84249(9) 0.0171(4) Uani 1 1 d . . . O11 O 0.73444(11) 0.19306(12) 0.83738(9) 0.0206(4) Uani 1 1 d . . . O31 O 0.55961(10) 0.34811(11) 0.75589(9) 0.0152(4) Uani 1 1 d . . . C10 C 0.69528(15) 0.23823(16) 0.86275(13) 0.0179(6) Uani 1 1 d . . . C11 C 0.72095(18) 0.26802(19) 0.92382(14) 0.0260(7) Uani 1 1 d . . . H11A H 0.7678 0.2468 0.9353 0.039 Uiso 1 1 calc R . . H11B H 0.6874 0.2534 0.9535 0.039 Uiso 1 1 calc R . . H11C H 0.7243 0.3231 0.9222 0.039 Uiso 1 1 calc R . . C30 C 0.5000 0.3796(2) 0.7500 0.0166(8) Uani 1 2 d S . . C31 C 0.5000 0.4648(3) 0.7500 0.0363(13) Uani 1 2 d S . . H31A H 0.5456 0.4832 0.7370 0.054 Uiso 0.50 1 calc PR . . H31B H 0.4931 0.4832 0.7906 0.054 Uiso 0.50 1 calc PR . . H31C H 0.4614 0.4832 0.7223 0.054 Uiso 0.50 1 calc PR . . C100 C 0.69786(15) 0.27524(15) 0.67195(12) 0.0149(6) Uani 1 1 d . . . C101 C 0.65442(16) 0.32674(16) 0.63846(13) 0.0180(6) Uani 1 1 d . . . H101 H 0.6101 0.3413 0.6529 0.022 Uiso 1 1 calc R . . C102 C 0.67483(18) 0.35644(17) 0.58518(14) 0.0237(7) Uani 1 1 d . . . H102 H 0.6439 0.3903 0.5633 0.028 Uiso 1 1 calc R . . C103 C 0.74001(19) 0.33780(18) 0.56278(14) 0.0274(7) Uani 1 1 d . . . H103 H 0.7533 0.3578 0.5256 0.033 Uiso 1 1 calc R . . C104 C 0.78445(17) 0.28981(18) 0.59584(14) 0.0244(7) Uani 1 1 d . . . H104 H 0.8293 0.2778 0.5813 0.029 Uiso 1 1 calc R . . C105 C 0.76594(16) 0.25772(16) 0.65040(13) 0.0184(6) Uani 1 1 d . . . C106 C 0.81843(16) 0.20966(17) 0.68097(13) 0.0205(6) Uani 1 1 d . . . H106 H 0.8639 0.2072 0.6650 0.025 Uiso 1 1 calc R . . C107 C 0.86523(16) 0.11940(19) 0.75162(15) 0.0255(7) Uani 1 1 d . . . H10A H 0.9063 0.1491 0.7685 0.031 Uiso 1 1 calc R . . H10B H 0.8815 0.0870 0.7191 0.031 Uiso 1 1 calc R . . C108 C 0.83549(16) 0.07037(19) 0.80095(14) 0.0259(7) Uani 1 1 d . . . H10C H 0.8657 0.0250 0.8071 0.031 Uiso 1 1 calc R . . H10D H 0.8379 0.0991 0.8391 0.031 Uiso 1 1 calc R . . C109 C 0.72819(17) 0.01762(18) 0.84120(13) 0.0240(7) Uani 1 1 d . . . H10E H 0.7061 0.0593 0.8629 0.029 Uiso 1 1 calc R . . H10F H 0.7640 -0.0075 0.8688 0.029 Uiso 1 1 calc R . . C110 C 0.67246(18) -0.03815(18) 0.81740(13) 0.0248(7) Uani 1 1 d . . . H11D H 0.6820 -0.0889 0.8346 0.030 Uiso 1 1 calc R . . H11E H 0.6245 -0.0219 0.8276 0.030 Uiso 1 1 calc R . . C111 C 0.66084(18) -0.11489(17) 0.72592(15) 0.0260(7) Uani 1 1 d . . . H11F H 0.6187 -0.1352 0.7447 0.031 Uiso 1 1 calc R . . H11G H 0.7012 -0.1492 0.7360 0.031 Uiso 1 1 calc R . . C112 C 0.64609(18) -0.11286(17) 0.65823(15) 0.0258(7) Uani 1 1 d . . . H11H H 0.6907 -0.1033 0.6384 0.031 Uiso 1 1 calc R . . H11I H 0.6265 -0.1619 0.6438 0.031 Uiso 1 1 calc R . . C113 C 0.54399(17) -0.06511(17) 0.60422(13) 0.0230(6) Uani 1 1 d . . . H113 H 0.5430 -0.1133 0.5855 0.028 Uiso 1 1 calc R . . C114 C 0.48779(16) -0.01308(17) 0.58538(13) 0.0209(6) Uani 1 1 d . . . C115 C 0.43413(18) -0.04086(19) 0.54467(14) 0.0261(7) Uani 1 1 d . . . H115 H 0.4358 -0.0920 0.5322 0.031 Uiso 1 1 calc R . . C116 C 0.37911(18) 0.0042(2) 0.52233(14) 0.0281(7) Uani 1 1 d . . . H116 H 0.3429 -0.0157 0.4953 0.034 Uiso 1 1 calc R . . C117 C 0.37736(17) 0.07904(19) 0.53989(13) 0.0245(7) Uani 1 1 d . . . H117 H 0.3401 0.1108 0.5241 0.029 Uiso 1 1 calc R . . C118 C 0.42924(16) 0.10819(18) 0.58011(13) 0.0211(6) Uani 1 1 d . . . H118 H 0.4268 0.1597 0.5916 0.025 Uiso 1 1 calc R . . C119 C 0.48539(15) 0.06324(17) 0.60434(12) 0.0178(6) Uani 1 1 d . . . C120 C 0.75368(16) -0.01910(17) 0.74517(13) 0.0209(6) Uani 1 1 d . . . H120 H 0.7841 -0.0613 0.7619 0.025 Uiso 1 1 calc R . . C121 C 0.77369(16) -0.00238(17) 0.68239(13) 0.0196(6) Uani 1 1 d . . . C122 C 0.82841(16) -0.04316(17) 0.65855(14) 0.0224(6) Uani 1 1 d . . . H122 H 0.8518 -0.0818 0.6817 0.027 Uiso 1 1 calc R . . C123 C 0.84888(17) -0.02752(18) 0.60109(14) 0.0258(7) Uani 1 1 d . . . H123 H 0.8863 -0.0551 0.5849 0.031 Uiso 1 1 calc R . . C124 C 0.81381(17) 0.02898(18) 0.56770(14) 0.0253(7) Uani 1 1 d . . . H124 H 0.8277 0.0401 0.5285 0.030 Uiso 1 1 calc R . . C125 C 0.75879(16) 0.06928(17) 0.59093(13) 0.0198(6) Uani 1 1 d . . . H125 H 0.7354 0.1077 0.5675 0.024 Uiso 1 1 calc R . . C126 C 0.73744(15) 0.05391(16) 0.64860(13) 0.0167(6) Uani 1 1 d . . . H1H H 0.601(2) 0.105(2) 0.7922(18) 0.028(11) Uiso 1 1 d . . . H3W1 H 0.5097(18) 0.251(2) 0.6639(16) 0.016(9) Uiso 1 1 d . . . H3W2 H 0.516(2) 0.173(3) 0.6729(19) 0.042(12) Uiso 1 1 d . . . O1W O 0.47794(13) 0.32815(14) 0.60565(12) 0.0248(5) Uani 1 1 d . . . H1W1 H 0.442(3) 0.318(3) 0.615(2) 0.044(16) Uiso 1 1 d . . . H1W2 H 0.481(3) 0.313(3) 0.575(2) 0.045(16) Uiso 1 1 d . . . O2W O 0.61071(12) 0.17837(12) 0.55532(10) 0.0259(5) Uani 1 1 d . . . H2W1 H 0.6051 0.1546 0.5813 0.040 Uiso 1 1 d . . . H2W2 H 0.5736 0.1971 0.5364 0.040 Uiso 1 1 d . . . O4W O 0.5020(3) 0.2609(4) 0.4967(3) 0.0283(15) Uiso 0.50 1 d P A 1 O5W O 0.5253(3) 0.2954(4) 0.4477(3) 0.0318(14) Uiso 0.50 1 d P B 2 O6W O 0.4932(5) 0.2392(6) 0.4951(4) 0.024(2) Uiso 0.25 1 d P C 3 O7W O 0.5453(12) 0.2372(13) 0.4475(10) 0.027(5) Uiso 0.10 1 d P D 4 O8W O 0.4675(6) 0.3439(7) 0.4210(5) 0.024(2) Uiso 0.20 1 d P E 5 O9W' O 0.4806(13) 0.3747(15) 0.4355(11) 0.027(5) Uiso 0.10 1 d P F 6 O9W" O 0.4595(11) 0.3628(12) 0.4780(9) 0.020(4) Uiso 0.10 1 d P G 7 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 Ni11 0.01510(19) 0.0168(2) 0.01251(18) 0.00036(13) 0.00005(13) 0.00355(13) Ni12 0.0197(2) 0.01248(19) 0.01402(19) -0.00034(13) 0.00195(14) 0.00234(14) Ni13 0.01363(18) 0.01203(19) 0.01046(18) -0.00044(12) -0.00015(13) 0.00094(13) Cl1 0.0248(5) 0.0160(5) 0.0218(5) 0.000 0.0068(4) 0.000 O101 0.0170(10) 0.0171(10) 0.0135(9) 0.0010(8) 0.0021(7) 0.0009(8) O102 0.0218(10) 0.0150(10) 0.0157(10) -0.0033(8) -0.0013(8) 0.0007(8) O103 0.0189(10) 0.0154(10) 0.0153(10) -0.0002(8) 0.0019(8) 0.0037(8) N101 0.0167(12) 0.0214(13) 0.0208(13) -0.0038(10) -0.0002(10) 0.0034(10) N102 0.0265(14) 0.0158(12) 0.0205(13) -0.0016(10) 0.0068(10) 0.0026(10) N103 0.0211(13) 0.0271(14) 0.0135(12) 0.0006(10) 0.0004(10) 0.0080(11) N104 0.0275(14) 0.0169(12) 0.0185(13) 0.0029(10) 0.0058(10) 0.0058(10) O3W 0.0167(10) 0.0121(10) 0.0115(9) 0.0015(8) 0.0002(7) 0.0000(8) O1H 0.0191(10) 0.0147(10) 0.0117(10) 0.0023(8) 0.0020(8) 0.0008(8) O13 0.0169(10) 0.0202(10) 0.0141(10) -0.0016(8) -0.0005(8) 0.0006(8) O31 0.0146(10) 0.0137(10) 0.0172(10) -0.0013(7) 0.0009(7) 0.0009(8) O11 0.0198(10) 0.0260(11) 0.0156(10) -0.0016(8) -0.0023(8) 0.0054(9) C10 0.0199(15) 0.0198(15) 0.0138(14) 0.0022(11) -0.0014(11) -0.0010(12) C11 0.0277(17) 0.0336(18) 0.0157(15) -0.0030(13) -0.0058(12) 0.0033(14) C30 0.019(2) 0.015(2) 0.0151(19) 0.000 0.0021(15) 0.000 C31 0.018(2) 0.015(2) 0.076(4) 0.000 0.002(2) 0.000 C100 0.0189(14) 0.0129(13) 0.0130(13) -0.0036(10) 0.0002(11) -0.0026(11) C101 0.0196(14) 0.0175(14) 0.0170(14) -0.0007(11) 0.0018(11) -0.0027(11) C102 0.0322(17) 0.0202(15) 0.0182(15) 0.0037(12) -0.0009(12) -0.0017(13) C103 0.0393(19) 0.0254(16) 0.0187(15) 0.0016(13) 0.0104(13) -0.0040(14) C104 0.0280(16) 0.0240(16) 0.0226(15) -0.0041(13) 0.0120(13) -0.0029(13) C105 0.0218(15) 0.0161(14) 0.0177(14) -0.0053(11) 0.0050(11) -0.0036(11) C106 0.0173(14) 0.0214(15) 0.0233(15) -0.0063(12) 0.0050(11) -0.0028(12) C107 0.0163(15) 0.0309(17) 0.0290(17) 0.0002(14) -0.0005(12) 0.0050(13) C108 0.0216(16) 0.0341(18) 0.0216(15) 0.0004(13) -0.0027(12) 0.0107(13) C109 0.0336(17) 0.0251(16) 0.0134(14) 0.0039(12) 0.0026(12) 0.0101(13) C110 0.0339(18) 0.0234(16) 0.0178(15) 0.0067(12) 0.0066(13) 0.0080(13) C111 0.0328(18) 0.0159(15) 0.0295(17) 0.0018(12) 0.0038(13) 0.0051(13) C112 0.0316(17) 0.0160(15) 0.0303(17) -0.0051(12) 0.0054(13) 0.0055(13) C113 0.0326(17) 0.0169(15) 0.0203(15) -0.0043(12) 0.0071(13) -0.0030(13) C114 0.0239(15) 0.0218(15) 0.0174(14) -0.0046(12) 0.0044(12) -0.0040(12) C115 0.0329(18) 0.0257(17) 0.0198(15) -0.0075(12) 0.0028(13) -0.0067(14) C116 0.0299(17) 0.0368(19) 0.0174(15) -0.0074(13) -0.0005(13) -0.0106(14) C117 0.0224(15) 0.0338(18) 0.0170(14) -0.0016(13) 0.0000(12) -0.0026(13) C118 0.0254(16) 0.0219(15) 0.0158(14) -0.0028(11) -0.0003(12) -0.0013(12) C119 0.0214(15) 0.0206(15) 0.0117(13) -0.0025(11) 0.0043(11) -0.0033(12) C120 0.0245(15) 0.0181(15) 0.0203(15) 0.0023(12) 0.0027(12) 0.0086(12) C121 0.0234(15) 0.0188(15) 0.0167(14) 0.0009(11) 0.0015(11) 0.0039(12) C122 0.0228(15) 0.0197(15) 0.0247(16) 0.0011(12) 0.0013(12) 0.0075(12) C123 0.0263(16) 0.0265(17) 0.0256(16) -0.0001(13) 0.0085(13) 0.0099(13) C124 0.0294(17) 0.0283(17) 0.0190(15) 0.0021(13) 0.0090(13) 0.0066(13) C125 0.0243(15) 0.0193(15) 0.0157(14) 0.0016(11) 0.0007(11) 0.0036(12) C126 0.0178(14) 0.0154(14) 0.0169(14) -0.0019(11) 0.0005(11) 0.0030(11) O1W 0.0217(13) 0.0292(13) 0.0239(13) 0.0083(10) 0.0051(10) 0.0038(10) O2W 0.0343(13) 0.0224(11) 0.0206(11) 0.0019(9) -0.0012(9) -0.0005(9) _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 Ni11 N101 2.000(3) . ? Ni11 O101 2.009(2) . ? Ni11 O1H 2.036(2) . ? Ni11 O11 2.075(2) . ? Ni11 O103 2.086(2) . ? Ni11 N103 2.107(3) . ? Ni11 Ni13 2.9511(7) . ? Ni12 N102 2.029(3) . ? Ni12 O102 2.038(2) . ? Ni12 O103 2.041(2) . ? Ni12 O1H 2.083(2) . ? Ni12 N104 2.209(3) . ? Ni12 Cl1 2.4668(6) . ? Ni13 O31 2.020(2) . ? Ni13 O13 2.038(2) . ? Ni13 O101 2.049(2) . ? Ni13 O3W 2.064(2) . ? Ni13 O1H 2.067(2) . ? Ni13 O3W 2.140(2) 2_656 ? Cl1 Ni12 2.4668(6) 2_656 ? O101 C100 1.313(3) . ? O102 C119 1.328(3) . ? O103 C126 1.338(3) . ? N101 C106 1.280(4) . ? N101 C107 1.465(4) . ? N102 C113 1.280(4) . ? N102 C112 1.464(4) . ? N103 C108 1.475(4) . ? N103 C120 1.487(4) . ? N103 C109 1.496(4) . ? N104 C111 1.479(4) . ? N104 C120 1.491(4) . ? N104 C110 1.496(4) . ? O3W Ni13 2.140(2) 2_656 ? O3W H3W1 0.80(4) . ? O3W H3W2 0.90(5) . ? O1H H1H 0.73(4) . ? O13 C10 1.263(4) . ? O31 C30 1.255(3) . ? O11 C10 1.250(4) . ? C10 C11 1.512(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C30 O31 1.255(3) 2_656 ? C30 C31 1.512(6) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C100 C101 1.409(4) . ? C100 C105 1.434(4) . ? C101 C102 1.378(4) . ? C101 H101 0.9500 . ? C102 C103 1.396(5) . ? C102 H102 0.9500 . ? C103 C104 1.376(5) . ? C103 H103 0.9500 . ? C104 C105 1.408(4) . ? C104 H104 0.9500 . ? C105 C106 1.444(4) . ? C106 H106 0.9500 . ? C107 C108 1.537(5) . ? C107 H10A 0.9900 . ? C107 H10B 0.9900 . ? C108 H10C 0.9900 . ? C108 H10D 0.9900 . ? C109 C110 1.515(5) . ? C109 H10E 0.9900 . ? C109 H10F 0.9900 . ? C110 H11D 0.9900 . ? C110 H11E 0.9900 . ? C111 C112 1.519(5) . ? C111 H11F 0.9900 . ? C111 H11G 0.9900 . ? C112 H11H 0.9900 . ? C112 H11I 0.9900 . ? C113 C114 1.448(5) . ? C113 H113 0.9500 . ? C114 C115 1.405(4) . ? C114 C119 1.420(4) . ? C115 C116 1.378(5) . ? C115 H115 0.9500 . ? C116 C117 1.384(5) . ? C116 H116 0.9500 . ? C117 C118 1.385(4) . ? C117 H117 0.9500 . ? C118 C119 1.406(4) . ? C118 H118 0.9500 . ? C120 C121 1.504(4) . ? C120 H120 1.0000 . ? C121 C122 1.394(4) . ? C121 C126 1.403(4) . ? C122 C123 1.391(4) . ? C122 H122 0.9500 . ? C123 C124 1.391(5) . ? C123 H123 0.9500 . ? C124 C125 1.388(4) . ? C124 H124 0.9500 . ? C125 C126 1.400(4) . ? C125 H125 0.9500 . ? O1W H1W1 0.75(5) . ? O1W H1W2 0.74(5) . ? O2W H2W1 0.7293 . ? O2W H2W2 0.8607 . ? 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 N101 Ni11 O101 90.15(9) . . ? N101 Ni11 O1H 169.87(9) . . ? O101 Ni11 O1H 84.51(8) . . ? N101 Ni11 O11 91.80(9) . . ? O101 Ni11 O11 90.54(8) . . ? O1H Ni11 O11 96.83(8) . . ? N101 Ni11 O103 91.14(9) . . ? O101 Ni11 O103 91.21(8) . . ? O1H Ni11 O103 80.40(8) . . ? O11 Ni11 O103 176.57(8) . . ? N101 Ni11 N103 83.53(10) . . ? O101 Ni11 N103 173.35(9) . . ? O1H Ni11 N103 102.04(9) . . ? O11 Ni11 N103 87.58(9) . . ? O103 Ni11 N103 91.00(9) . . ? N101 Ni11 Ni13 132.81(8) . . ? O101 Ni11 Ni13 43.88(6) . . ? O1H Ni11 Ni13 44.43(6) . . ? O11 Ni11 Ni13 80.78(6) . . ? O103 Ni11 Ni13 98.48(5) . . ? N103 Ni11 Ni13 141.74(7) . . ? N102 Ni12 O102 88.19(9) . . ? N102 Ni12 O103 100.95(9) . . ? O102 Ni12 O103 89.40(8) . . ? N102 Ni12 O1H 177.67(9) . . ? O102 Ni12 O1H 93.76(8) . . ? O103 Ni12 O1H 80.35(8) . . ? N102 Ni12 N104 81.90(10) . . ? O102 Ni12 N104 169.20(9) . . ? O103 Ni12 N104 88.27(9) . . ? O1H Ni12 N104 96.24(9) . . ? N102 Ni12 Cl1 87.11(7) . . ? O102 Ni12 Cl1 91.90(6) . . ? O103 Ni12 Cl1 171.87(6) . . ? O1H Ni12 Cl1 91.56(6) . . ? N104 Ni12 Cl1 91.90(7) . . ? O31 Ni13 O13 86.90(8) . . ? O31 Ni13 O101 94.58(8) . . ? O13 Ni13 O101 89.28(8) . . ? O31 Ni13 O3W 88.23(8) . . ? O13 Ni13 O3W 168.62(8) . . ? O101 Ni13 O3W 101.36(8) . . ? O31 Ni13 O1H 176.52(8) . . ? O13 Ni13 O1H 95.25(8) . . ? O101 Ni13 O1H 82.73(8) . . ? O3W Ni13 O1H 90.14(8) . . ? O31 Ni13 O3W 90.15(8) . 2_656 ? O13 Ni13 O3W 87.70(8) . 2_656 ? O101 Ni13 O3W 174.25(8) . 2_656 ? O3W Ni13 O3W 82.03(9) . 2_656 ? O1H Ni13 O3W 92.68(8) . 2_656 ? O31 Ni13 Ni11 134.56(6) . . ? O13 Ni13 Ni11 79.25(6) . . ? O101 Ni13 Ni11 42.81(6) . . ? O3W Ni13 Ni11 111.32(6) . . ? O1H Ni13 Ni11 43.59(6) . . ? O3W Ni13 Ni11 131.66(6) 2_656 . ? Ni12 Cl1 Ni12 131.61(5) . 2_656 ? C100 O101 Ni11 122.30(17) . . ? C100 O101 Ni13 137.03(18) . . ? Ni11 O101 Ni13 93.31(8) . . ? C119 O102 Ni12 125.67(18) . . ? C126 O103 Ni12 117.91(17) . . ? C126 O103 Ni11 114.86(17) . . ? Ni12 O103 Ni11 94.60(8) . . ? C106 N101 C107 119.8(3) . . ? C106 N101 Ni11 121.9(2) . . ? C107 N101 Ni11 114.8(2) . . ? C113 N102 C112 118.7(3) . . ? C113 N102 Ni12 125.5(2) . . ? C112 N102 Ni12 114.5(2) . . ? C108 N103 C120 114.4(2) . . ? C108 N103 C109 111.2(2) . . ? C120 N103 C109 102.1(2) . . ? C108 N103 Ni11 103.24(19) . . ? C120 N103 Ni11 114.24(18) . . ? C109 N103 Ni11 111.95(18) . . ? C111 N104 C120 111.7(2) . . ? C111 N104 C110 111.0(2) . . ? C120 N104 C110 101.9(2) . . ? C111 N104 Ni12 103.99(19) . . ? C120 N104 Ni12 114.62(18) . . ? C110 N104 Ni12 113.90(18) . . ? Ni13 O3W Ni13 95.42(8) . 2_656 ? Ni13 O3W H3W1 116(2) . . ? Ni13 O3W H3W1 106(2) 2_656 . ? Ni13 O3W H3W2 112(3) . . ? Ni13 O3W H3W2 117(3) 2_656 . ? H3W1 O3W H3W2 110(4) . . ? Ni11 O1H Ni13 91.97(8) . . ? Ni11 O1H Ni12 94.85(8) . . ? Ni13 O1H Ni12 135.44(11) . . ? Ni11 O1H H1H 114(3) . . ? Ni13 O1H H1H 113(3) . . ? Ni12 O1H H1H 104(3) . . ? C10 O13 Ni13 128.75(18) . . ? C30 O31 Ni13 128.6(2) . . ? C10 O11 Ni11 125.17(18) . . ? O11 C10 O13 126.0(3) . . ? O11 C10 C11 117.9(3) . . ? O13 C10 C11 116.1(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O31 C30 O31 127.2(4) . 2_656 ? O31 C30 C31 116.41(19) . . ? O31 C30 C31 116.41(19) 2_656 . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O101 C100 C101 120.2(3) . . ? O101 C100 C105 122.1(3) . . ? C101 C100 C105 117.7(3) . . ? C102 C101 C100 121.4(3) . . ? C102 C101 H101 119.3 . . ? C100 C101 H101 119.3 . . ? C101 C102 C103 121.3(3) . . ? C101 C102 H102 119.3 . . ? C103 C102 H102 119.3 . . ? C104 C103 C102 118.3(3) . . ? C104 C103 H103 120.8 . . ? C102 C103 H103 120.8 . . ? C103 C104 C105 122.5(3) . . ? C103 C104 H104 118.7 . . ? C105 C104 H104 118.7 . . ? C104 C105 C100 118.7(3) . . ? C104 C105 C106 116.5(3) . . ? C100 C105 C106 124.8(3) . . ? N101 C106 C105 125.6(3) . . ? N101 C106 H106 117.2 . . ? C105 C106 H106 117.2 . . ? N101 C107 C108 108.6(2) . . ? N101 C107 H10A 110.0 . . ? C108 C107 H10A 110.0 . . ? N101 C107 H10B 110.0 . . ? C108 C107 H10B 110.0 . . ? H10A C107 H10B 108.4 . . ? N103 C108 C107 113.0(2) . . ? N103 C108 H10C 109.0 . . ? C107 C108 H10C 109.0 . . ? N103 C108 H10D 109.0 . . ? C107 C108 H10D 109.0 . . ? H10C C108 H10D 107.8 . . ? N103 C109 C110 104.8(2) . . ? N103 C109 H10E 110.8 . . ? C110 C109 H10E 110.8 . . ? N103 C109 H10F 110.8 . . ? C110 C109 H10F 110.8 . . ? H10E C109 H10F 108.9 . . ? N104 C110 C109 105.6(2) . . ? N104 C110 H11D 110.6 . . ? C109 C110 H11D 110.6 . . ? N104 C110 H11E 110.6 . . ? C109 C110 H11E 110.6 . . ? H11D C110 H11E 108.8 . . ? N104 C111 C112 111.9(3) . . ? N104 C111 H11F 109.2 . . ? C112 C111 H11F 109.2 . . ? N104 C111 H11G 109.2 . . ? C112 C111 H11G 109.2 . . ? H11F C111 H11G 107.9 . . ? N102 C112 C111 108.3(2) . . ? N102 C112 H11H 110.0 . . ? C111 C112 H11H 110.0 . . ? N102 C112 H11I 110.0 . . ? C111 C112 H11I 110.0 . . ? H11H C112 H11I 108.4 . . ? N102 C113 C114 126.3(3) . . ? N102 C113 H113 116.9 . . ? C114 C113 H113 116.9 . . ? C115 C114 C119 119.4(3) . . ? C115 C114 C113 116.6(3) . . ? C119 C114 C113 123.9(3) . . ? C116 C115 C114 121.6(3) . . ? C116 C115 H115 119.2 . . ? C114 C115 H115 119.2 . . ? C115 C116 C117 119.0(3) . . ? C115 C116 H116 120.5 . . ? C117 C116 H116 120.5 . . ? C116 C117 C118 120.8(3) . . ? C116 C117 H117 119.6 . . ? C118 C117 H117 119.6 . . ? C117 C118 C119 121.4(3) . . ? C117 C118 H118 119.3 . . ? C119 C118 H118 119.3 . . ? O102 C119 C118 119.5(3) . . ? O102 C119 C114 122.8(3) . . ? C118 C119 C114 117.6(3) . . ? N103 C120 N104 101.0(2) . . ? N103 C120 C121 113.9(2) . . ? N104 C120 C121 115.2(2) . . ? N103 C120 H120 108.8 . . ? N104 C120 H120 108.8 . . ? C121 C120 H120 108.8 . . ? C122 C121 C126 120.8(3) . . ? C122 C121 C120 119.3(3) . . ? C126 C121 C120 119.9(3) . . ? C123 C122 C121 120.3(3) . . ? C123 C122 H122 119.8 . . ? C121 C122 H122 119.8 . . ? C124 C123 C122 119.2(3) . . ? C124 C123 H123 120.4 . . ? C122 C123 H123 120.4 . . ? C125 C124 C123 120.8(3) . . ? C125 C124 H124 119.6 . . ? C123 C124 H124 119.6 . . ? C124 C125 C126 120.6(3) . . ? C124 C125 H125 119.7 . . ? C126 C125 H125 119.7 . . ? O103 C126 C125 120.3(3) . . ? O103 C126 C121 121.3(3) . . ? C125 C126 C121 118.3(3) . . ? H1W1 O1W H1W2 106(5) . . ? H2W1 O2W H2W2 117.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N101 Ni11 Ni13 O31 -9.39(13) . . . . ? O101 Ni11 Ni13 O31 -26.05(11) . . . . ? O1H Ni11 Ni13 O31 -175.79(12) . . . . ? O11 Ni11 Ni13 O31 74.47(10) . . . . ? O103 Ni11 Ni13 O31 -108.92(10) . . . . ? N103 Ni11 Ni13 O31 148.51(14) . . . . ? N101 Ni11 Ni13 O13 -84.07(11) . . . . ? O101 Ni11 Ni13 O13 -100.73(10) . . . . ? O1H Ni11 Ni13 O13 109.54(10) . . . . ? O11 Ni11 Ni13 O13 -0.20(8) . . . . ? O103 Ni11 Ni13 O13 176.40(8) . . . . ? N103 Ni11 Ni13 O13 73.84(13) . . . . ? N101 Ni11 Ni13 O101 16.66(13) . . . . ? O1H Ni11 Ni13 O101 -149.73(12) . . . . ? O11 Ni11 Ni13 O101 100.52(10) . . . . ? O103 Ni11 Ni13 O101 -82.87(10) . . . . ? N103 Ni11 Ni13 O101 174.57(14) . . . . ? N101 Ni11 Ni13 O3W 100.34(12) . . . . ? O101 Ni11 Ni13 O3W 83.68(10) . . . . ? O1H Ni11 Ni13 O3W -66.05(11) . . . . ? O11 Ni11 Ni13 O3W -175.79(9) . . . . ? O103 Ni11 Ni13 O3W 0.81(8) . . . . ? N103 Ni11 Ni13 O3W -101.75(13) . . . . ? N101 Ni11 Ni13 O1H 166.39(13) . . . . ? O101 Ni11 Ni13 O1H 149.73(12) . . . . ? O11 Ni11 Ni13 O1H -109.74(10) . . . . ? O103 Ni11 Ni13 O1H 66.86(10) . . . . ? N103 Ni11 Ni13 O1H -35.70(14) . . . . ? N101 Ni11 Ni13 O3W -161.15(12) . . . 2_656 ? O101 Ni11 Ni13 O3W -177.81(11) . . . 2_656 ? O1H Ni11 Ni13 O3W 32.45(11) . . . 2_656 ? O11 Ni11 Ni13 O3W -77.29(10) . . . 2_656 ? O103 Ni11 Ni13 O3W 99.32(9) . . . 2_656 ? N103 Ni11 Ni13 O3W -3.25(14) . . . 2_656 ? N102 Ni12 Cl1 Ni12 -145.65(7) . . . 2_656 ? O102 Ni12 Cl1 Ni12 -57.56(6) . . . 2_656 ? O1H Ni12 Cl1 Ni12 36.26(6) . . . 2_656 ? N104 Ni12 Cl1 Ni12 132.56(7) . . . 2_656 ? N101 Ni11 O101 C100 37.5(2) . . . . ? O1H Ni11 O101 C100 -133.9(2) . . . . ? O11 Ni11 O101 C100 129.3(2) . . . . ? O103 Ni11 O101 C100 -53.7(2) . . . . ? Ni13 Ni11 O101 C100 -154.7(2) . . . . ? N101 Ni11 O101 Ni13 -167.86(9) . . . . ? O1H Ni11 O101 Ni13 20.76(8) . . . . ? O11 Ni11 O101 Ni13 -76.05(8) . . . . ? O103 Ni11 O101 Ni13 100.99(8) . . . . ? O31 Ni13 O101 C100 -50.4(3) . . . . ? O13 Ni13 O101 C100 -137.2(3) . . . . ? O3W Ni13 O101 C100 38.7(3) . . . . ? O1H Ni13 O101 C100 127.4(3) . . . . ? Ni11 Ni13 O101 C100 147.9(3) . . . . ? O31 Ni13 O101 Ni11 161.71(8) . . . . ? O13 Ni13 O101 Ni11 74.88(8) . . . . ? O3W Ni13 O101 Ni11 -109.19(8) . . . . ? O1H Ni13 O101 Ni11 -20.51(8) . . . . ? N102 Ni12 O102 C119 29.4(2) . . . . ? O103 Ni12 O102 C119 130.4(2) . . . . ? O1H Ni12 O102 C119 -149.3(2) . . . . ? N104 Ni12 O102 C119 52.9(6) . . . . ? Cl1 Ni12 O102 C119 -57.6(2) . . . . ? N102 Ni12 O103 C126 -33.6(2) . . . . ? O102 Ni12 O103 C126 -121.61(19) . . . . ? O1H Ni12 O103 C126 144.5(2) . . . . ? N104 Ni12 O103 C126 47.84(19) . . . . ? N102 Ni12 O103 Ni11 -154.89(9) . . . . ? O102 Ni12 O103 Ni11 117.06(8) . . . . ? O1H Ni12 O103 Ni11 23.15(8) . . . . ? N104 Ni12 O103 Ni11 -73.49(9) . . . . ? N101 Ni11 O103 C126 38.2(2) . . . . ? O101 Ni11 O103 C126 128.37(19) . . . . ? O1H Ni11 O103 C126 -147.41(19) . . . . ? N103 Ni11 O103 C126 -45.36(19) . . . . ? Ni13 Ni11 O103 C126 171.83(18) . . . . ? N101 Ni11 O103 Ni12 161.89(9) . . . . ? O101 Ni11 O103 Ni12 -107.94(8) . . . . ? O1H Ni11 O103 Ni12 -23.71(8) . . . . ? N103 Ni11 O103 Ni12 78.34(9) . . . . ? Ni13 Ni11 O103 Ni12 -64.47(6) . . . . ? O101 Ni11 N101 C106 -33.0(2) . . . . ? O1H Ni11 N101 C106 25.1(7) . . . . ? O11 Ni11 N101 C106 -123.5(2) . . . . ? O103 Ni11 N101 C106 58.2(2) . . . . ? N103 Ni11 N101 C106 149.1(2) . . . . ? Ni13 Ni11 N101 C106 -44.5(3) . . . . ? O101 Ni11 N101 C107 168.1(2) . . . . ? O1H Ni11 N101 C107 -133.8(5) . . . . ? O11 Ni11 N101 C107 77.5(2) . . . . ? O103 Ni11 N101 C107 -100.7(2) . . . . ? N103 Ni11 N101 C107 -9.8(2) . . . . ? Ni13 Ni11 N101 C107 156.63(17) . . . . ? O102 Ni12 N102 C113 -24.1(3) . . . . ? O103 Ni12 N102 C113 -113.2(3) . . . . ? N104 Ni12 N102 C113 160.2(3) . . . . ? Cl1 Ni12 N102 C113 67.8(3) . . . . ? O102 Ni12 N102 C112 169.2(2) . . . . ? O103 Ni12 N102 C112 80.1(2) . . . . ? N104 Ni12 N102 C112 -6.5(2) . . . . ? Cl1 Ni12 N102 C112 -98.8(2) . . . . ? N101 Ni11 N103 C108 28.96(18) . . . . ? O1H Ni11 N103 C108 -159.61(17) . . . . ? O11 Ni11 N103 C108 -63.14(18) . . . . ? O103 Ni11 N103 C108 119.99(18) . . . . ? Ni13 Ni11 N103 C108 -134.92(15) . . . . ? N101 Ni11 N103 C120 -95.9(2) . . . . ? O1H Ni11 N103 C120 75.5(2) . . . . ? O11 Ni11 N103 C120 172.0(2) . . . . ? O103 Ni11 N103 C120 -4.9(2) . . . . ? Ni13 Ni11 N103 C120 100.2(2) . . . . ? N101 Ni11 N103 C109 148.7(2) . . . . ? O1H Ni11 N103 C109 -39.9(2) . . . . ? O11 Ni11 N103 C109 56.6(2) . . . . ? O103 Ni11 N103 C109 -120.3(2) . . . . ? Ni13 Ni11 N103 C109 -15.2(3) . . . . ? N102 Ni12 N104 C111 -19.10(19) . . . . ? O102 Ni12 N104 C111 -42.8(6) . . . . ? O103 Ni12 N104 C111 -120.42(19) . . . . ? O1H Ni12 N104 C111 159.49(18) . . . . ? Cl1 Ni12 N104 C111 67.71(18) . . . . ? N102 Ni12 N104 C120 103.1(2) . . . . ? O102 Ni12 N104 C120 79.4(5) . . . . ? O103 Ni12 N104 C120 1.81(19) . . . . ? O1H Ni12 N104 C120 -78.3(2) . . . . ? Cl1 Ni12 N104 C120 -170.05(19) . . . . ? N102 Ni12 N104 C110 -140.1(2) . . . . ? O102 Ni12 N104 C110 -163.8(4) . . . . ? O103 Ni12 N104 C110 118.6(2) . . . . ? O1H Ni12 N104 C110 38.5(2) . . . . ? Cl1 Ni12 N104 C110 -53.3(2) . . . . ? O31 Ni13 O3W Ni13 -73.69(8) . . . 2_656 ? O13 Ni13 O3W Ni13 -9.0(5) . . . 2_656 ? O101 Ni13 O3W Ni13 -168.00(8) . . . 2_656 ? O1H Ni13 O3W Ni13 109.39(9) . . . 2_656 ? O3W Ni13 O3W Ni13 16.70(11) 2_656 . . 2_656 ? Ni11 Ni13 O3W Ni13 148.45(5) . . . 2_656 ? N101 Ni11 O1H Ni13 -79.0(5) . . . . ? O101 Ni11 O1H Ni13 -20.55(8) . . . . ? O11 Ni11 O1H Ni13 69.34(9) . . . . ? O103 Ni11 O1H Ni13 -112.71(8) . . . . ? N103 Ni11 O1H Ni13 158.32(8) . . . . ? N101 Ni11 O1H Ni12 56.9(5) . . . . ? O101 Ni11 O1H Ni12 115.38(9) . . . . ? O11 Ni11 O1H Ni12 -154.73(8) . . . . ? O103 Ni11 O1H Ni12 23.21(8) . . . . ? N103 Ni11 O1H Ni12 -65.76(10) . . . . ? Ni13 Ni11 O1H Ni12 135.93(11) . . . . ? O13 Ni13 O1H Ni11 -68.40(8) . . . . ? O101 Ni13 O1H Ni11 20.20(8) . . . . ? O3W Ni13 O1H Ni11 121.64(8) . . . . ? O3W Ni13 O1H Ni11 -156.34(8) 2_656 . . . ? O13 Ni13 O1H Ni12 -167.35(14) . . . . ? O101 Ni13 O1H Ni12 -78.75(15) . . . . ? O3W Ni13 O1H Ni12 22.69(15) . . . . ? O3W Ni13 O1H Ni12 104.71(15) 2_656 . . . ? Ni11 Ni13 O1H Ni12 -98.95(16) . . . . ? O102 Ni12 O1H Ni11 -112.50(9) . . . . ? O103 Ni12 O1H Ni11 -23.76(8) . . . . ? N104 Ni12 O1H Ni11 63.41(10) . . . . ? Cl1 Ni12 O1H Ni11 155.49(6) . . . . ? O102 Ni12 O1H Ni13 -14.72(15) . . . . ? O103 Ni12 O1H Ni13 74.03(15) . . . . ? N104 Ni12 O1H Ni13 161.19(15) . . . . ? Cl1 Ni12 O1H Ni13 -106.73(14) . . . . ? O31 Ni13 O13 C10 -135.2(2) . . . . ? O101 Ni13 O13 C10 -40.6(2) . . . . ? O3W Ni13 O13 C10 160.0(4) . . . . ? O1H Ni13 O13 C10 42.0(2) . . . . ? O3W Ni13 O13 C10 134.5(2) 2_656 . . . ? Ni11 Ni13 O13 C10 1.3(2) . . . . ? O13 Ni13 O31 C30 -122.37(17) . . . . ? O101 Ni13 O31 C30 148.60(16) . . . . ? O3W Ni13 O31 C30 47.34(16) . . . . ? O3W Ni13 O31 C30 -34.68(17) 2_656 . . . ? Ni11 Ni13 O31 C30 166.02(11) . . . . ? N101 Ni11 O11 C10 132.4(2) . . . . ? O101 Ni11 O11 C10 42.2(2) . . . . ? O1H Ni11 O11 C10 -42.3(2) . . . . ? N103 Ni11 O11 C10 -144.1(2) . . . . ? Ni13 Ni11 O11 C10 -0.7(2) . . . . ? Ni11 O11 C10 O13 2.0(4) . . . . ? Ni11 O11 C10 C11 -179.0(2) . . . . ? Ni13 O13 C10 O11 -2.4(4) . . . . ? Ni13 O13 C10 C11 178.6(2) . . . . ? Ni13 O31 C30 O31 -3.37(10) . . . 2_656 ? Ni13 O31 C30 C31 176.63(10) . . . . ? Ni11 O101 C100 C101 154.9(2) . . . . ? Ni13 O101 C100 C101 13.7(4) . . . . ? Ni11 O101 C100 C105 -25.7(3) . . . . ? Ni13 O101 C100 C105 -166.9(2) . . . . ? O101 C100 C101 C102 -177.4(3) . . . . ? C105 C100 C101 C102 3.3(4) . . . . ? C100 C101 C102 C103 -1.2(5) . . . . ? C101 C102 C103 C104 -1.2(5) . . . . ? C102 C103 C104 C105 1.5(5) . . . . ? C103 C104 C105 C100 0.6(5) . . . . ? C103 C104 C105 C106 -178.7(3) . . . . ? O101 C100 C105 C104 177.7(3) . . . . ? C101 C100 C105 C104 -2.9(4) . . . . ? O101 C100 C105 C106 -3.1(4) . . . . ? C101 C100 C105 C106 176.3(3) . . . . ? C107 N101 C106 C105 175.4(3) . . . . ? Ni11 N101 C106 C105 17.6(4) . . . . ? C104 C105 C106 N101 -173.1(3) . . . . ? C100 C105 C106 N101 7.7(5) . . . . ? C106 N101 C107 C108 -171.1(3) . . . . ? Ni11 N101 C107 C108 -11.7(3) . . . . ? C120 N103 C108 C107 80.5(3) . . . . ? C109 N103 C108 C107 -164.5(3) . . . . ? Ni11 N103 C108 C107 -44.3(3) . . . . ? N101 C107 C108 N103 38.7(4) . . . . ? C108 N103 C109 C110 -152.2(3) . . . . ? C120 N103 C109 C110 -29.8(3) . . . . ? Ni11 N103 C109 C110 92.8(2) . . . . ? C111 N104 C110 C109 147.2(3) . . . . ? C120 N104 C110 C109 28.1(3) . . . . ? Ni12 N104 C110 C109 -95.9(2) . . . . ? N103 C109 C110 N104 1.0(3) . . . . ? C120 N104 C111 C112 -82.5(3) . . . . ? C110 N104 C111 C112 164.5(3) . . . . ? Ni12 N104 C111 C112 41.6(3) . . . . ? C113 N102 C112 C111 -137.1(3) . . . . ? Ni12 N102 C112 C111 30.6(3) . . . . ? N104 C111 C112 N102 -49.3(4) . . . . ? C112 N102 C113 C114 178.3(3) . . . . ? Ni12 N102 C113 C114 12.1(4) . . . . ? N102 C113 C114 C115 -175.2(3) . . . . ? N102 C113 C114 C119 6.5(5) . . . . ? C119 C114 C115 C116 0.3(5) . . . . ? C113 C114 C115 C116 -178.1(3) . . . . ? C114 C115 C116 C117 0.9(5) . . . . ? C115 C116 C117 C118 -1.1(5) . . . . ? C116 C117 C118 C119 0.2(5) . . . . ? Ni12 O102 C119 C118 159.8(2) . . . . ? Ni12 O102 C119 C114 -22.3(4) . . . . ? C117 C118 C119 O102 179.0(3) . . . . ? C117 C118 C119 C114 1.0(4) . . . . ? C115 C114 C119 O102 -179.2(3) . . . . ? C113 C114 C119 O102 -0.9(4) . . . . ? C115 C114 C119 C118 -1.2(4) . . . . ? C113 C114 C119 C118 177.0(3) . . . . ? C108 N103 C120 N104 167.9(2) . . . . ? C109 N103 C120 N104 47.7(3) . . . . ? Ni11 N103 C120 N104 -73.4(2) . . . . ? C108 N103 C120 C121 -68.0(3) . . . . ? C109 N103 C120 C121 171.8(2) . . . . ? Ni11 N103 C120 C121 50.7(3) . . . . ? C111 N104 C120 N103 -165.4(2) . . . . ? C110 N104 C120 N103 -46.9(3) . . . . ? Ni12 N104 C120 N103 76.6(2) . . . . ? C111 N104 C120 C121 71.4(3) . . . . ? C110 N104 C120 C121 -170.0(2) . . . . ? Ni12 N104 C120 C121 -46.5(3) . . . . ? N103 C120 C121 C122 120.1(3) . . . . ? N104 C120 C121 C122 -123.8(3) . . . . ? N103 C120 C121 C126 -59.8(4) . . . . ? N104 C120 C121 C126 56.3(4) . . . . ? C126 C121 C122 C123 1.3(5) . . . . ? C120 C121 C122 C123 -178.6(3) . . . . ? C121 C122 C123 C124 -0.3(5) . . . . ? C122 C123 C124 C125 -0.3(5) . . . . ? C123 C124 C125 C126 0.1(5) . . . . ? Ni12 O103 C126 C125 125.4(2) . . . . ? Ni11 O103 C126 C125 -124.4(2) . . . . ? Ni12 O103 C126 C121 -56.5(3) . . . . ? Ni11 O103 C126 C121 53.7(3) . . . . ? C124 C125 C126 O103 179.0(3) . . . . ? C124 C125 C126 C121 0.9(4) . . . . ? C122 C121 C126 O103 -179.7(3) . . . . ? C120 C121 C126 O103 0.2(4) . . . . ? C122 C121 C126 C125 -1.5(4) . . . . ? C120 C121 C126 C125 178.3(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3W H3W1 O1W 0.80(4) 1.96(4) 2.731(3) 164(3) . O3W H3W2 O102 0.90(5) 1.62(5) 2.520(3) 173(4) . O1W H1W1 O13 0.75(5) 2.05(6) 2.759(3) 158(5) 2_656 O1W H1W2 O4W 0.74(5) 2.04(6) 2.772(6) 170(5) . O1W H1W2 O6W 0.74(5) 2.23(6) 2.957(10) 165(5) . O1W H1W2 O9W" 0.74(5) 2.35(6) 2.91(2) 134(5) . O2W H2W1 O102 0.73 2.24 2.903(3) 152.0 . O2W H2W1 O103 0.73 2.66 3.230(3) 136.7 . O2W H2W2 O6W 0.86 1.88 2.739(9) 179.3 . O2W H2W2 O4W 0.86 1.93 2.779(6) 166.7 . O2W H2W2 O7W 0.86 2.14 2.83(2) 136.8 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.132 _refine_diff_density_min -0.887 _refine_diff_density_rms 0.103 #END data_2_2H2O_7.5MeOH _database_code_depnum_ccdc_archive 'CCDC 781533' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C60 H63 Br6 Cl N8 Ni6 O16), 7.5(C H4 O), (H2 O), (O)' _chemical_formula_sum 'C67.50 H95 Br6 Cl N8 Ni6 O25.50' _chemical_formula_weight 2293.69 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 13.8111(3) _cell_length_b 25.1992(7) _cell_length_c 25.1121(7) _cell_angle_alpha 90 _cell_angle_beta 92.554(2) _cell_angle_gamma 90 _cell_volume 8731.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1955 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 25.925 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.745 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4620 _exptl_absorpt_coefficient_mu 4.120 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4244 _exptl_absorpt_correction_T_max 0.6625 _exptl_absorpt_process_details 'SADABS Bruker (2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker X8 KappaAPEXII' _diffrn_measurement_method 'omega/phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'not significant' _diffrn_reflns_number 92323 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15359 _reflns_number_gt 12335 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER APEX' _computing_cell_refinement 'BRUKER APEX' _computing_data_reduction ? _computing_structure_solution 'Sir-92 (Altomare, 1993)' _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^)+(0.0525P)^2^+1.0295P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15359 _refine_ls_number_parameters 1022 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0862 _refine_ls_R_factor_gt 0.0703 _refine_ls_wR_factor_ref 0.1854 _refine_ls_wR_factor_gt 0.1823 _refine_ls_goodness_of_fit_ref 2.167 _refine_ls_restrained_S_all 2.167 _refine_ls_shift/su_max 0.039 _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 Ni11 Ni 0.72120(6) 0.26794(4) 0.66895(4) 0.0191(2) Uani 1 1 d . . . Ni12 Ni 0.55654(6) 0.18935(4) 0.66877(4) 0.0175(2) Uani 1 1 d . . . Ni13 Ni 0.58113(6) 0.33034(4) 0.72915(4) 0.0193(2) Uani 1 1 d . . . Ni21 Ni 0.22178(6) 0.26494(4) 0.81732(4) 0.0180(2) Uani 1 1 d . . . Ni22 Ni 0.38708(6) 0.18685(4) 0.81783(4) 0.0168(2) Uani 1 1 d . . . Ni23 Ni 0.36807(6) 0.33032(4) 0.76437(4) 0.0198(2) Uani 1 1 d . . . Cl1 Cl 0.47479(12) 0.14683(8) 0.74319(7) 0.0223(4) Uani 1 1 d . . . N101 N 0.8164(4) 0.2899(3) 0.6161(2) 0.0202(14) Uani 1 1 d . . . N102 N 0.5088(4) 0.1284(3) 0.6223(2) 0.0220(14) Uani 1 1 d . . . N103 N 0.8066(4) 0.1986(3) 0.6778(2) 0.0221(15) Uani 1 1 d . . . N104 N 0.6828(4) 0.1380(2) 0.6804(2) 0.0186(14) Uani 1 1 d . . . N201 N 0.1199(4) 0.2840(3) 0.8673(2) 0.0203(14) Uani 1 1 d . . . N202 N 0.4333(4) 0.1245(3) 0.8627(2) 0.0201(14) Uani 1 1 d . . . N203 N 0.1383(4) 0.1954(2) 0.8027(2) 0.0182(14) Uani 1 1 d . . . N204 N 0.2625(4) 0.1357(2) 0.8008(2) 0.0196(14) Uani 1 1 d . . . O101 O 0.6502(3) 0.3359(2) 0.6592(2) 0.0235(12) Uani 1 1 d . . . O102 O 0.4345(3) 0.2296(2) 0.6498(2) 0.0209(12) Uani 1 1 d . . . O103 O 0.6282(3) 0.2305(2) 0.61137(19) 0.0193(11) Uani 1 1 d . . . O201 O 0.2929(3) 0.3326(2) 0.8326(2) 0.0228(12) Uani 1 1 d . . . O202 O 0.5069(3) 0.22689(19) 0.84005(19) 0.0198(12) Uani 1 1 d . . . O203 O 0.3088(3) 0.2245(2) 0.87643(19) 0.0189(11) Uani 1 1 d . . . O1H O 0.6103(3) 0.2507(2) 0.71692(19) 0.0189(11) Uani 1 1 d . . . H1 H 0.6011 0.2425 0.7424 0.023 Uiso 1 1 d R . . O2H O 0.3374(3) 0.25035(19) 0.77192(19) 0.0181(11) Uani 1 1 d . . . H2 H 0.3612 0.2452 0.7417 0.022 Uiso 1 1 d R . . O11 O 0.8122(3) 0.2996(2) 0.7278(2) 0.0253(13) Uani 1 1 d . . . O13 O 0.7045(3) 0.3458(2) 0.77298(19) 0.0211(12) Uani 1 1 d . . . O21 O 0.1354(3) 0.2991(2) 0.7570(2) 0.0233(12) Uani 1 1 d . . . O23 O 0.2491(3) 0.3476(2) 0.7179(2) 0.0263(13) Uani 1 1 d . . . O31 O 0.5526(3) 0.4094(2) 0.7370(2) 0.0253(12) Uani 1 1 d . . . O33 O 0.3956(3) 0.4103(2) 0.7577(2) 0.0260(13) Uani 1 1 d . . . O3W O 0.4440(3) 0.3187(2) 0.69543(19) 0.0202(11) Uani 1 1 d . . . H3WA H 0.4209 0.3367 0.6690 0.024 Uiso 1 1 d R . . H3WB H 0.4265 0.2905 0.6770 0.024 Uiso 1 1 d R . . O4W O 0.5063(3) 0.31808(19) 0.79911(19) 0.0172(11) Uani 1 1 d . . . H4wA H 0.5119 0.2825 0.8051 0.021 Uiso 1 1 d R . . H4wB H 0.4995 0.3500 0.8195 0.021 Uiso 1 1 d R . . C10 C 0.7887(5) 0.3324(3) 0.7630(3) 0.0221(17) Uani 1 1 d . . . C11 C 0.8708(5) 0.3555(3) 0.7971(3) 0.0273(19) Uani 1 1 d . . . H11A H 0.9310 0.3367 0.7901 0.041 Uiso 1 1 calc R . . H11B H 0.8567 0.3518 0.8348 0.041 Uiso 1 1 calc R . . H11C H 0.8782 0.3932 0.7885 0.041 Uiso 1 1 calc R . . C20 C 0.1610(5) 0.3322(3) 0.7222(3) 0.0237(18) Uani 1 1 d . . . C21 C 0.0850(6) 0.3555(3) 0.6864(3) 0.032(2) Uani 1 1 d . . . H21A H 0.0246 0.3356 0.6894 0.048 Uiso 1 1 calc R . . H21B H 0.1054 0.3540 0.6495 0.048 Uiso 1 1 calc R . . H21C H 0.0745 0.3926 0.6964 0.048 Uiso 1 1 calc R . . C30 C 0.4723(6) 0.4324(3) 0.7435(3) 0.0273(19) Uani 1 1 d . . . C31 C 0.4679(6) 0.4923(3) 0.7328(5) 0.054(3) Uani 1 1 d . . . H31A H 0.5104 0.5108 0.7590 0.081 Uiso 1 1 calc R . . H31B H 0.4012 0.5048 0.7356 0.081 Uiso 1 1 calc R . . H31C H 0.4895 0.4995 0.6968 0.081 Uiso 1 1 calc R . . C100 C 0.6590(5) 0.3713(3) 0.6207(3) 0.0218(18) Uani 1 1 d . . . C101 C 0.5887(5) 0.4113(3) 0.6130(3) 0.0235(18) Uani 1 1 d . . . H101 H 0.5357 0.4124 0.6358 0.028 Uiso 1 1 calc R . . C102 C 0.5943(6) 0.4492(3) 0.5733(3) 0.0292(19) Uani 1 1 d . . . H102 H 0.5458 0.4757 0.5691 0.035 Uiso 1 1 calc R . . C103 C 0.6706(6) 0.4480(3) 0.5400(3) 0.032(2) Uani 1 1 d . . . Br11 Br 0.67921(7) 0.50143(4) 0.48656(4) 0.0460(3) Uani 1 1 d . . . C104 C 0.7419(5) 0.4101(3) 0.5463(3) 0.0271(19) Uani 1 1 d . . . H104 H 0.7955 0.4106 0.5239 0.033 Uiso 1 1 calc R . . C105 C 0.7366(5) 0.3708(3) 0.5855(3) 0.0252(19) Uani 1 1 d . . . C106 C 0.8131(5) 0.3305(3) 0.5869(3) 0.0231(18) Uani 1 1 d . . . H106 H 0.8649 0.3355 0.5636 0.028 Uiso 1 1 calc R . . C107 C 0.8970(5) 0.2523(3) 0.6117(3) 0.0263(19) Uani 1 1 d . . . H10A H 0.9586 0.2720 0.6088 0.032 Uiso 1 1 calc R . . H10B H 0.8866 0.2304 0.5793 0.032 Uiso 1 1 calc R . . C108 C 0.9030(5) 0.2166(3) 0.6612(3) 0.0245(18) Uani 1 1 d . . . H10C H 0.9430 0.1851 0.6536 0.029 Uiso 1 1 calc R . . H10D H 0.9358 0.2362 0.6910 0.029 Uiso 1 1 calc R . . C109 C 0.8130(5) 0.1781(3) 0.7338(3) 0.0254(19) Uani 1 1 d . . . H10E H 0.8059 0.2072 0.7598 0.030 Uiso 1 1 calc R . . H10F H 0.8758 0.1600 0.7415 0.030 Uiso 1 1 calc R . . C110 C 0.7289(5) 0.1390(3) 0.7361(3) 0.0218(17) Uani 1 1 d . . . H11D H 0.7527 0.1032 0.7466 0.026 Uiso 1 1 calc R . . H11E H 0.6817 0.1509 0.7621 0.026 Uiso 1 1 calc R . . C111 C 0.6443(5) 0.0843(3) 0.6682(3) 0.0245(18) Uani 1 1 d . . . H11F H 0.6085 0.0711 0.6988 0.029 Uiso 1 1 calc R . . H11G H 0.6989 0.0597 0.6627 0.029 Uiso 1 1 calc R . . C112 C 0.5765(5) 0.0846(3) 0.6182(3) 0.0254(18) Uani 1 1 d . . . H11H H 0.6146 0.0890 0.5860 0.031 Uiso 1 1 calc R . . H11I H 0.5407 0.0506 0.6152 0.031 Uiso 1 1 calc R . . C113 C 0.4196(5) 0.1216(3) 0.6044(3) 0.0218(17) Uani 1 1 d . . . H113 H 0.4042 0.0884 0.5883 0.026 Uiso 1 1 calc R . . C114 C 0.3415(5) 0.1600(3) 0.6068(3) 0.0189(17) Uani 1 1 d . . . C115 C 0.2509(5) 0.1436(3) 0.5834(3) 0.0253(18) Uani 1 1 d . . . H115 H 0.2437 0.1091 0.5683 0.030 Uiso 1 1 calc R . . C116 C 0.1737(5) 0.1781(3) 0.5828(3) 0.0245(19) Uani 1 1 d . . . Br12 Br 0.05339(6) 0.15709(4) 0.54911(4) 0.0440(3) Uani 1 1 d . . . C117 C 0.1813(5) 0.2270(3) 0.6050(3) 0.0259(19) Uani 1 1 d . . . H117 H 0.1266 0.2499 0.6046 0.031 Uiso 1 1 calc R . . C118 C 0.2701(5) 0.2440(3) 0.6286(3) 0.0229(17) Uani 1 1 d . . . H118 H 0.2747 0.2782 0.6446 0.027 Uiso 1 1 calc R . . C119 C 0.3524(5) 0.2108(3) 0.6289(3) 0.0194(17) Uani 1 1 d . . . C120 C 0.7677(5) 0.1529(3) 0.6486(3) 0.0201(17) Uani 1 1 d . . . H120 H 0.8164 0.1235 0.6512 0.024 Uiso 1 1 calc R . . C121 C 0.7435(5) 0.1641(3) 0.5902(3) 0.0190(16) Uani 1 1 d . . . C122 C 0.7979(5) 0.1378(3) 0.5527(3) 0.0232(18) Uani 1 1 d . . . H122 H 0.8441 0.1116 0.5634 0.028 Uiso 1 1 calc R . . C123 C 0.7825(5) 0.1511(3) 0.4991(3) 0.0207(17) Uani 1 1 d . . . Br13 Br 0.86034(6) 0.11756(3) 0.44760(3) 0.0297(2) Uani 1 1 d . . . C124 C 0.7156(5) 0.1884(3) 0.4833(3) 0.0261(18) Uani 1 1 d . . . H124 H 0.7063 0.1969 0.4465 0.031 Uiso 1 1 calc R . . C125 C 0.6617(5) 0.2137(3) 0.5203(3) 0.0259(19) Uani 1 1 d . . . H125 H 0.6138 0.2387 0.5087 0.031 Uiso 1 1 calc R . . C126 C 0.6760(5) 0.2033(3) 0.5750(3) 0.0182(16) Uani 1 1 d . . . C200 C 0.2743(5) 0.3683(3) 0.8691(3) 0.0227(17) Uani 1 1 d . . . C201 C 0.3412(6) 0.4104(3) 0.8789(3) 0.0282(19) Uani 1 1 d . . . H201 H 0.3977 0.4126 0.8588 0.034 Uiso 1 1 calc R . . C202 C 0.3253(6) 0.4478(3) 0.9171(3) 0.031(2) Uani 1 1 d . . . H202 H 0.3704 0.4759 0.9231 0.038 Uiso 1 1 calc R . . C203 C 0.2436(7) 0.4449(3) 0.9470(3) 0.033(2) Uani 1 1 d . . . Br21 Br 0.22146(9) 0.49775(4) 1.00011(4) 0.0572(3) Uani 1 1 d . . . C204 C 0.1764(7) 0.4054(3) 0.9387(3) 0.032(2) Uani 1 1 d . . . H204 H 0.1199 0.4044 0.9590 0.038 Uiso 1 1 calc R . . C205 C 0.1918(5) 0.3658(3) 0.8996(3) 0.0214(17) Uani 1 1 d . . . C206 C 0.1166(5) 0.3250(3) 0.8960(3) 0.0214(17) Uani 1 1 d . . . H206 H 0.0614 0.3296 0.9167 0.026 Uiso 1 1 calc R . . C207 C 0.0419(5) 0.2450(3) 0.8689(3) 0.0232(18) Uani 1 1 d . . . H20A H -0.0209 0.2634 0.8722 0.028 Uiso 1 1 calc R . . H20B H 0.0527 0.2217 0.9004 0.028 Uiso 1 1 calc R . . C208 C 0.0392(5) 0.2114(3) 0.8175(3) 0.0233(18) Uani 1 1 d . . . H20C H -0.0003 0.1792 0.8229 0.028 Uiso 1 1 calc R . . H20D H 0.0079 0.2321 0.7880 0.028 Uiso 1 1 calc R . . C209 C 0.1380(5) 0.1783(3) 0.7461(3) 0.0227(18) Uani 1 1 d . . . H20E H 0.1485 0.2090 0.7224 0.027 Uiso 1 1 calc R . . H20F H 0.0757 0.1612 0.7353 0.027 Uiso 1 1 calc R . . C210 C 0.2226(5) 0.1384(3) 0.7439(3) 0.0213(17) Uani 1 1 d . . . H21D H 0.1991 0.1032 0.7314 0.026 Uiso 1 1 calc R . . H21E H 0.2724 0.1512 0.7198 0.026 Uiso 1 1 calc R . . C211 C 0.3012(5) 0.0817(3) 0.8124(3) 0.0224(17) Uani 1 1 d . . . H21F H 0.3401 0.0698 0.7825 0.027 Uiso 1 1 calc R . . H21G H 0.2465 0.0566 0.8155 0.027 Uiso 1 1 calc R . . C212 C 0.3640(5) 0.0807(3) 0.8639(3) 0.0263(18) Uani 1 1 d . . . H21H H 0.3229 0.0845 0.8949 0.032 Uiso 1 1 calc R . . H21I H 0.3990 0.0465 0.8671 0.032 Uiso 1 1 calc R . . C213 C 0.5194(5) 0.1166(3) 0.8803(3) 0.0219(17) Uani 1 1 d . . . H213 H 0.5346 0.0826 0.8947 0.026 Uiso 1 1 calc R . . C214 C 0.5975(5) 0.1561(3) 0.8800(3) 0.0226(18) Uani 1 1 d . . . C215 C 0.6890(5) 0.1374(4) 0.9014(3) 0.0275(19) Uani 1 1 d . . . H215 H 0.6943 0.1027 0.9160 0.033 Uiso 1 1 calc R . . C216 C 0.7702(5) 0.1701(4) 0.9009(3) 0.036(2) Uani 1 1 d . . . Br22 Br 0.88947(6) 0.14680(4) 0.93228(4) 0.0474(3) Uani 1 1 d . . . C217 C 0.7620(5) 0.2202(3) 0.8788(3) 0.028(2) Uani 1 1 d . . . H217 H 0.8177 0.2422 0.8779 0.034 Uiso 1 1 calc R . . C218 C 0.6751(5) 0.2384(3) 0.8582(3) 0.0268(19) Uani 1 1 d . . . H218 H 0.6719 0.2730 0.8431 0.032 Uiso 1 1 calc R . . C219 C 0.5887(5) 0.2070(3) 0.8585(3) 0.0185(17) Uani 1 1 d . . . C220 C 0.1745(5) 0.1479(3) 0.8308(3) 0.0217(17) Uani 1 1 d . . . H220 H 0.1265 0.1185 0.8250 0.026 Uiso 1 1 calc R . . C221 C 0.1935(5) 0.1556(3) 0.8902(3) 0.0194(17) Uani 1 1 d . . . C222 C 0.1401(5) 0.1246(3) 0.9244(3) 0.0247(18) Uani 1 1 d . . . H222 H 0.0965 0.0983 0.9106 0.030 Uiso 1 1 calc R . . C223 C 0.1515(6) 0.1325(4) 0.9783(3) 0.030(2) Uani 1 1 d . . . Br23 Br 0.07607(6) 0.09182(4) 1.02574(3) 0.0400(3) Uani 1 1 d . . . C224 C 0.2161(6) 0.1702(4) 0.9991(3) 0.038(2) Uani 1 1 d . . . H224 H 0.2239 0.1750 1.0366 0.045 Uiso 1 1 calc R . . C225 C 0.2692(6) 0.2006(4) 0.9649(3) 0.033(2) Uani 1 1 d . . . H225 H 0.3135 0.2263 0.9793 0.040 Uiso 1 1 calc R . . C226 C 0.2589(5) 0.1942(3) 0.9093(3) 0.0238(18) Uani 1 1 d . . . O1S O 0.4658(5) 0.3073(3) 0.5571(2) 0.0468(17) Uani 1 1 d . . . H1S H 0.5087 0.2896 0.5739 0.070 Uiso 1 1 calc R . . C1S C 0.5052(7) 0.3287(4) 0.5092(3) 0.040(2) Uani 1 1 d . . . H1S1 H 0.4688 0.3606 0.4982 0.059 Uiso 1 1 calc R . . H1S2 H 0.5000 0.3021 0.4807 0.059 Uiso 1 1 calc R . . H1S3 H 0.5735 0.3380 0.5163 0.059 Uiso 1 1 calc R . . O2S O 0.2291(5) 0.4729(3) 0.7576(3) 0.066(2) Uani 1 1 d . . . H2S H 0.2750 0.4511 0.7610 0.098 Uiso 1 1 calc R . . C2S C 0.1524(7) 0.4575(5) 0.7921(4) 0.064(3) Uani 1 1 d . . . H2S1 H 0.1789 0.4542 0.8288 0.096 Uiso 1 1 calc R . . H2S2 H 0.1251 0.4234 0.7802 0.096 Uiso 1 1 calc R . . H2S3 H 0.1014 0.4846 0.7906 0.096 Uiso 1 1 calc R . . O3S O 0.5656(4) 0.3647(3) 0.8915(2) 0.0421(16) Uani 1 1 d . . . H3S H 0.5874 0.3693 0.8611 0.063 Uiso 1 1 calc R . . C3S C 0.5824(8) 0.4113(5) 0.9228(5) 0.064(3) Uani 1 1 d . . . H3S1 H 0.5326 0.4142 0.9493 0.096 Uiso 1 1 calc R . . H3S2 H 0.5796 0.4426 0.8996 0.096 Uiso 1 1 calc R . . H3S3 H 0.6465 0.4091 0.9411 0.096 Uiso 1 1 calc R . . O4S O 0.8849(5) 0.4803(3) 0.7165(3) 0.059(2) Uani 1 1 d . . . H4S H 0.8347 0.4797 0.7342 0.089 Uiso 1 1 calc R . . C4S C 0.8672(10) 0.4537(5) 0.6680(5) 0.096(5) Uani 1 1 d . . . H4S1 H 0.8965 0.4735 0.6393 0.144 Uiso 1 1 calc R . . H4S2 H 0.7971 0.4508 0.6606 0.144 Uiso 1 1 calc R . . H4S3 H 0.8956 0.4181 0.6703 0.144 Uiso 1 1 calc R . . O5S O 0.7135(5) 0.4728(3) 0.7643(3) 0.063(2) Uani 1 1 d . . . H5S H 0.6696 0.4529 0.7515 0.094 Uiso 1 1 calc R . . C5S C 0.7054(11) 0.4768(7) 0.8211(5) 0.101(5) Uani 1 1 d . . . H5S1 H 0.7539 0.5019 0.8357 0.151 Uiso 1 1 calc R . . H5S2 H 0.7163 0.4418 0.8374 0.151 Uiso 1 1 calc R . . H5S3 H 0.6404 0.4894 0.8289 0.151 Uiso 1 1 calc R . . O6S O 0.4494(4) 0.2941(2) 0.9350(2) 0.0379(15) Uiso 1 1 d . . . H6S H 0.4898 0.3157 0.9234 0.057 Uiso 1 1 calc R . . C6S C 0.4086(7) 0.3155(4) 0.9821(4) 0.045(2) Uiso 1 1 d . . . H6S1 H 0.3401 0.3239 0.9746 0.067 Uiso 1 1 calc R . . H6S2 H 0.4436 0.3479 0.9929 0.067 Uiso 1 1 calc R . . H6S3 H 0.4143 0.2893 1.0109 0.067 Uiso 1 1 calc R . . O7S O 0.0303(7) 0.5774(4) 0.8376(4) 0.023(2) Uiso 0.50 1 d P . . H7S H 0.0213 0.5747 0.8044 0.035 Uiso 0.50 1 calc PR . . C7S C -0.0273(10) 0.5413(6) 0.8624(6) 0.022(3) Uiso 0.50 1 d P . . H7S1 H 0.0069 0.5280 0.8947 0.033 Uiso 0.50 1 calc PR . . H7S2 H -0.0421 0.5116 0.8382 0.033 Uiso 0.50 1 calc PR . . H7S3 H -0.0878 0.5585 0.8719 0.033 Uiso 0.50 1 calc PR . . O8S O 0.1666(5) 0.5381(3) 0.6814(3) 0.071(2) Uiso 1 1 d . . . H8S H 0.1865 0.5172 0.7056 0.106 Uiso 1 1 calc R . . C8S C 0.1522(12) 0.5093(7) 0.6324(7) 0.116(6) Uiso 1 1 d . . . H8S1 H 0.1356 0.5342 0.6034 0.175 Uiso 1 1 calc R . . H8S2 H 0.0992 0.4838 0.6357 0.175 Uiso 1 1 calc R . . H8S3 H 0.2118 0.4903 0.6245 0.175 Uiso 1 1 calc R . . O1W O 0.0004(5) 0.5689(3) 0.7303(3) 0.0544(19) Uani 1 1 d . . . H1W1 H -0.0441 0.5411 0.7279 0.065 Uiso 1 1 d R . . H2W1 H 0.0527 0.5603 0.7033 0.071 Uiso 1 1 d R . . O2W O 0.3590(7) 0.3684(4) 0.6164(4) 0.015(2) Uiso 0.45 1 d P A 1 O2W' O 0.3327(10) 0.4045(6) 0.6122(6) 0.023(3) Uiso 0.35 1 d P B 2 O2W" O 0.3559(15) 0.4028(9) 0.6423(10) 0.010(5) Uiso 0.20 1 d P C 3 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 Ni11 0.0128(4) 0.0279(6) 0.0170(5) -0.0069(4) 0.0045(4) 0.0009(4) Ni12 0.0149(5) 0.0218(6) 0.0160(5) -0.0045(4) 0.0027(4) 0.0020(4) Ni13 0.0147(5) 0.0237(6) 0.0201(5) -0.0078(4) 0.0070(4) -0.0023(4) Ni21 0.0123(4) 0.0219(6) 0.0200(5) -0.0040(4) 0.0055(4) -0.0020(4) Ni22 0.0133(4) 0.0201(5) 0.0173(5) -0.0049(4) 0.0039(4) -0.0015(4) Ni23 0.0147(5) 0.0203(6) 0.0250(6) -0.0069(4) 0.0088(4) -0.0031(4) Cl1 0.0218(9) 0.0222(10) 0.0235(10) -0.0046(8) 0.0081(8) -0.0005(7) N101 0.015(3) 0.029(4) 0.017(3) -0.009(3) 0.003(3) 0.002(3) N102 0.021(3) 0.025(4) 0.020(4) -0.006(3) 0.005(3) 0.004(3) N103 0.018(3) 0.035(4) 0.013(3) -0.002(3) 0.005(3) -0.001(3) N104 0.024(3) 0.021(4) 0.012(3) -0.003(3) 0.004(3) 0.003(3) N201 0.011(3) 0.030(4) 0.019(3) 0.000(3) 0.001(2) -0.001(3) N202 0.016(3) 0.029(4) 0.016(3) -0.001(3) 0.004(3) -0.003(3) N203 0.019(3) 0.024(4) 0.012(3) -0.001(3) 0.002(2) -0.001(3) N204 0.023(3) 0.023(4) 0.014(3) -0.006(3) 0.003(3) -0.005(3) O101 0.017(3) 0.030(3) 0.025(3) -0.002(3) 0.010(2) 0.004(2) O102 0.014(2) 0.023(3) 0.025(3) -0.007(2) -0.003(2) 0.002(2) O103 0.017(2) 0.024(3) 0.018(3) 0.001(2) 0.002(2) 0.001(2) O201 0.016(2) 0.027(3) 0.027(3) -0.013(2) 0.008(2) -0.002(2) O202 0.015(2) 0.021(3) 0.024(3) -0.008(2) -0.001(2) 0.000(2) O203 0.016(2) 0.022(3) 0.019(3) -0.005(2) 0.005(2) -0.003(2) O1H 0.016(2) 0.027(3) 0.014(3) -0.003(2) 0.006(2) -0.001(2) O2H 0.014(2) 0.021(3) 0.020(3) -0.008(2) 0.006(2) 0.000(2) O11 0.016(3) 0.039(4) 0.021(3) -0.009(3) 0.001(2) -0.002(2) O13 0.016(3) 0.034(3) 0.013(3) -0.007(2) 0.004(2) -0.004(2) O21 0.022(3) 0.021(3) 0.028(3) 0.000(2) 0.005(2) -0.004(2) O23 0.018(3) 0.032(3) 0.030(3) -0.002(3) 0.011(2) 0.003(2) O31 0.023(3) 0.022(3) 0.032(3) -0.009(3) 0.010(2) -0.006(2) O33 0.021(3) 0.021(3) 0.037(3) -0.010(3) 0.015(2) -0.003(2) O3W 0.017(3) 0.022(3) 0.021(3) -0.001(2) 0.004(2) 0.001(2) O4W 0.017(2) 0.014(3) 0.022(3) -0.006(2) 0.006(2) -0.001(2) C10 0.022(4) 0.021(4) 0.024(4) 0.002(4) 0.003(3) -0.008(3) C11 0.023(4) 0.039(5) 0.020(4) -0.007(4) -0.002(3) -0.001(4) C20 0.016(4) 0.028(5) 0.028(5) -0.008(4) 0.009(3) -0.001(3) C21 0.030(4) 0.033(5) 0.034(5) 0.004(4) 0.005(4) -0.005(4) C30 0.032(5) 0.023(5) 0.029(5) -0.007(4) 0.016(4) -0.004(4) C31 0.039(5) 0.018(5) 0.108(9) -0.011(5) 0.041(6) -0.001(4) C100 0.017(4) 0.028(5) 0.021(4) -0.013(4) 0.002(3) -0.010(3) C101 0.022(4) 0.028(5) 0.019(4) -0.011(4) -0.001(3) -0.003(3) C102 0.029(4) 0.020(5) 0.038(5) -0.011(4) 0.001(4) 0.000(3) C103 0.040(5) 0.032(5) 0.026(5) 0.001(4) 0.008(4) -0.001(4) Br11 0.0578(6) 0.0340(6) 0.0478(6) 0.0055(5) 0.0187(5) 0.0056(4) C104 0.024(4) 0.031(5) 0.027(5) -0.008(4) 0.008(3) -0.010(4) C105 0.017(4) 0.035(5) 0.024(4) -0.011(4) 0.002(3) -0.004(3) C106 0.018(4) 0.034(5) 0.018(4) -0.004(4) 0.011(3) -0.006(3) C107 0.015(4) 0.038(5) 0.027(5) -0.012(4) 0.011(3) 0.002(3) C108 0.010(3) 0.041(5) 0.022(4) -0.014(4) 0.006(3) 0.001(3) C109 0.020(4) 0.039(5) 0.017(4) 0.000(4) 0.003(3) 0.015(4) C110 0.022(4) 0.035(5) 0.008(4) 0.001(3) -0.001(3) 0.010(3) C111 0.028(4) 0.021(5) 0.025(4) 0.000(4) 0.007(3) 0.012(3) C112 0.021(4) 0.027(5) 0.029(5) -0.002(4) 0.006(3) 0.002(3) C113 0.030(4) 0.023(4) 0.014(4) -0.011(3) 0.005(3) -0.007(3) C114 0.013(3) 0.036(5) 0.007(4) -0.002(3) -0.001(3) -0.001(3) C115 0.026(4) 0.033(5) 0.017(4) -0.014(4) 0.004(3) -0.005(4) C116 0.016(4) 0.041(5) 0.017(4) -0.015(4) 0.007(3) -0.014(3) Br12 0.0158(4) 0.0734(7) 0.0427(6) -0.0351(5) 0.0011(4) -0.0004(4) C117 0.014(4) 0.039(5) 0.025(4) -0.001(4) 0.002(3) 0.003(3) C118 0.018(4) 0.029(5) 0.022(4) 0.000(4) 0.003(3) -0.004(3) C119 0.019(4) 0.025(5) 0.014(4) 0.001(3) 0.006(3) -0.005(3) C120 0.020(4) 0.029(5) 0.012(4) 0.000(3) 0.007(3) 0.006(3) C121 0.018(4) 0.026(4) 0.013(4) -0.008(3) 0.003(3) -0.002(3) C122 0.024(4) 0.025(5) 0.021(4) -0.001(4) 0.006(3) -0.005(3) C123 0.027(4) 0.025(5) 0.009(4) -0.004(3) 0.000(3) -0.009(3) Br13 0.0344(4) 0.0377(5) 0.0180(4) -0.0078(4) 0.0138(3) -0.0061(4) C124 0.033(4) 0.029(5) 0.017(4) -0.004(4) 0.002(3) -0.006(4) C125 0.016(4) 0.037(5) 0.024(4) 0.004(4) -0.004(3) 0.000(3) C126 0.016(4) 0.025(4) 0.014(4) -0.006(3) 0.006(3) 0.000(3) C200 0.032(4) 0.017(4) 0.019(4) 0.000(3) 0.007(3) 0.006(3) C201 0.030(4) 0.022(5) 0.034(5) -0.006(4) 0.010(4) -0.003(4) C202 0.053(5) 0.020(5) 0.022(5) -0.005(4) 0.011(4) -0.010(4) C203 0.060(6) 0.019(5) 0.022(5) -0.002(4) 0.017(4) -0.002(4) Br21 0.1094(9) 0.0270(6) 0.0384(6) -0.0136(4) 0.0402(6) -0.0155(5) C204 0.059(6) 0.016(5) 0.022(5) 0.003(4) 0.019(4) 0.009(4) C205 0.032(4) 0.019(4) 0.014(4) 0.001(3) 0.007(3) 0.003(3) C206 0.020(4) 0.024(5) 0.021(4) 0.002(4) 0.012(3) 0.006(3) C207 0.013(4) 0.024(5) 0.033(5) 0.002(4) 0.006(3) 0.002(3) C208 0.008(3) 0.036(5) 0.026(4) 0.003(4) 0.002(3) -0.002(3) C209 0.023(4) 0.031(5) 0.014(4) -0.005(3) 0.003(3) -0.007(3) C210 0.025(4) 0.027(5) 0.012(4) -0.006(3) -0.002(3) -0.006(3) C211 0.022(4) 0.010(4) 0.035(5) -0.006(3) 0.002(3) -0.006(3) C212 0.028(4) 0.020(5) 0.032(5) 0.004(4) 0.006(4) -0.002(3) C213 0.023(4) 0.022(4) 0.021(4) 0.005(3) 0.002(3) 0.003(3) C214 0.019(4) 0.035(5) 0.014(4) -0.005(4) 0.003(3) -0.001(3) C215 0.014(4) 0.050(6) 0.019(4) 0.006(4) 0.006(3) -0.001(4) C216 0.006(4) 0.072(7) 0.031(5) 0.011(5) 0.009(3) 0.003(4) Br22 0.0147(4) 0.0737(8) 0.0536(6) 0.0335(5) 0.0003(4) -0.0010(4) C217 0.011(4) 0.041(6) 0.033(5) 0.001(4) 0.006(3) -0.007(3) C218 0.025(4) 0.033(5) 0.022(4) -0.001(4) 0.010(3) -0.001(4) C219 0.014(4) 0.031(5) 0.011(4) -0.010(3) 0.001(3) 0.003(3) C220 0.020(4) 0.028(5) 0.017(4) -0.001(3) 0.004(3) -0.004(3) C221 0.017(4) 0.024(4) 0.018(4) 0.001(3) 0.004(3) 0.002(3) C222 0.016(4) 0.030(5) 0.028(5) -0.001(4) -0.001(3) 0.000(3) C223 0.028(4) 0.042(6) 0.022(5) 0.010(4) 0.009(3) 0.005(4) Br23 0.0289(4) 0.0663(7) 0.0253(5) 0.0147(4) 0.0072(4) -0.0026(4) C224 0.028(4) 0.066(7) 0.020(5) -0.007(4) 0.005(4) -0.008(4) C225 0.028(4) 0.051(6) 0.021(5) -0.012(4) -0.001(4) -0.011(4) C226 0.015(4) 0.037(5) 0.020(4) -0.013(4) 0.003(3) -0.004(3) O1S 0.053(4) 0.061(5) 0.027(4) 0.002(3) -0.001(3) -0.007(3) C1S 0.052(6) 0.034(6) 0.032(5) 0.000(4) -0.005(4) -0.004(4) O2S 0.040(4) 0.061(5) 0.097(6) 0.017(4) 0.020(4) 0.020(4) C2S 0.054(7) 0.081(9) 0.058(7) 0.014(6) 0.018(5) 0.025(6) O3S 0.047(4) 0.050(4) 0.029(4) -0.020(3) -0.004(3) -0.006(3) C3S 0.053(7) 0.069(8) 0.069(8) -0.014(7) -0.015(6) -0.006(6) O4S 0.046(4) 0.070(5) 0.062(5) -0.017(4) -0.012(4) -0.007(4) C4S 0.105(11) 0.078(10) 0.099(11) -0.050(9) -0.042(9) 0.023(8) O5S 0.039(4) 0.048(5) 0.102(7) 0.022(4) -0.006(4) -0.019(3) C5S 0.102(11) 0.133(14) 0.067(10) -0.018(9) -0.003(8) -0.022(10) O1W 0.043(4) 0.042(4) 0.078(5) 0.011(4) 0.008(4) 0.003(3) _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 Ni11 O101 1.983(5) . ? Ni11 N101 1.988(6) . ? Ni11 O1H 2.037(5) . ? Ni11 O11 2.059(5) . ? Ni11 N103 2.113(6) . ? Ni11 O103 2.114(5) . ? Ni11 Ni13 2.9599(13) . ? Ni12 O102 2.006(5) . ? Ni12 N102 2.021(6) . ? Ni12 O103 2.063(5) . ? Ni12 O1H 2.080(5) . ? Ni12 N104 2.181(6) . ? Ni12 Cl1 2.471(2) . ? Ni13 O13 2.025(5) . ? Ni13 O101 2.041(5) . ? Ni13 O31 2.041(5) . ? Ni13 O3W 2.061(5) . ? Ni13 O1H 2.071(5) . ? Ni13 O4W 2.100(5) . ? Ni21 N201 1.986(6) . ? Ni21 O201 1.997(5) . ? Ni21 O2H 2.036(5) . ? Ni21 O21 2.074(5) . ? Ni21 N203 2.121(6) . ? Ni21 O203 2.128(5) . ? Ni21 Ni23 2.9670(13) . ? Ni22 O202 1.997(5) . ? Ni22 N202 2.020(6) . ? Ni22 O2H 2.071(5) . ? Ni22 O203 2.092(5) . ? Ni22 N204 2.177(6) . ? Ni22 Cl1 2.4899(19) . ? Ni23 O23 2.020(5) . ? Ni23 O201 2.043(5) . ? Ni23 O33 2.059(5) . ? Ni23 O2H 2.070(5) . ? Ni23 O3W 2.084(5) . ? Ni23 O4W 2.087(5) . ? N101 C106 1.259(10) . ? N101 C107 1.469(9) . ? N102 C113 1.303(9) . ? N102 C112 1.453(9) . ? N103 C120 1.458(10) . ? N103 C108 1.483(9) . ? N103 C109 1.498(9) . ? N104 C111 1.482(10) . ? N104 C120 1.495(9) . ? N104 C110 1.511(9) . ? N201 C206 1.261(9) . ? N201 C207 1.459(9) . ? N202 C213 1.266(9) . ? N202 C212 1.462(9) . ? N203 C220 1.466(9) . ? N203 C209 1.483(9) . ? N203 C208 1.491(9) . ? N204 C211 1.486(9) . ? N204 C220 1.490(9) . ? N204 C210 1.511(9) . ? O101 C100 1.325(9) . ? O102 C119 1.316(8) . ? O103 C126 1.339(8) . ? O201 C200 1.318(9) . ? O202 C219 1.302(8) . ? O203 C226 1.338(9) . ? O1H H1 0.6890 . ? O2H H2 0.8511 . ? O11 C10 1.263(9) . ? O13 C10 1.246(9) . ? O21 C20 1.267(9) . ? O23 C20 1.288(8) . ? O31 C30 1.269(9) . ? O33 C30 1.262(9) . ? O3W H3WA 0.8546 . ? O3W H3WB 0.8750 . ? O4W H4wA 0.9126 . ? O4W H4wB 0.9613 . ? C10 C11 1.507(10) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C20 C21 1.474(11) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C30 C31 1.533(12) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C100 C101 1.406(11) . ? C100 C105 1.420(10) . ? C101 C102 1.385(11) . ? C101 H101 0.9500 . ? C102 C103 1.374(11) . ? C102 H102 0.9500 . ? C103 C104 1.376(11) . ? C103 Br11 1.909(8) . ? C104 C105 1.399(11) . ? C104 H104 0.9500 . ? C105 C106 1.465(11) . ? C106 H106 0.9500 . ? C107 C108 1.535(11) . ? C107 H10A 0.9900 . ? C107 H10B 0.9900 . ? C108 H10C 0.9900 . ? C108 H10D 0.9900 . ? C109 C110 1.527(11) . ? C109 H10E 0.9900 . ? C109 H10F 0.9900 . ? C110 H11D 0.9900 . ? C110 H11E 0.9900 . ? C111 C112 1.532(11) . ? C111 H11F 0.9900 . ? C111 H11G 0.9900 . ? C112 H11H 0.9900 . ? C112 H11I 0.9900 . ? C113 C114 1.453(10) . ? C113 H113 0.9500 . ? C114 C119 1.400(10) . ? C114 C115 1.421(10) . ? C115 C116 1.376(11) . ? C115 H115 0.9500 . ? C116 C117 1.355(11) . ? C116 Br12 1.906(7) . ? C117 C118 1.404(10) . ? C117 H117 0.9500 . ? C118 C119 1.412(10) . ? C118 H118 0.9500 . ? C120 C121 1.516(10) . ? C120 H120 1.0000 . ? C121 C122 1.398(10) . ? C121 C126 1.398(10) . ? C122 C123 1.394(10) . ? C122 H122 0.9500 . ? C123 C124 1.365(11) . ? C123 Br13 1.914(7) . ? C124 C125 1.374(11) . ? C124 H124 0.9500 . ? C125 C126 1.405(10) . ? C125 H125 0.9500 . ? C200 C205 1.403(10) . ? C200 C201 1.421(11) . ? C201 C202 1.369(11) . ? C201 H201 0.9500 . ? C202 C203 1.385(11) . ? C202 H202 0.9500 . ? C203 C204 1.371(12) . ? C203 Br21 1.919(8) . ? C204 C205 1.421(10) . ? C204 H204 0.9500 . ? C205 C206 1.462(11) . ? C206 H206 0.9500 . ? C207 C208 1.544(11) . ? C207 H20A 0.9900 . ? C207 H20B 0.9900 . ? C208 H20C 0.9900 . ? C208 H20D 0.9900 . ? C209 C210 1.544(10) . ? C209 H20E 0.9900 . ? C209 H20F 0.9900 . ? C210 H21D 0.9900 . ? C210 H21E 0.9900 . ? C211 C212 1.525(11) . ? C211 H21F 0.9900 . ? C211 H21G 0.9900 . ? C212 H21H 0.9900 . ? C212 H21I 0.9900 . ? C213 C214 1.467(10) . ? C213 H213 0.9500 . ? C214 C219 1.397(11) . ? C214 C215 1.430(10) . ? C215 C216 1.393(11) . ? C215 H215 0.9500 . ? C216 C217 1.381(12) . ? C216 Br22 1.887(8) . ? C217 C218 1.365(11) . ? C217 H217 0.9500 . ? C218 C219 1.432(10) . ? C218 H218 0.9500 . ? C220 C221 1.514(10) . ? C220 H220 1.0000 . ? C221 C222 1.397(10) . ? C221 C226 1.398(10) . ? C222 C223 1.370(11) . ? C222 H222 0.9500 . ? C223 C224 1.388(12) . ? C223 Br23 1.915(8) . ? C224 C225 1.386(12) . ? C224 H224 0.9500 . ? C225 C226 1.407(10) . ? C225 H225 0.9500 . ? O1S C1S 1.445(10) . ? O1S H1S 0.8400 . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? O2S C2S 1.450(11) . ? O2S H2S 0.8400 . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? O3S C3S 1.426(11) . ? O3S H3S 0.8400 . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? O4S C4S 1.403(12) . ? O4S H4S 0.8400 . ? C4S H4S1 0.9800 . ? C4S H4S2 0.9800 . ? C4S H4S3 0.9800 . ? O5S C5S 1.438(14) . ? O5S H5S 0.8400 . ? C5S H5S1 0.9800 . ? C5S H5S2 0.9800 . ? C5S H5S3 0.9800 . ? O6S C6S 1.438(10) . ? O6S H6S 0.8400 . ? C6S H6S1 0.9800 . ? C6S H6S2 0.9800 . ? C6S H6S3 0.9800 . ? O7S C7S 1.376(17) . ? O7S H7S 0.8400 . ? C7S H7S1 0.9800 . ? C7S H7S2 0.9800 . ? C7S H7S3 0.9800 . ? O8S C8S 1.434(16) . ? O8S H8S 0.8400 . ? C8S H8S1 0.9800 . ? C8S H8S2 0.9800 . ? C8S H8S3 0.9800 . ? O1W H1W1 0.9319 . ? O1W H2W1 1.0359 . ? 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 O101 Ni11 N101 90.8(2) . . ? O101 Ni11 O1H 82.9(2) . . ? N101 Ni11 O1H 172.3(2) . . ? O101 Ni11 O11 92.1(2) . . ? N101 Ni11 O11 88.3(2) . . ? O1H Ni11 O11 96.25(19) . . ? O101 Ni11 N103 175.6(2) . . ? N101 Ni11 N103 85.3(2) . . ? O1H Ni11 N103 101.1(2) . . ? O11 Ni11 N103 85.7(2) . . ? O101 Ni11 O103 91.1(2) . . ? N101 Ni11 O103 93.9(2) . . ? O1H Ni11 O103 81.91(18) . . ? O11 Ni11 O103 176.1(2) . . ? N103 Ni11 O103 91.3(2) . . ? O101 Ni11 Ni13 43.42(14) . . ? N101 Ni11 Ni13 131.27(19) . . ? O1H Ni11 Ni13 44.37(14) . . ? O11 Ni11 Ni13 79.58(14) . . ? N103 Ni11 Ni13 139.42(16) . . ? O103 Ni11 Ni13 101.28(13) . . ? O102 Ni12 N102 89.9(2) . . ? O102 Ni12 O103 90.3(2) . . ? N102 Ni12 O103 97.6(2) . . ? O102 Ni12 O1H 92.06(19) . . ? N102 Ni12 O1H 178.0(2) . . ? O103 Ni12 O1H 82.13(19) . . ? O102 Ni12 N104 172.0(2) . . ? N102 Ni12 N104 82.2(2) . . ? O103 Ni12 N104 89.2(2) . . ? O1H Ni12 N104 95.8(2) . . ? O102 Ni12 Cl1 89.48(15) . . ? N102 Ni12 Cl1 87.65(18) . . ? O103 Ni12 Cl1 174.74(15) . . ? O1H Ni12 Cl1 92.64(14) . . ? N104 Ni12 Cl1 91.80(16) . . ? O13 Ni13 O101 92.31(19) . . ? O13 Ni13 O31 85.5(2) . . ? O101 Ni13 O31 96.6(2) . . ? O13 Ni13 O3W 170.57(19) . . ? O101 Ni13 O3W 96.5(2) . . ? O31 Ni13 O3W 90.1(2) . . ? O13 Ni13 O1H 95.9(2) . . ? O101 Ni13 O1H 80.6(2) . . ? O31 Ni13 O1H 177.0(2) . . ? O3W Ni13 O1H 88.98(19) . . ? O13 Ni13 O4W 90.39(18) . . ? O101 Ni13 O4W 175.1(2) . . ? O31 Ni13 O4W 87.6(2) . . ? O3W Ni13 O4W 81.12(18) . . ? O1H Ni13 O4W 95.03(19) . . ? O13 Ni13 Ni11 80.01(14) . . ? O101 Ni13 Ni11 41.90(15) . . ? O31 Ni13 Ni11 134.48(15) . . ? O3W Ni13 Ni11 108.91(14) . . ? O1H Ni13 Ni11 43.46(13) . . ? O4W Ni13 Ni11 134.92(14) . . ? N201 Ni21 O201 91.6(2) . . ? N201 Ni21 O2H 173.2(2) . . ? O201 Ni21 O2H 82.57(19) . . ? N201 Ni21 O21 87.7(2) . . ? O201 Ni21 O21 92.7(2) . . ? O2H Ni21 O21 96.1(2) . . ? N201 Ni21 N203 85.1(2) . . ? O201 Ni21 N203 176.4(2) . . ? O2H Ni21 N203 100.8(2) . . ? O21 Ni21 N203 85.8(2) . . ? N201 Ni21 O203 94.0(2) . . ? O201 Ni21 O203 91.0(2) . . ? O2H Ni21 O203 82.62(19) . . ? O21 Ni21 O203 175.9(2) . . ? N203 Ni21 O203 90.6(2) . . ? N201 Ni21 Ni23 131.66(19) . . ? O201 Ni21 Ni23 43.36(14) . . ? O2H Ni21 Ni23 44.18(14) . . ? O21 Ni21 Ni23 79.80(14) . . ? N203 Ni21 Ni23 139.19(16) . . ? O203 Ni21 Ni23 101.75(13) . . ? O202 Ni22 N202 90.0(2) . . ? O202 Ni22 O2H 90.87(19) . . ? N202 Ni22 O2H 179.1(2) . . ? O202 Ni22 O203 91.26(19) . . ? N202 Ni22 O203 97.0(2) . . ? O2H Ni22 O203 82.66(19) . . ? O202 Ni22 N204 172.8(2) . . ? N202 Ni22 N204 82.9(2) . . ? O2H Ni22 N204 96.3(2) . . ? O203 Ni22 N204 88.7(2) . . ? O202 Ni22 Cl1 89.43(14) . . ? N202 Ni22 Cl1 87.26(17) . . ? O2H Ni22 Cl1 93.11(14) . . ? O203 Ni22 Cl1 175.73(15) . . ? N204 Ni22 Cl1 91.10(16) . . ? O23 Ni23 O201 92.8(2) . . ? O23 Ni23 O33 83.7(2) . . ? O201 Ni23 O33 98.2(2) . . ? O23 Ni23 O2H 95.6(2) . . ? O201 Ni23 O2H 80.6(2) . . ? O33 Ni23 O2H 178.67(19) . . ? O23 Ni23 O3W 88.64(19) . . ? O201 Ni23 O3W 173.6(2) . . ? O33 Ni23 O3W 88.2(2) . . ? O2H Ni23 O3W 92.98(19) . . ? O23 Ni23 O4W 168.2(2) . . ? O201 Ni23 O4W 98.24(19) . . ? O33 Ni23 O4W 90.6(2) . . ? O2H Ni23 O4W 90.30(19) . . ? O3W Ni23 O4W 80.88(18) . . ? O23 Ni23 Ni21 79.99(15) . . ? O201 Ni23 Ni21 42.16(14) . . ? O33 Ni23 Ni21 135.41(14) . . ? O2H Ni23 Ni21 43.29(13) . . ? O3W Ni23 Ni21 132.23(14) . . ? O4W Ni23 Ni21 111.07(14) . . ? Ni12 Cl1 Ni22 130.38(9) . . ? C106 N101 C107 119.1(6) . . ? C106 N101 Ni11 127.5(5) . . ? C107 N101 Ni11 113.4(5) . . ? C113 N102 C112 118.5(6) . . ? C113 N102 Ni12 125.3(5) . . ? C112 N102 Ni12 115.0(5) . . ? C120 N103 C108 114.5(6) . . ? C120 N103 C109 101.8(6) . . ? C108 N103 C109 110.7(6) . . ? C120 N103 Ni11 114.1(4) . . ? C108 N103 Ni11 102.9(5) . . ? C109 N103 Ni11 113.2(4) . . ? C111 N104 C120 113.7(5) . . ? C111 N104 C110 109.8(6) . . ? C120 N104 C110 100.5(5) . . ? C111 N104 Ni12 103.7(4) . . ? C120 N104 Ni12 114.9(4) . . ? C110 N104 Ni12 114.5(4) . . ? C206 N201 C207 119.4(6) . . ? C206 N201 Ni21 127.1(5) . . ? C207 N201 Ni21 113.5(5) . . ? C213 N202 C212 118.7(7) . . ? C213 N202 Ni22 125.8(5) . . ? C212 N202 Ni22 114.1(5) . . ? C220 N203 C209 102.2(6) . . ? C220 N203 C208 113.4(6) . . ? C209 N203 C208 110.7(5) . . ? C220 N203 Ni21 114.9(4) . . ? C209 N203 Ni21 112.6(4) . . ? C208 N203 Ni21 103.4(4) . . ? C211 N204 C220 112.6(6) . . ? C211 N204 C210 109.9(6) . . ? C220 N204 C210 101.4(5) . . ? C211 N204 Ni22 103.3(4) . . ? C220 N204 Ni22 115.7(4) . . ? C210 N204 Ni22 114.2(4) . . ? C100 O101 Ni11 127.7(4) . . ? C100 O101 Ni13 137.3(5) . . ? Ni11 O101 Ni13 94.7(2) . . ? C119 O102 Ni12 127.8(5) . . ? C126 O103 Ni12 119.1(4) . . ? C126 O103 Ni11 113.0(4) . . ? Ni12 O103 Ni11 92.42(19) . . ? C200 O201 Ni21 127.4(5) . . ? C200 O201 Ni23 136.5(5) . . ? Ni21 O201 Ni23 94.5(2) . . ? C219 O202 Ni22 126.9(5) . . ? C226 O203 Ni22 118.1(4) . . ? C226 O203 Ni21 114.4(4) . . ? Ni22 O203 Ni21 91.14(19) . . ? Ni11 O1H Ni13 92.2(2) . . ? Ni11 O1H Ni12 94.16(19) . . ? Ni13 O1H Ni12 137.7(2) . . ? Ni11 O1H H1 141.9 . . ? Ni13 O1H H1 96.3 . . ? Ni12 O1H H1 103.9 . . ? Ni21 O2H Ni23 92.54(19) . . ? Ni21 O2H Ni22 94.4(2) . . ? Ni23 O2H Ni22 137.7(2) . . ? Ni21 O2H H2 150.6 . . ? Ni23 O2H H2 88.7 . . ? Ni22 O2H H2 104.4 . . ? C10 O11 Ni11 126.1(5) . . ? C10 O13 Ni13 127.5(5) . . ? C20 O21 Ni21 127.4(5) . . ? C20 O23 Ni23 129.3(5) . . ? C30 O31 Ni13 129.2(5) . . ? C30 O33 Ni23 128.1(5) . . ? Ni13 O3W Ni23 97.2(2) . . ? Ni13 O3W H3WA 123.2 . . ? Ni23 O3W H3WA 112.7 . . ? Ni13 O3W H3WB 124.0 . . ? Ni23 O3W H3WB 114.6 . . ? H3WA O3W H3WB 86.3 . . ? Ni23 O4W Ni13 95.9(2) . . ? Ni23 O4W H4wA 106.4 . . ? Ni13 O4W H4wA 103.9 . . ? Ni23 O4W H4wB 89.4 . . ? Ni13 O4W H4wB 112.8 . . ? H4wA O4W H4wB 138.2 . . ? O13 C10 O11 126.1(7) . . ? O13 C10 C11 117.8(7) . . ? O11 C10 C11 116.1(6) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O21 C20 O23 123.4(7) . . ? O21 C20 C21 118.0(6) . . ? O23 C20 C21 118.5(7) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O33 C30 O31 125.7(8) . . ? O33 C30 C31 117.3(7) . . ? O31 C30 C31 117.1(7) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O101 C100 C101 119.9(6) . . ? O101 C100 C105 123.0(7) . . ? C101 C100 C105 117.1(7) . . ? C102 C101 C100 122.2(7) . . ? C102 C101 H101 118.9 . . ? C100 C101 H101 118.9 . . ? C103 C102 C101 119.5(8) . . ? C103 C102 H102 120.3 . . ? C101 C102 H102 120.3 . . ? C102 C103 C104 120.6(8) . . ? C102 C103 Br11 119.1(6) . . ? C104 C103 Br11 120.3(6) . . ? C103 C104 C105 120.8(7) . . ? C103 C104 H104 119.6 . . ? C105 C104 H104 119.6 . . ? C104 C105 C100 119.7(7) . . ? C104 C105 C106 116.5(7) . . ? C100 C105 C106 123.7(7) . . ? N101 C106 C105 125.7(7) . . ? N101 C106 H106 117.1 . . ? C105 C106 H106 117.1 . . ? N101 C107 C108 109.4(6) . . ? N101 C107 H10A 109.8 . . ? C108 C107 H10A 109.8 . . ? N101 C107 H10B 109.8 . . ? C108 C107 H10B 109.8 . . ? H10A C107 H10B 108.3 . . ? N103 C108 C107 113.0(6) . . ? N103 C108 H10C 109.0 . . ? C107 C108 H10C 109.0 . . ? N103 C108 H10D 109.0 . . ? C107 C108 H10D 109.0 . . ? H10C C108 H10D 107.8 . . ? N103 C109 C110 104.2(6) . . ? N103 C109 H10E 110.9 . . ? C110 C109 H10E 110.9 . . ? N103 C109 H10F 110.9 . . ? C110 C109 H10F 110.9 . . ? H10E C109 H10F 108.9 . . ? N104 C110 C109 105.4(6) . . ? N104 C110 H11D 110.7 . . ? C109 C110 H11D 110.7 . . ? N104 C110 H11E 110.7 . . ? C109 C110 H11E 110.7 . . ? H11D C110 H11E 108.8 . . ? N104 C111 C112 111.4(6) . . ? N104 C111 H11F 109.4 . . ? C112 C111 H11F 109.4 . . ? N104 C111 H11G 109.4 . . ? C112 C111 H11G 109.4 . . ? H11F C111 H11G 108.0 . . ? N102 C112 C111 108.5(6) . . ? N102 C112 H11H 110.0 . . ? C111 C112 H11H 110.0 . . ? N102 C112 H11I 110.0 . . ? C111 C112 H11I 110.0 . . ? H11H C112 H11I 108.4 . . ? N102 C113 C114 126.2(7) . . ? N102 C113 H113 116.9 . . ? C114 C113 H113 116.9 . . ? C119 C114 C115 120.6(7) . . ? C119 C114 C113 123.9(6) . . ? C115 C114 C113 115.5(7) . . ? C116 C115 C114 119.1(7) . . ? C116 C115 H115 120.4 . . ? C114 C115 H115 120.4 . . ? C117 C116 C115 121.7(7) . . ? C117 C116 Br12 119.1(6) . . ? C115 C116 Br12 119.2(6) . . ? C116 C117 C118 120.1(7) . . ? C116 C117 H117 119.9 . . ? C118 C117 H117 119.9 . . ? C117 C118 C119 120.6(7) . . ? C117 C118 H118 119.7 . . ? C119 C118 H118 119.7 . . ? O102 C119 C114 124.3(7) . . ? O102 C119 C118 117.9(7) . . ? C114 C119 C118 117.9(7) . . ? N103 C120 N104 102.1(5) . . ? N103 C120 C121 113.6(6) . . ? N104 C120 C121 114.8(6) . . ? N103 C120 H120 108.7 . . ? N104 C120 H120 108.7 . . ? C121 C120 H120 108.7 . . ? C122 C121 C126 121.5(7) . . ? C122 C121 C120 117.5(7) . . ? C126 C121 C120 120.7(6) . . ? C123 C122 C121 118.3(7) . . ? C123 C122 H122 120.9 . . ? C121 C122 H122 120.9 . . ? C124 C123 C122 121.2(7) . . ? C124 C123 Br13 120.1(5) . . ? C122 C123 Br13 118.7(6) . . ? C123 C124 C125 120.2(7) . . ? C123 C124 H124 119.9 . . ? C125 C124 H124 119.9 . . ? C124 C125 C126 121.2(7) . . ? C124 C125 H125 119.4 . . ? C126 C125 H125 119.4 . . ? O103 C126 C121 121.2(6) . . ? O103 C126 C125 121.2(7) . . ? C121 C126 C125 117.5(6) . . ? O201 C200 C205 122.5(7) . . ? O201 C200 C201 118.9(7) . . ? C205 C200 C201 118.5(7) . . ? C202 C201 C200 120.7(7) . . ? C202 C201 H201 119.6 . . ? C200 C201 H201 119.6 . . ? C201 C202 C203 120.2(8) . . ? C201 C202 H202 119.9 . . ? C203 C202 H202 119.9 . . ? C204 C203 C202 121.3(7) . . ? C204 C203 Br21 118.8(6) . . ? C202 C203 Br21 119.9(6) . . ? C203 C204 C205 119.6(8) . . ? C203 C204 H204 120.2 . . ? C205 C204 H204 120.2 . . ? C200 C205 C204 119.7(7) . . ? C200 C205 C206 126.1(7) . . ? C204 C205 C206 114.2(7) . . ? N201 C206 C205 124.7(7) . . ? N201 C206 H206 117.7 . . ? C205 C206 H206 117.7 . . ? N201 C207 C208 109.7(6) . . ? N201 C207 H20A 109.7 . . ? C208 C207 H20A 109.7 . . ? N201 C207 H20B 109.7 . . ? C208 C207 H20B 109.7 . . ? H20A C207 H20B 108.2 . . ? N203 C208 C207 111.6(6) . . ? N203 C208 H20C 109.3 . . ? C207 C208 H20C 109.3 . . ? N203 C208 H20D 109.3 . . ? C207 C208 H20D 109.3 . . ? H20C C208 H20D 108.0 . . ? N203 C209 C210 104.7(6) . . ? N203 C209 H20E 110.8 . . ? C210 C209 H20E 110.8 . . ? N203 C209 H20F 110.8 . . ? C210 C209 H20F 110.8 . . ? H20E C209 H20F 108.9 . . ? N204 C210 C209 103.8(6) . . ? N204 C210 H21D 111.0 . . ? C209 C210 H21D 111.0 . . ? N204 C210 H21E 111.0 . . ? C209 C210 H21E 111.0 . . ? H21D C210 H21E 109.0 . . ? N204 C211 C212 111.6(6) . . ? N204 C211 H21F 109.3 . . ? C212 C211 H21F 109.3 . . ? N204 C211 H21G 109.3 . . ? C212 C211 H21G 109.3 . . ? H21F C211 H21G 108.0 . . ? N202 C212 C211 108.6(6) . . ? N202 C212 H21H 110.0 . . ? C211 C212 H21H 110.0 . . ? N202 C212 H21I 110.0 . . ? C211 C212 H21I 110.0 . . ? H21H C212 H21I 108.4 . . ? N202 C213 C214 124.8(7) . . ? N202 C213 H213 117.6 . . ? C214 C213 H213 117.6 . . ? C219 C214 C215 120.5(7) . . ? C219 C214 C213 125.1(7) . . ? C215 C214 C213 114.4(7) . . ? C216 C215 C214 120.1(8) . . ? C216 C215 H215 120.0 . . ? C214 C215 H215 120.0 . . ? C217 C216 C215 119.5(7) . . ? C217 C216 Br22 120.5(6) . . ? C215 C216 Br22 120.0(7) . . ? C218 C217 C216 121.0(7) . . ? C218 C217 H217 119.5 . . ? C216 C217 H217 119.5 . . ? C217 C218 C219 122.0(8) . . ? C217 C218 H218 119.0 . . ? C219 C218 H218 119.0 . . ? O202 C219 C214 123.4(7) . . ? O202 C219 C218 119.7(7) . . ? C214 C219 C218 116.9(7) . . ? N203 C220 N204 101.1(5) . . ? N203 C220 C221 114.3(6) . . ? N204 C220 C221 114.5(6) . . ? N203 C220 H220 108.9 . . ? N204 C220 H220 108.9 . . ? C221 C220 H220 108.9 . . ? C222 C221 C226 121.9(7) . . ? C222 C221 C220 117.5(7) . . ? C226 C221 C220 120.5(7) . . ? C223 C222 C221 119.1(7) . . ? C223 C222 H222 120.5 . . ? C221 C222 H222 120.5 . . ? C222 C223 C224 121.0(7) . . ? C222 C223 Br23 119.6(6) . . ? C224 C223 Br23 119.4(6) . . ? C225 C224 C223 119.6(8) . . ? C225 C224 H224 120.2 . . ? C223 C224 H224 120.2 . . ? C224 C225 C226 121.3(8) . . ? C224 C225 H225 119.4 . . ? C226 C225 H225 119.4 . . ? O203 C226 C221 121.9(7) . . ? O203 C226 C225 121.0(7) . . ? C221 C226 C225 117.1(7) . . ? C1S O1S H1S 109.5 . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C2S O2S H2S 109.5 . . ? O2S C2S H2S1 109.5 . . ? O2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? O2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? C3S O3S H3S 109.5 . . ? O3S C3S H3S1 109.5 . . ? O3S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? O3S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? C4S O4S H4S 109.5 . . ? O4S C4S H4S1 109.5 . . ? O4S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? O4S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? C5S O5S H5S 109.5 . . ? O5S C5S H5S1 109.5 . . ? O5S C5S H5S2 109.5 . . ? H5S1 C5S H5S2 109.5 . . ? O5S C5S H5S3 109.5 . . ? H5S1 C5S H5S3 109.5 . . ? H5S2 C5S H5S3 109.5 . . ? C6S O6S H6S 109.5 . . ? O6S C6S H6S1 109.5 . . ? O6S C6S H6S2 109.5 . . ? H6S1 C6S H6S2 109.5 . . ? O6S C6S H6S3 109.5 . . ? H6S1 C6S H6S3 109.5 . . ? H6S2 C6S H6S3 109.5 . . ? C7S O7S H7S 109.5 . . ? O7S C7S H7S1 109.5 . . ? O7S C7S H7S2 109.5 . . ? H7S1 C7S H7S2 109.5 . . ? O7S C7S H7S3 109.5 . . ? H7S1 C7S H7S3 109.5 . . ? H7S2 C7S H7S3 109.5 . . ? C8S O8S H8S 109.5 . . ? O8S C8S H8S1 109.5 . . ? O8S C8S H8S2 109.5 . . ? H8S1 C8S H8S2 109.5 . . ? O8S C8S H8S3 109.5 . . ? H8S1 C8S H8S3 109.5 . . ? H8S2 C8S H8S3 109.5 . . ? H1W1 O1W H2W1 106.1 . . ? 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 O101 Ni11 Ni13 O13 -104.9(3) . . . . ? N101 Ni11 Ni13 O13 -79.0(3) . . . . ? O1H Ni11 Ni13 O13 109.7(2) . . . . ? O11 Ni11 Ni13 O13 -0.5(2) . . . . ? N103 Ni11 Ni13 O13 70.0(3) . . . . ? O103 Ni11 Ni13 O13 175.6(2) . . . . ? N101 Ni11 Ni13 O101 26.0(3) . . . . ? O1H Ni11 Ni13 O101 -145.3(3) . . . . ? O11 Ni11 Ni13 O101 104.4(3) . . . . ? N103 Ni11 Ni13 O101 175.0(3) . . . . ? O103 Ni11 Ni13 O101 -79.5(3) . . . . ? O101 Ni11 Ni13 O31 -31.5(3) . . . . ? N101 Ni11 Ni13 O31 -5.5(3) . . . . ? O1H Ni11 Ni13 O31 -176.9(3) . . . . ? O11 Ni11 Ni13 O31 72.9(3) . . . . ? N103 Ni11 Ni13 O31 143.5(3) . . . . ? O103 Ni11 Ni13 O31 -111.0(3) . . . . ? O101 Ni11 Ni13 O3W 78.2(3) . . . . ? N101 Ni11 Ni13 O3W 104.2(3) . . . . ? O1H Ni11 Ni13 O3W -67.1(2) . . . . ? O11 Ni11 Ni13 O3W -177.4(2) . . . . ? N103 Ni11 Ni13 O3W -106.8(3) . . . . ? O103 Ni11 Ni13 O3W -1.3(2) . . . . ? O101 Ni11 Ni13 O1H 145.3(3) . . . . ? N101 Ni11 Ni13 O1H 171.3(3) . . . . ? O11 Ni11 Ni13 O1H -110.3(2) . . . . ? N103 Ni11 Ni13 O1H -39.7(3) . . . . ? O103 Ni11 Ni13 O1H 65.9(2) . . . . ? O101 Ni11 Ni13 O4W 174.6(3) . . . . ? N101 Ni11 Ni13 O4W -159.4(3) . . . . ? O1H Ni11 Ni13 O4W 29.3(3) . . . . ? O11 Ni11 Ni13 O4W -81.0(2) . . . . ? N103 Ni11 Ni13 O4W -10.4(3) . . . . ? O103 Ni11 Ni13 O4W 95.1(2) . . . . ? N201 Ni21 Ni23 O23 -78.1(3) . . . . ? O201 Ni21 Ni23 O23 -105.5(3) . . . . ? O2H Ni21 Ni23 O23 109.4(2) . . . . ? O21 Ni21 Ni23 O23 -0.4(2) . . . . ? N203 Ni21 Ni23 O23 70.7(3) . . . . ? O203 Ni21 Ni23 O23 175.7(2) . . . . ? N201 Ni21 Ni23 O201 27.5(3) . . . . ? O2H Ni21 Ni23 O201 -145.0(3) . . . . ? O21 Ni21 Ni23 O201 105.1(3) . . . . ? N203 Ni21 Ni23 O201 176.3(3) . . . . ? O203 Ni21 Ni23 O201 -78.8(3) . . . . ? N201 Ni21 Ni23 O33 -7.8(3) . . . . ? O201 Ni21 Ni23 O33 -35.3(3) . . . . ? O2H Ni21 Ni23 O33 179.7(3) . . . . ? O21 Ni21 Ni23 O33 69.9(3) . . . . ? N203 Ni21 Ni23 O33 141.0(3) . . . . ? O203 Ni21 Ni23 O33 -114.0(3) . . . . ? N201 Ni21 Ni23 O2H 172.5(3) . . . . ? O201 Ni21 Ni23 O2H 145.0(3) . . . . ? O21 Ni21 Ni23 O2H -109.8(2) . . . . ? N203 Ni21 Ni23 O2H -38.7(3) . . . . ? O203 Ni21 Ni23 O2H 66.3(2) . . . . ? N201 Ni21 Ni23 O3W -157.0(3) . . . . ? O201 Ni21 Ni23 O3W 175.6(3) . . . . ? O2H Ni21 Ni23 O3W 30.5(3) . . . . ? O21 Ni21 Ni23 O3W -79.3(2) . . . . ? N203 Ni21 Ni23 O3W -8.1(3) . . . . ? O203 Ni21 Ni23 O3W 96.8(2) . . . . ? N201 Ni21 Ni23 O4W 106.1(3) . . . . ? O201 Ni21 Ni23 O4W 78.7(3) . . . . ? O2H Ni21 Ni23 O4W -66.4(2) . . . . ? O21 Ni21 Ni23 O4W -176.2(2) . . . . ? N203 Ni21 Ni23 O4W -105.0(3) . . . . ? O203 Ni21 Ni23 O4W -0.1(2) . . . . ? O102 Ni12 Cl1 Ni22 -53.57(17) . . . . ? N102 Ni12 Cl1 Ni22 -143.47(19) . . . . ? O1H Ni12 Cl1 Ni22 38.47(16) . . . . ? N104 Ni12 Cl1 Ni22 134.38(18) . . . . ? O202 Ni22 Cl1 Ni12 -58.12(17) . . . . ? N202 Ni22 Cl1 Ni12 -148.14(19) . . . . ? O2H Ni22 Cl1 Ni12 32.72(16) . . . . ? N204 Ni22 Cl1 Ni12 129.05(19) . . . . ? O101 Ni11 N101 C106 -7.1(7) . . . . ? O11 Ni11 N101 C106 -99.2(7) . . . . ? N103 Ni11 N101 C106 175.0(7) . . . . ? O103 Ni11 N101 C106 84.1(7) . . . . ? Ni13 Ni11 N101 C106 -24.6(8) . . . . ? O101 Ni11 N101 C107 174.3(5) . . . . ? O11 Ni11 N101 C107 82.2(5) . . . . ? N103 Ni11 N101 C107 -3.6(5) . . . . ? O103 Ni11 N101 C107 -94.6(5) . . . . ? Ni13 Ni11 N101 C107 156.7(4) . . . . ? O102 Ni12 N102 C113 -15.9(6) . . . . ? O103 Ni12 N102 C113 -106.1(6) . . . . ? N104 Ni12 N102 C113 165.8(6) . . . . ? Cl1 Ni12 N102 C113 73.6(6) . . . . ? O102 Ni12 N102 C112 176.8(5) . . . . ? O103 Ni12 N102 C112 86.5(5) . . . . ? N104 Ni12 N102 C112 -1.6(5) . . . . ? Cl1 Ni12 N102 C112 -93.8(5) . . . . ? N101 Ni11 N103 C120 -100.0(5) . . . . ? O1H Ni11 N103 C120 75.8(5) . . . . ? O11 Ni11 N103 C120 171.3(5) . . . . ? O103 Ni11 N103 C120 -6.2(5) . . . . ? Ni13 Ni11 N103 C120 102.9(5) . . . . ? N101 Ni11 N103 C108 24.7(4) . . . . ? O1H Ni11 N103 C108 -159.5(4) . . . . ? O11 Ni11 N103 C108 -64.0(4) . . . . ? O103 Ni11 N103 C108 118.5(4) . . . . ? Ni13 Ni11 N103 C108 -132.5(4) . . . . ? N101 Ni11 N103 C109 144.2(5) . . . . ? O1H Ni11 N103 C109 -40.0(5) . . . . ? O11 Ni11 N103 C109 55.5(5) . . . . ? O103 Ni11 N103 C109 -122.0(5) . . . . ? Ni13 Ni11 N103 C109 -13.0(6) . . . . ? N102 Ni12 N104 C111 -22.9(4) . . . . ? O103 Ni12 N104 C111 -120.7(4) . . . . ? O1H Ni12 N104 C111 157.3(4) . . . . ? Cl1 Ni12 N104 C111 64.4(4) . . . . ? O102 Ni12 N104 C120 90.1(16) . . . . ? N102 Ni12 N104 C120 101.7(5) . . . . ? O103 Ni12 N104 C120 3.9(5) . . . . ? O1H Ni12 N104 C120 -78.1(5) . . . . ? Cl1 Ni12 N104 C120 -170.9(4) . . . . ? N102 Ni12 N104 C110 -142.6(5) . . . . ? O103 Ni12 N104 C110 119.6(5) . . . . ? O1H Ni12 N104 C110 37.6(5) . . . . ? Cl1 Ni12 N104 C110 -55.2(5) . . . . ? O201 Ni21 N201 C206 -2.2(7) . . . . ? O21 Ni21 N201 C206 -94.8(7) . . . . ? N203 Ni21 N201 C206 179.2(7) . . . . ? O203 Ni21 N201 C206 88.9(7) . . . . ? Ni23 Ni21 N201 C206 -20.6(8) . . . . ? O201 Ni21 N201 C207 177.3(5) . . . . ? O21 Ni21 N201 C207 84.7(5) . . . . ? N203 Ni21 N201 C207 -1.3(5) . . . . ? O203 Ni21 N201 C207 -91.6(5) . . . . ? Ni23 Ni21 N201 C207 158.9(4) . . . . ? O202 Ni22 N202 C213 -17.7(6) . . . . ? O203 Ni22 N202 C213 -109.0(6) . . . . ? N204 Ni22 N202 C213 163.2(6) . . . . ? Cl1 Ni22 N202 C213 71.7(6) . . . . ? O202 Ni22 N202 C212 176.2(5) . . . . ? O203 Ni22 N202 C212 84.9(5) . . . . ? N204 Ni22 N202 C212 -2.9(5) . . . . ? Cl1 Ni22 N202 C212 -94.4(5) . . . . ? N201 Ni21 N203 C220 -100.5(5) . . . . ? O2H Ni21 N203 C220 76.0(5) . . . . ? O21 Ni21 N203 C220 171.4(5) . . . . ? O203 Ni21 N203 C220 -6.6(5) . . . . ? Ni23 Ni21 N203 C220 102.4(5) . . . . ? N201 Ni21 N203 C209 143.1(5) . . . . ? O2H Ni21 N203 C209 -40.4(5) . . . . ? O21 Ni21 N203 C209 55.0(5) . . . . ? O203 Ni21 N203 C209 -123.0(5) . . . . ? Ni23 Ni21 N203 C209 -14.1(6) . . . . ? N201 Ni21 N203 C208 23.6(4) . . . . ? O2H Ni21 N203 C208 -159.9(4) . . . . ? O21 Ni21 N203 C208 -64.5(4) . . . . ? O203 Ni21 N203 C208 117.5(4) . . . . ? Ni23 Ni21 N203 C208 -133.6(4) . . . . ? N202 Ni22 N204 C211 -22.1(4) . . . . ? O2H Ni22 N204 C211 158.3(4) . . . . ? O203 Ni22 N204 C211 -119.3(4) . . . . ? Cl1 Ni22 N204 C211 65.0(4) . . . . ? N202 Ni22 N204 C220 101.4(5) . . . . ? O2H Ni22 N204 C220 -78.2(5) . . . . ? O203 Ni22 N204 C220 4.3(5) . . . . ? Cl1 Ni22 N204 C220 -171.5(5) . . . . ? N202 Ni22 N204 C210 -141.4(5) . . . . ? O2H Ni22 N204 C210 39.0(5) . . . . ? O203 Ni22 N204 C210 121.5(5) . . . . ? Cl1 Ni22 N204 C210 -54.3(5) . . . . ? N101 Ni11 O101 C100 13.9(6) . . . . ? O1H Ni11 O101 C100 -161.8(6) . . . . ? O11 Ni11 O101 C100 102.2(6) . . . . ? O103 Ni11 O101 C100 -80.1(6) . . . . ? Ni13 Ni11 O101 C100 174.6(7) . . . . ? N101 Ni11 O101 Ni13 -160.8(2) . . . . ? O1H Ni11 O101 Ni13 23.62(19) . . . . ? O11 Ni11 O101 Ni13 -72.4(2) . . . . ? O103 Ni11 O101 Ni13 105.3(2) . . . . ? O13 Ni13 O101 C100 -101.5(7) . . . . ? O31 Ni13 O101 C100 -15.8(7) . . . . ? O3W Ni13 O101 C100 75.0(7) . . . . ? O1H Ni13 O101 C100 162.9(7) . . . . ? Ni11 Ni13 O101 C100 -173.7(8) . . . . ? O13 Ni13 O101 Ni11 72.2(2) . . . . ? O31 Ni13 O101 Ni11 157.9(2) . . . . ? O3W Ni13 O101 Ni11 -111.2(2) . . . . ? O1H Ni13 O101 Ni11 -23.35(19) . . . . ? N102 Ni12 O102 C119 17.0(6) . . . . ? O103 Ni12 O102 C119 114.6(6) . . . . ? O1H Ni12 O102 C119 -163.3(6) . . . . ? Cl1 Ni12 O102 C119 -70.6(5) . . . . ? O102 Ni12 O103 C126 -127.3(5) . . . . ? N102 Ni12 O103 C126 -37.4(5) . . . . ? O1H Ni12 O103 C126 140.6(5) . . . . ? N104 Ni12 O103 C126 44.7(5) . . . . ? O102 Ni12 O103 Ni11 114.53(19) . . . . ? N102 Ni12 O103 Ni11 -155.6(2) . . . . ? O1H Ni12 O103 Ni11 22.48(18) . . . . ? N104 Ni12 O103 Ni11 -73.5(2) . . . . ? O101 Ni11 O103 C126 131.2(5) . . . . ? N101 Ni11 O103 C126 40.3(5) . . . . ? O1H Ni11 O103 C126 -146.1(5) . . . . ? N103 Ni11 O103 C126 -45.1(5) . . . . ? Ni13 Ni11 O103 C126 173.8(4) . . . . ? O101 Ni11 O103 Ni12 -105.6(2) . . . . ? N101 Ni11 O103 Ni12 163.4(2) . . . . ? O1H Ni11 O103 Ni12 -22.99(19) . . . . ? N103 Ni11 O103 Ni12 78.1(2) . . . . ? Ni13 Ni11 O103 Ni12 -63.12(16) . . . . ? N201 Ni21 O201 C200 7.4(6) . . . . ? O2H Ni21 O201 C200 -169.0(6) . . . . ? O21 Ni21 O201 C200 95.2(6) . . . . ? O203 Ni21 O201 C200 -86.6(6) . . . . ? Ni23 Ni21 O201 C200 167.2(7) . . . . ? N201 Ni21 O201 Ni23 -159.8(2) . . . . ? O2H Ni21 O201 Ni23 23.8(2) . . . . ? O21 Ni21 O201 Ni23 -72.0(2) . . . . ? O203 Ni21 O201 Ni23 106.2(2) . . . . ? O23 Ni23 O201 C200 -93.5(7) . . . . ? O33 Ni23 O201 C200 -9.4(7) . . . . ? O2H Ni23 O201 C200 171.3(7) . . . . ? O4W Ni23 O201 C200 82.4(7) . . . . ? Ni21 Ni23 O201 C200 -165.2(8) . . . . ? O23 Ni23 O201 Ni21 71.8(2) . . . . ? O33 Ni23 O201 Ni21 155.8(2) . . . . ? O2H Ni23 O201 Ni21 -23.47(19) . . . . ? O4W Ni23 O201 Ni21 -112.4(2) . . . . ? N202 Ni22 O202 C219 21.3(6) . . . . ? O2H Ni22 O202 C219 -159.1(5) . . . . ? O203 Ni22 O202 C219 118.2(5) . . . . ? Cl1 Ni22 O202 C219 -66.0(5) . . . . ? O202 Ni22 O203 C226 -128.5(5) . . . . ? N202 Ni22 O203 C226 -38.4(5) . . . . ? O2H Ni22 O203 C226 140.7(5) . . . . ? N204 Ni22 O203 C226 44.3(5) . . . . ? O202 Ni22 O203 Ni21 112.8(2) . . . . ? N202 Ni22 O203 Ni21 -157.0(2) . . . . ? O2H Ni22 O203 Ni21 22.13(17) . . . . ? N204 Ni22 O203 Ni21 -74.3(2) . . . . ? N201 Ni21 O203 C226 41.6(5) . . . . ? O201 Ni21 O203 C226 133.3(5) . . . . ? O2H Ni21 O203 C226 -144.3(5) . . . . ? N203 Ni21 O203 C226 -43.5(5) . . . . ? Ni23 Ni21 O203 C226 175.7(4) . . . . ? N201 Ni21 O203 Ni22 163.4(2) . . . . ? O201 Ni21 O203 Ni22 -104.91(19) . . . . ? O2H Ni21 O203 Ni22 -22.53(18) . . . . ? N203 Ni21 O203 Ni22 78.3(2) . . . . ? Ni23 Ni21 O203 Ni22 -62.57(15) . . . . ? O101 Ni11 O1H Ni13 -23.19(19) . . . . ? O11 Ni11 O1H Ni13 68.1(2) . . . . ? N103 Ni11 O1H Ni13 155.0(2) . . . . ? O103 Ni11 O1H Ni13 -115.3(2) . . . . ? O101 Ni11 O1H Ni12 115.0(2) . . . . ? O11 Ni11 O1H Ni12 -153.7(2) . . . . ? N103 Ni11 O1H Ni12 -66.9(2) . . . . ? O103 Ni11 O1H Ni12 22.84(19) . . . . ? Ni13 Ni11 O1H Ni12 138.2(3) . . . . ? O13 Ni13 O1H Ni11 -68.8(2) . . . . ? O101 Ni13 O1H Ni11 22.63(18) . . . . ? O3W Ni13 O1H Ni11 119.34(19) . . . . ? O4W Ni13 O1H Ni11 -159.67(18) . . . . ? O13 Ni13 O1H Ni12 -167.4(3) . . . . ? O101 Ni13 O1H Ni12 -76.0(4) . . . . ? O3W Ni13 O1H Ni12 20.7(4) . . . . ? O4W Ni13 O1H Ni12 101.7(3) . . . . ? Ni11 Ni13 O1H Ni12 -98.6(4) . . . . ? O102 Ni12 O1H Ni11 -113.4(2) . . . . ? O103 Ni12 O1H Ni11 -23.42(19) . . . . ? N104 Ni12 O1H Ni11 64.9(2) . . . . ? Cl1 Ni12 O1H Ni11 157.02(15) . . . . ? O102 Ni12 O1H Ni13 -15.6(4) . . . . ? O103 Ni12 O1H Ni13 74.4(3) . . . . ? N104 Ni12 O1H Ni13 162.8(3) . . . . ? Cl1 Ni12 O1H Ni13 -105.1(3) . . . . ? O201 Ni21 O2H Ni23 -23.4(2) . . . . ? O21 Ni21 O2H Ni23 68.6(2) . . . . ? N203 Ni21 O2H Ni23 155.4(2) . . . . ? O203 Ni21 O2H Ni23 -115.3(2) . . . . ? O201 Ni21 O2H Ni22 114.8(2) . . . . ? O21 Ni21 O2H Ni22 -153.22(19) . . . . ? N203 Ni21 O2H Ni22 -66.4(2) . . . . ? O203 Ni21 O2H Ni22 22.84(18) . . . . ? Ni23 Ni21 O2H Ni22 138.2(3) . . . . ? O23 Ni23 O2H Ni21 -68.9(2) . . . . ? O201 Ni23 O2H Ni21 22.94(18) . . . . ? O3W Ni23 O2H Ni21 -157.87(19) . . . . ? O4W Ni23 O2H Ni21 121.25(19) . . . . ? O23 Ni23 O2H Ni22 -168.3(3) . . . . ? O201 Ni23 O2H Ni22 -76.4(4) . . . . ? O3W Ni23 O2H Ni22 102.8(3) . . . . ? O4W Ni23 O2H Ni22 21.9(3) . . . . ? Ni21 Ni23 O2H Ni22 -99.3(4) . . . . ? O202 Ni22 O2H Ni21 -114.4(2) . . . . ? O203 Ni22 O2H Ni21 -23.25(18) . . . . ? N204 Ni22 O2H Ni21 64.7(2) . . . . ? Cl1 Ni22 O2H Ni21 156.12(14) . . . . ? O202 Ni22 O2H Ni23 -15.8(4) . . . . ? O203 Ni22 O2H Ni23 75.4(3) . . . . ? N204 Ni22 O2H Ni23 163.3(3) . . . . ? Cl1 Ni22 O2H Ni23 -105.2(3) . . . . ? O101 Ni11 O11 C10 37.5(6) . . . . ? N101 Ni11 O11 C10 128.3(6) . . . . ? O1H Ni11 O11 C10 -45.6(6) . . . . ? N103 Ni11 O11 C10 -146.3(6) . . . . ? Ni13 Ni11 O11 C10 -4.3(6) . . . . ? O101 Ni13 O13 C10 -34.4(6) . . . . ? O31 Ni13 O13 C10 -130.8(6) . . . . ? O1H Ni13 O13 C10 46.5(6) . . . . ? O4W Ni13 O13 C10 141.5(6) . . . . ? Ni11 Ni13 O13 C10 5.8(6) . . . . ? N201 Ni21 O21 C20 131.6(6) . . . . ? O201 Ni21 O21 C20 40.1(6) . . . . ? O2H Ni21 O21 C20 -42.7(6) . . . . ? N203 Ni21 O21 C20 -143.2(6) . . . . ? Ni23 Ni21 O21 C20 -1.5(6) . . . . ? O201 Ni23 O23 C20 -37.7(6) . . . . ? O33 Ni23 O23 C20 -135.7(6) . . . . ? O2H Ni23 O23 C20 43.1(6) . . . . ? O3W Ni23 O23 C20 136.0(6) . . . . ? O4W Ni23 O23 C20 163.0(9) . . . . ? Ni21 Ni23 O23 C20 2.6(6) . . . . ? O13 Ni13 O31 C30 -142.2(7) . . . . ? O101 Ni13 O31 C30 126.0(7) . . . . ? O3W Ni13 O31 C30 29.5(7) . . . . ? O4W Ni13 O31 C30 -51.6(7) . . . . ? Ni11 Ni13 O31 C30 146.5(6) . . . . ? O23 Ni23 O33 C30 -127.9(7) . . . . ? O201 Ni23 O33 C30 140.2(7) . . . . ? O3W Ni23 O33 C30 -39.1(7) . . . . ? O4W Ni23 O33 C30 41.8(7) . . . . ? Ni21 Ni23 O33 C30 163.3(6) . . . . ? O101 Ni13 O3W Ni23 -167.6(2) . . . . ? O31 Ni13 O3W Ni23 -71.0(2) . . . . ? O1H Ni13 O3W Ni23 111.9(2) . . . . ? O4W Ni13 O3W Ni23 16.6(2) . . . . ? Ni11 Ni13 O3W Ni23 151.21(12) . . . . ? O23 Ni23 O3W Ni13 157.9(2) . . . . ? O33 Ni23 O3W Ni13 74.1(2) . . . . ? O2H Ni23 O3W Ni13 -106.6(2) . . . . ? O4W Ni23 O3W Ni13 -16.8(2) . . . . ? Ni21 Ni23 O3W Ni13 -126.99(14) . . . . ? O23 Ni23 O4W Ni13 -11.0(11) . . . . ? O201 Ni23 O4W Ni13 -170.1(2) . . . . ? O33 Ni23 O4W Ni13 -71.7(2) . . . . ? O2H Ni23 O4W Ni13 109.4(2) . . . . ? O3W Ni23 O4W Ni13 16.4(2) . . . . ? Ni21 Ni23 O4W Ni13 148.27(11) . . . . ? O13 Ni13 O4W Ni23 159.3(2) . . . . ? O31 Ni13 O4W Ni23 73.9(2) . . . . ? O3W Ni13 O4W Ni23 -16.6(2) . . . . ? O1H Ni13 O4W Ni23 -104.75(19) . . . . ? Ni11 Ni13 O4W Ni23 -124.47(14) . . . . ? Ni13 O13 C10 O11 -11.6(11) . . . . ? Ni13 O13 C10 C11 170.8(5) . . . . ? Ni11 O11 C10 O13 10.5(11) . . . . ? Ni11 O11 C10 C11 -171.8(5) . . . . ? Ni21 O21 C20 O23 3.9(11) . . . . ? Ni21 O21 C20 C21 -173.8(5) . . . . ? Ni23 O23 C20 O21 -4.6(11) . . . . ? Ni23 O23 C20 C21 173.0(5) . . . . ? Ni23 O33 C30 O31 -9.5(12) . . . . ? Ni23 O33 C30 C31 169.9(6) . . . . ? Ni13 O31 C30 O33 15.8(12) . . . . ? Ni13 O31 C30 C31 -163.5(6) . . . . ? Ni11 O101 C100 C101 165.9(5) . . . . ? Ni13 O101 C100 C101 -22.0(11) . . . . ? Ni11 O101 C100 C105 -13.2(10) . . . . ? Ni13 O101 C100 C105 158.9(5) . . . . ? O101 C100 C101 C102 -179.8(7) . . . . ? C105 C100 C101 C102 -0.6(11) . . . . ? C100 C101 C102 C103 0.1(12) . . . . ? C101 C102 C103 C104 -1.0(12) . . . . ? C101 C102 C103 Br11 -178.5(6) . . . . ? C102 C103 C104 C105 2.4(12) . . . . ? Br11 C103 C104 C105 179.8(6) . . . . ? C103 C104 C105 C100 -2.9(12) . . . . ? C103 C104 C105 C106 176.5(7) . . . . ? O101 C100 C105 C104 -178.9(7) . . . . ? C101 C100 C105 C104 2.0(10) . . . . ? O101 C100 C105 C106 1.7(11) . . . . ? C101 C100 C105 C106 -177.4(7) . . . . ? C107 N101 C106 C105 178.3(7) . . . . ? Ni11 N101 C106 C105 -0.3(11) . . . . ? C104 C105 C106 N101 -174.0(7) . . . . ? C100 C105 C106 N101 5.4(12) . . . . ? C106 N101 C107 C108 162.9(7) . . . . ? Ni11 N101 C107 C108 -18.3(7) . . . . ? C120 N103 C108 C107 82.4(8) . . . . ? C109 N103 C108 C107 -163.2(6) . . . . ? Ni11 N103 C108 C107 -42.0(7) . . . . ? N101 C107 C108 N103 41.9(9) . . . . ? C120 N103 C109 C110 -31.8(7) . . . . ? C108 N103 C109 C110 -153.9(6) . . . . ? Ni11 N103 C109 C110 91.2(6) . . . . ? C111 N104 C110 C109 146.8(6) . . . . ? C120 N104 C110 C109 26.7(7) . . . . ? Ni12 N104 C110 C109 -97.0(6) . . . . ? N103 C109 C110 N104 2.5(7) . . . . ? C120 N104 C111 C112 -81.9(7) . . . . ? C110 N104 C111 C112 166.4(6) . . . . ? Ni12 N104 C111 C112 43.6(6) . . . . ? C113 N102 C112 C111 -142.7(7) . . . . ? Ni12 N102 C112 C111 25.6(7) . . . . ? N104 C111 C112 N102 -47.4(8) . . . . ? C112 N102 C113 C114 177.8(7) . . . . ? Ni12 N102 C113 C114 10.8(11) . . . . ? N102 C113 C114 C119 0.5(12) . . . . ? N102 C113 C114 C115 178.6(7) . . . . ? C119 C114 C115 C116 -0.3(11) . . . . ? C113 C114 C115 C116 -178.5(7) . . . . ? C114 C115 C116 C117 -1.4(12) . . . . ? C114 C115 C116 Br12 177.7(5) . . . . ? C115 C116 C117 C118 1.1(12) . . . . ? Br12 C116 C117 C118 -178.0(6) . . . . ? C116 C117 C118 C119 0.9(11) . . . . ? Ni12 O102 C119 C114 -12.3(10) . . . . ? Ni12 O102 C119 C118 167.6(5) . . . . ? C115 C114 C119 O102 -177.9(7) . . . . ? C113 C114 C119 O102 0.1(11) . . . . ? C115 C114 C119 C118 2.1(10) . . . . ? C113 C114 C119 C118 -179.8(7) . . . . ? C117 C118 C119 O102 177.6(7) . . . . ? C117 C118 C119 C114 -2.5(11) . . . . ? C108 N103 C120 N104 169.4(6) . . . . ? C109 N103 C120 N104 49.9(6) . . . . ? Ni11 N103 C120 N104 -72.4(6) . . . . ? C108 N103 C120 C121 -66.4(8) . . . . ? C109 N103 C120 C121 174.1(6) . . . . ? Ni11 N103 C120 C121 51.7(6) . . . . ? C111 N104 C120 N103 -164.8(6) . . . . ? C110 N104 C120 N103 -47.6(6) . . . . ? Ni12 N104 C120 N103 75.9(6) . . . . ? C111 N104 C120 C121 71.8(8) . . . . ? C110 N104 C120 C121 -170.9(6) . . . . ? Ni12 N104 C120 C121 -47.4(7) . . . . ? N103 C120 C121 C122 114.2(7) . . . . ? N104 C120 C121 C122 -128.8(7) . . . . ? N103 C120 C121 C126 -59.6(9) . . . . ? N104 C120 C121 C126 57.4(9) . . . . ? C126 C121 C122 C123 -0.7(11) . . . . ? C120 C121 C122 C123 -174.5(7) . . . . ? C121 C122 C123 C124 -0.6(11) . . . . ? C121 C122 C123 Br13 177.4(5) . . . . ? C122 C123 C124 C125 -0.1(12) . . . . ? Br13 C123 C124 C125 -178.0(6) . . . . ? C123 C124 C125 C126 2.1(12) . . . . ? Ni12 O103 C126 C121 -51.8(8) . . . . ? Ni11 O103 C126 C121 55.0(8) . . . . ? Ni12 O103 C126 C125 129.4(6) . . . . ? Ni11 O103 C126 C125 -123.8(6) . . . . ? C122 C121 C126 O103 -176.1(6) . . . . ? C120 C121 C126 O103 -2.6(10) . . . . ? C122 C121 C126 C125 2.6(11) . . . . ? C120 C121 C126 C125 176.2(7) . . . . ? C124 C125 C126 O103 175.4(7) . . . . ? C124 C125 C126 C121 -3.3(11) . . . . ? Ni21 O201 C200 C205 -7.3(10) . . . . ? Ni23 O201 C200 C205 154.1(6) . . . . ? Ni21 O201 C200 C201 171.3(5) . . . . ? Ni23 O201 C200 C201 -27.3(11) . . . . ? O201 C200 C201 C202 -179.0(7) . . . . ? C205 C200 C201 C202 -0.4(12) . . . . ? C200 C201 C202 C203 0.4(13) . . . . ? C201 C202 C203 C204 -0.9(13) . . . . ? C201 C202 C203 Br21 -179.7(7) . . . . ? C202 C203 C204 C205 1.5(13) . . . . ? Br21 C203 C204 C205 -179.8(6) . . . . ? O201 C200 C205 C204 179.5(7) . . . . ? C201 C200 C205 C204 0.9(11) . . . . ? O201 C200 C205 C206 0.1(12) . . . . ? C201 C200 C205 C206 -178.5(7) . . . . ? C203 C204 C205 C200 -1.5(12) . . . . ? C203 C204 C205 C206 178.0(7) . . . . ? C207 N201 C206 C205 177.4(7) . . . . ? Ni21 N201 C206 C205 -3.1(11) . . . . ? C200 C205 C206 N201 5.6(13) . . . . ? C204 C205 C206 N201 -173.9(7) . . . . ? C206 N201 C207 C208 158.3(7) . . . . ? Ni21 N201 C207 C208 -21.3(7) . . . . ? C220 N203 C208 C207 83.5(8) . . . . ? C209 N203 C208 C207 -162.2(6) . . . . ? Ni21 N203 C208 C207 -41.5(7) . . . . ? N201 C207 C208 N203 43.3(8) . . . . ? C220 N203 C209 C210 -31.1(7) . . . . ? C208 N203 C209 C210 -152.2(6) . . . . ? Ni21 N203 C209 C210 92.7(6) . . . . ? C211 N204 C210 C209 147.9(6) . . . . ? C220 N204 C210 C209 28.6(7) . . . . ? Ni22 N204 C210 C209 -96.6(5) . . . . ? N203 C209 C210 N204 1.1(7) . . . . ? C220 N204 C211 C212 -82.0(7) . . . . ? C210 N204 C211 C212 165.8(6) . . . . ? Ni22 N204 C211 C212 43.6(6) . . . . ? C213 N202 C212 C211 -139.9(7) . . . . ? Ni22 N202 C212 C211 27.3(7) . . . . ? N204 C211 C212 N202 -48.7(8) . . . . ? C212 N202 C213 C214 177.8(7) . . . . ? Ni22 N202 C213 C214 12.3(11) . . . . ? N202 C213 C214 C219 -2.6(12) . . . . ? N202 C213 C214 C215 -179.1(7) . . . . ? C219 C214 C215 C216 0.0(11) . . . . ? C213 C214 C215 C216 176.7(7) . . . . ? C214 C215 C216 C217 -1.2(12) . . . . ? C214 C215 C216 Br22 176.9(6) . . . . ? C215 C216 C217 C218 1.1(13) . . . . ? Br22 C216 C217 C218 -177.0(6) . . . . ? C216 C217 C218 C219 0.2(12) . . . . ? Ni22 O202 C219 C214 -19.1(9) . . . . ? Ni22 O202 C219 C218 162.0(5) . . . . ? C215 C214 C219 O202 -177.7(7) . . . . ? C213 C214 C219 O202 6.0(11) . . . . ? C215 C214 C219 C218 1.3(10) . . . . ? C213 C214 C219 C218 -175.1(7) . . . . ? C217 C218 C219 O202 177.6(7) . . . . ? C217 C218 C219 C214 -1.4(11) . . . . ? C209 N203 C220 N204 50.0(6) . . . . ? C208 N203 C220 N204 169.2(5) . . . . ? Ni21 N203 C220 N204 -72.2(6) . . . . ? C209 N203 C220 C221 173.4(6) . . . . ? C208 N203 C220 C221 -67.3(8) . . . . ? Ni21 N203 C220 C221 51.3(7) . . . . ? C211 N204 C220 N203 -166.2(5) . . . . ? C210 N204 C220 N203 -48.8(6) . . . . ? Ni22 N204 C220 N203 75.4(6) . . . . ? C211 N204 C220 C221 70.5(8) . . . . ? C210 N204 C220 C221 -172.1(6) . . . . ? Ni22 N204 C220 C221 -48.0(8) . . . . ? N203 C220 C221 C222 118.5(7) . . . . ? N204 C220 C221 C222 -125.6(7) . . . . ? N203 C220 C221 C226 -58.5(9) . . . . ? N204 C220 C221 C226 57.5(9) . . . . ? C226 C221 C222 C223 0.5(11) . . . . ? C220 C221 C222 C223 -176.4(7) . . . . ? C221 C222 C223 C224 -1.0(12) . . . . ? C221 C222 C223 Br23 178.2(6) . . . . ? C222 C223 C224 C225 0.7(13) . . . . ? Br23 C223 C224 C225 -178.5(7) . . . . ? C223 C224 C225 C226 0.1(13) . . . . ? Ni22 O203 C226 C221 -52.1(9) . . . . ? Ni21 O203 C226 C221 53.4(8) . . . . ? Ni22 O203 C226 C225 128.9(7) . . . . ? Ni21 O203 C226 C225 -125.6(7) . . . . ? C222 C221 C226 O203 -178.8(7) . . . . ? C220 C221 C226 O203 -2.0(11) . . . . ? C222 C221 C226 C225 0.2(11) . . . . ? C220 C221 C226 C225 177.1(7) . . . . ? C224 C225 C226 O203 178.5(8) . . . . ? C224 C225 C226 C221 -0.6(12) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1H H1 O202 0.69 2.85 3.515(7) 162 . O1H H1 Cl1 0.69 2.98 3.302(5) 113 . O2H H2 O102 0.85 2.59 3.440(7) 180 . O3W H3WA O2W 0.85 1.73 2.584(11) 172 . O3W H3WA O2W' 0.85 2.51 3.335(17) 164 . O3W H3WA O2W" 0.85 1.99 2.76(2) 149 . O3W H3WB O102 0.88 1.69 2.521(7) 159 . O4W H4wA O202 0.91 1.66 2.517(7) 156 . O4W H4wB O3S 0.96 2.02 2.695(7) 125 . O1S H1S O103 0.84 2.39 3.220(8) 172 . O2S H2S O33 0.84 1.96 2.789(8) 168 . O3S H3S O4W 0.84 2.28 2.695(7) 111 . O4S H4S O5S 0.84 1.87 2.708(10) 171 . O5S H5S O31 0.84 1.97 2.798(8) 167 . O6S H6S O3S 0.84 1.83 2.663(9) 173 . O7S H7S O1W 0.84 1.88 2.716(12) 180 . O8S H8S O2S 0.84 1.80 2.639(11) 180 . O1W H1W1 O4S 0.93 1.83 2.756(10) 170 1_455 O1W H2W1 O8S 1.04 1.78 2.763(10) 157 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.003 _refine_diff_density_min -1.774 _refine_diff_density_rms 0.162 #END data_3_H2O_2MeOH_2MeCN _database_code_depnum_ccdc_archive 'CCDC 781534' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H69 N11 Ni6 O16, 2(C H4 O), 2(C2 H3 N), H2 O' _chemical_formula_sum 'C66 H85 N13 Ni6 O19' _chemical_formula_weight 1716.73 _chemical_absolute_configuration . 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.765(3) _cell_length_b 12.792(3) _cell_length_c 21.443(5) _cell_angle_alpha 90 _cell_angle_beta 90.772(4) _cell_angle_gamma 90 _cell_volume 3501.0(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 951 _cell_measurement_theta_min 2.225 _cell_measurement_theta_max 26.375 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 1.663 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5087 _exptl_absorpt_correction_T_max 0.9518 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker CCD SMART1000 ' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.15 _diffrn_reflns_number 29609 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0609 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.68 _reflns_number_total 12876 _reflns_number_gt 10744 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction ? _computing_structure_solution 'SIR-2004 (Burla, 2004)' _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^)+(0.0257P)^2^+3.8586P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.007(10) _refine_ls_number_reflns 12876 _refine_ls_number_parameters 952 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0805 _refine_ls_wR_factor_gt 0.0722 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni11 Ni -0.43617(5) -0.65178(5) -0.62374(3) 0.01254(13) Uani 1 1 d . . . Ni12 Ni -0.40658(5) -0.64273(5) -0.76450(3) 0.01276(13) Uani 1 1 d . . . Ni13 Ni -0.39172(4) -0.42704(5) -0.63924(3) 0.01196(13) Uani 1 1 d . . . Ni21 Ni -0.22981(5) -0.20514(5) -0.85031(3) 0.01325(14) Uani 1 1 d . . . Ni22 Ni -0.17232(5) -0.43502(5) -0.83102(3) 0.01274(13) Uani 1 1 d . . . Ni23 Ni -0.35326(5) -0.25371(5) -0.73771(3) 0.01185(13) Uani 1 1 d . . . N101 N -0.5335(3) -0.7289(3) -0.56779(17) 0.0136(9) Uani 1 1 d . . . N102 N -0.4541(3) -0.7251(3) -0.83958(18) 0.0148(9) Uani 1 1 d . . . N103 N -0.3640(3) -0.7997(3) -0.63401(18) 0.0141(9) Uani 1 1 d . . . N104 N -0.3381(3) -0.7982(3) -0.73956(18) 0.0147(9) Uani 1 1 d . . . N201 N -0.1450(3) -0.0802(3) -0.87365(19) 0.0158(9) Uani 1 1 d . . . N202 N -0.0519(3) -0.5292(3) -0.85308(19) 0.0172(9) Uani 1 1 d . . . N203 N -0.2173(3) -0.2434(3) -0.94575(17) 0.0130(9) Uani 1 1 d . . . N204 N -0.1787(3) -0.4178(3) -0.93573(17) 0.0151(9) Uani 1 1 d . . . N1 N -0.2711(3) -0.5833(3) -0.82394(19) 0.0153(9) Uani 1 1 d . . . N2 N -0.2447(3) -0.6484(4) -0.8610(2) 0.0251(10) Uani 1 1 d . . . N3 N -0.2190(5) -0.7125(4) -0.8961(2) 0.0471(15) Uani 1 1 d . . . O101 O -0.5112(3) -0.5167(2) -0.60743(15) 0.0163(8) Uani 1 1 d . . . O102 O -0.4850(2) -0.5168(2) -0.79799(14) 0.0134(7) Uani 1 1 d . . . O103 O -0.5258(2) -0.6747(2) -0.70396(14) 0.0132(7) Uani 1 1 d . . . O201 O -0.2409(2) -0.1504(3) -0.76332(14) 0.0162(7) Uani 1 1 d . . . O202 O -0.1409(3) -0.4568(3) -0.73936(14) 0.0165(8) Uani 1 1 d . . . O203 O -0.0950(2) -0.2922(3) -0.82954(15) 0.0144(8) Uani 1 1 d . . . O1H O -0.3523(3) -0.5634(2) -0.68644(15) 0.0134(7) Uani 1 1 d . . . O2H O -0.2971(3) -0.3368(3) -0.81370(16) 0.0153(8) Uani 1 1 d . . . O3W O -0.2630(2) -0.3448(2) -0.67795(14) 0.0134(7) Uani 1 1 d . . . H3W1 H -0.2200 -0.3244 -0.6533 0.016 Uiso 1 1 d R . . H3W2 H -0.2183 -0.3763 -0.7010 0.016 Uiso 1 1 d R . . O4W O -0.4651(2) -0.3717(2) -0.71987(14) 0.0118(7) Uani 1 1 d . . . H4W1 H -0.5177 -0.3365 -0.7158 0.014 Uiso 1 1 d R . . H4W2 H -0.4779 -0.4283 -0.7375 0.014 Uiso 1 1 d R . . O11 O -0.3314(3) -0.6276(2) -0.54944(15) 0.0170(8) Uani 1 1 d . . . O13 O -0.2992(3) -0.4575(2) -0.56200(15) 0.0164(8) Uani 1 1 d . . . O23 O -0.4638(2) -0.1781(2) -0.79090(14) 0.0151(7) Uani 1 1 d . . . O21 O -0.3722(2) -0.1323(3) -0.87463(15) 0.0164(7) Uani 1 1 d . . . O31 O -0.4374(3) -0.2967(3) -0.59466(15) 0.0168(8) Uani 1 1 d . . . O33 O -0.4112(3) -0.1705(2) -0.66582(14) 0.0152(8) Uani 1 1 d . . . C10 C -0.2915(4) -0.5436(4) -0.5329(2) 0.0165(11) Uani 1 1 d . . . C11 C -0.2233(4) -0.5432(4) -0.4744(2) 0.0247(13) Uani 1 1 d . . . H11A H -0.2273 -0.6116 -0.4540 0.037 Uiso 1 1 calc R . . H11B H -0.2480 -0.4890 -0.4458 0.037 Uiso 1 1 calc R . . H11C H -0.1506 -0.5287 -0.4856 0.037 Uiso 1 1 calc R . . C20 C -0.4544(4) -0.1342(4) -0.8431(2) 0.0143(10) Uani 1 1 d . . . C21 C -0.5514(4) -0.0838(4) -0.8697(2) 0.0171(11) Uani 1 1 d . . . H21A H -0.5983 -0.1378 -0.8865 0.026 Uiso 1 1 calc R . . H21B H -0.5321 -0.0356 -0.9031 0.026 Uiso 1 1 calc R . . H21C H -0.5872 -0.0450 -0.8368 0.026 Uiso 1 1 calc R . . C30 C -0.4504(4) -0.2050(4) -0.6158(2) 0.0148(10) Uani 1 1 d . . . C31 C -0.5194(4) -0.1334(4) -0.5797(2) 0.0216(12) Uani 1 1 d . . . H31A H -0.4761 -0.0824 -0.5570 0.032 Uiso 1 1 calc R . . H31B H -0.5602 -0.1743 -0.5499 0.032 Uiso 1 1 calc R . . H31C H -0.5671 -0.0967 -0.6084 0.032 Uiso 1 1 calc R . . C100 C -0.6058(4) -0.5056(4) -0.5855(2) 0.0142(11) Uani 1 1 d . . . C101 C -0.6591(4) -0.4093(4) -0.5919(2) 0.0177(11) Uani 1 1 d . . . H101 H -0.6265 -0.3534 -0.6135 0.021 Uiso 1 1 calc R . . C102 C -0.7567(4) -0.3946(4) -0.5675(2) 0.0207(12) Uani 1 1 d . . . H102 H -0.7901 -0.3287 -0.5724 0.025 Uiso 1 1 calc R . . C103 C -0.8084(4) -0.4743(4) -0.5358(2) 0.0228(12) Uani 1 1 d . . . H103 H -0.8759 -0.4634 -0.5188 0.027 Uiso 1 1 calc R . . C104 C -0.7587(4) -0.5689(4) -0.5298(2) 0.0223(12) Uani 1 1 d . . . H104 H -0.7926 -0.6233 -0.5077 0.027 Uiso 1 1 calc R . . C105 C -0.6599(4) -0.5885(4) -0.5550(2) 0.0142(11) Uani 1 1 d . . . C106 C -0.6183(4) -0.6943(4) -0.5462(2) 0.0159(11) Uani 1 1 d . . . H106 H -0.6587 -0.7411 -0.5220 0.019 Uiso 1 1 calc R . . C107 C -0.5042(4) -0.8394(4) -0.5570(2) 0.0176(11) Uani 1 1 d . . . H10A H -0.5501 -0.8858 -0.5823 0.021 Uiso 1 1 calc R . . H10B H -0.5130 -0.8574 -0.5125 0.021 Uiso 1 1 calc R . . C108 C -0.3907(4) -0.8546(4) -0.5754(2) 0.0204(12) Uani 1 1 d . . . H10C H -0.3446 -0.8286 -0.5413 0.024 Uiso 1 1 calc R . . H10D H -0.3769 -0.9303 -0.5805 0.024 Uiso 1 1 calc R . . C109 C -0.2482(4) -0.7927(4) -0.6407(2) 0.0198(12) Uani 1 1 d . . . H10E H -0.2132 -0.8541 -0.6216 0.024 Uiso 1 1 calc R . . H10F H -0.2207 -0.7285 -0.6207 0.024 Uiso 1 1 calc R . . C110 C -0.2310(4) -0.7902(4) -0.7115(2) 0.0173(11) Uani 1 1 d . . . H11D H -0.1968 -0.7241 -0.7241 0.021 Uiso 1 1 calc R . . H11E H -0.1868 -0.8496 -0.7247 0.021 Uiso 1 1 calc R . . C111 C -0.3365(4) -0.8578(4) -0.7989(2) 0.0190(11) Uani 1 1 d . . . H11F H -0.3308 -0.9334 -0.7896 0.023 Uiso 1 1 calc R . . H11G H -0.2742 -0.8371 -0.8230 0.023 Uiso 1 1 calc R . . C112 C -0.4342(4) -0.8380(4) -0.8375(2) 0.0210(12) Uani 1 1 d . . . H11H H -0.4248 -0.8652 -0.8803 0.025 Uiso 1 1 calc R . . H11I H -0.4946 -0.8745 -0.8189 0.025 Uiso 1 1 calc R . . C113 C -0.4859(4) -0.6856(4) -0.8919(2) 0.0157(11) Uani 1 1 d . . . H113 H -0.4931 -0.7324 -0.9261 0.019 Uiso 1 1 calc R . . C114 C -0.5120(4) -0.5768(4) -0.9036(2) 0.0162(11) Uani 1 1 d . . . C115 C -0.5408(4) -0.5509(4) -0.9645(2) 0.0195(11) Uani 1 1 d . . . H115 H -0.5386 -0.6035 -0.9957 0.023 Uiso 1 1 calc R . . C116 C -0.5722(4) -0.4519(4) -0.9810(2) 0.0194(12) Uani 1 1 d . . . H116 H -0.5921 -0.4364 -1.0229 0.023 Uiso 1 1 calc R . . C117 C -0.5745(4) -0.3745(4) -0.9352(2) 0.0179(11) Uani 1 1 d . . . H117 H -0.5963 -0.3056 -0.9457 0.022 Uiso 1 1 calc R . . C118 C -0.5452(4) -0.3977(4) -0.8746(2) 0.0162(11) Uani 1 1 d . . . H118 H -0.5475 -0.3439 -0.8440 0.019 Uiso 1 1 calc R . . C119 C -0.5117(3) -0.4994(4) -0.8562(2) 0.0128(10) Uani 1 1 d . . . C120 C -0.3970(4) -0.8565(4) -0.6908(2) 0.0123(10) Uani 1 1 d . . . H120 H -0.3694 -0.9296 -0.6885 0.015 Uiso 1 1 calc R . . C121 C -0.5134(4) -0.8607(4) -0.7010(2) 0.0146(11) Uani 1 1 d . . . C122 C -0.5639(4) -0.9581(4) -0.7032(2) 0.0168(11) Uani 1 1 d . . . H122 H -0.5234 -1.0203 -0.7040 0.020 Uiso 1 1 calc R . . C123 C -0.6718(4) -0.9645(4) -0.7042(2) 0.0229(12) Uani 1 1 d . . . H123 H -0.7057 -1.0306 -0.7057 0.028 Uiso 1 1 calc R . . C124 C -0.7299(4) -0.8733(4) -0.7031(2) 0.0221(12) Uani 1 1 d . . . H124 H -0.8042 -0.8773 -0.7022 0.027 Uiso 1 1 calc R . . C125 C -0.6820(4) -0.7762(4) -0.7033(2) 0.0180(11) Uani 1 1 d . . . H125 H -0.7235 -0.7145 -0.7031 0.022 Uiso 1 1 calc R . . C126 C -0.5736(4) -0.7687(4) -0.7038(2) 0.0127(10) Uani 1 1 d . . . C200 C -0.1691(4) -0.0942(4) -0.7339(2) 0.0150(11) Uani 1 1 d . . . C201 C -0.1664(4) -0.0880(4) -0.6686(2) 0.0210(12) Uani 1 1 d . . . H201 H -0.2196 -0.1218 -0.6455 0.025 Uiso 1 1 calc R . . C202 C -0.0886(4) -0.0341(4) -0.6369(2) 0.0244(13) Uani 1 1 d . . . H202 H -0.0876 -0.0334 -0.5926 0.029 Uiso 1 1 calc R . . C203 C -0.0114(4) 0.0194(4) -0.6695(3) 0.0287(14) Uani 1 1 d . . . H203 H 0.0429 0.0554 -0.6478 0.034 Uiso 1 1 calc R . . C204 C -0.0151(4) 0.0192(4) -0.7335(3) 0.0236(12) Uani 1 1 d . . . H204 H 0.0365 0.0571 -0.7556 0.028 Uiso 1 1 calc R . . C205 C -0.0931(4) -0.0355(4) -0.7674(2) 0.0177(11) Uani 1 1 d . . . C206 C -0.0888(4) -0.0286(4) -0.8348(2) 0.0184(11) Uani 1 1 d . . . H206 H -0.0396 0.0190 -0.8517 0.022 Uiso 1 1 calc R . . C207 C -0.1272(4) -0.0693(4) -0.9408(2) 0.0205(12) Uani 1 1 d . . . H20A H -0.0544 -0.0899 -0.9505 0.025 Uiso 1 1 calc R . . H20B H -0.1372 0.0045 -0.9535 0.025 Uiso 1 1 calc R . . C208 C -0.2044(4) -0.1391(4) -0.9761(2) 0.0177(11) Uani 1 1 d . . . H20C H -0.2733 -0.1038 -0.9786 0.021 Uiso 1 1 calc R . . H20D H -0.1794 -0.1493 -1.0192 0.021 Uiso 1 1 calc R . . C209 C -0.3120(4) -0.2975(4) -0.9713(2) 0.0178(11) Uani 1 1 d . . . H20E H -0.3216 -0.2826 -1.0163 0.021 Uiso 1 1 calc R . . H20F H -0.3757 -0.2757 -0.9489 0.021 Uiso 1 1 calc R . . C210 C -0.2883(4) -0.4140(4) -0.9602(2) 0.0171(11) Uani 1 1 d . . . H21D H -0.3373 -0.4439 -0.9296 0.021 Uiso 1 1 calc R . . H21E H -0.2948 -0.4539 -0.9996 0.021 Uiso 1 1 calc R . . C211 C -0.1213(4) -0.5104(4) -0.9590(2) 0.0198(12) Uani 1 1 d . . . H21F H -0.0991 -0.4971 -1.0023 0.024 Uiso 1 1 calc R . . H21G H -0.1690 -0.5715 -0.9596 0.024 Uiso 1 1 calc R . . C212 C -0.0251(4) -0.5361(4) -0.9189(2) 0.0184(11) Uani 1 1 d . . . H21H H -0.0003 -0.6075 -0.9285 0.022 Uiso 1 1 calc R . . H21I H 0.0321 -0.4863 -0.9282 0.022 Uiso 1 1 calc R . . C213 C -0.0088(4) -0.5958(4) -0.8160(2) 0.0155(11) Uani 1 1 d . . . H213 H 0.0347 -0.6472 -0.8344 0.019 Uiso 1 1 calc R . . C214 C -0.0197(4) -0.6003(4) -0.7491(2) 0.0150(11) Uani 1 1 d . . . C215 C 0.0391(4) -0.6766(4) -0.7174(2) 0.0204(12) Uani 1 1 d . . . H215 H 0.0809 -0.7232 -0.7410 0.024 Uiso 1 1 calc R . . C216 C 0.0390(4) -0.6868(4) -0.6535(2) 0.0229(12) Uani 1 1 d . . . H216 H 0.0794 -0.7397 -0.6334 0.027 Uiso 1 1 calc R . . C217 C -0.0212(4) -0.6188(4) -0.6191(2) 0.0237(12) Uani 1 1 d . . . H217 H -0.0208 -0.6236 -0.5749 0.028 Uiso 1 1 calc R . . C218 C -0.0823(4) -0.5435(4) -0.6486(2) 0.0172(11) Uani 1 1 d . . . H218 H -0.1251 -0.4996 -0.6239 0.021 Uiso 1 1 calc R . . C219 C -0.0831(4) -0.5297(4) -0.7139(2) 0.0145(11) Uani 1 1 d . . . C220 C -0.1333(4) -0.3184(4) -0.9594(2) 0.0154(11) Uani 1 1 d . . . H220 H -0.1276 -0.3242 -1.0057 0.018 Uiso 1 1 calc R . . C221 C -0.0276(4) -0.2928(4) -0.9334(2) 0.0155(11) Uani 1 1 d . . . C222 C 0.0572(4) -0.2825(4) -0.9726(2) 0.0200(12) Uani 1 1 d . . . H222 H 0.0467 -0.2896 -1.0163 0.024 Uiso 1 1 calc R . . C223 C 0.1571(4) -0.2620(5) -0.9494(3) 0.0277(13) Uani 1 1 d . . . H223 H 0.2148 -0.2547 -0.9766 0.033 Uiso 1 1 calc R . . C224 C 0.1702(4) -0.2525(5) -0.8853(3) 0.0316(14) Uani 1 1 d . . . H224 H 0.2384 -0.2401 -0.8686 0.038 Uiso 1 1 calc R . . C225 C 0.0878(4) -0.2604(5) -0.8452(3) 0.0266(13) Uani 1 1 d . . . H225 H 0.0996 -0.2513 -0.8016 0.032 Uiso 1 1 calc R . . C226 C -0.0139(4) -0.2818(4) -0.8678(2) 0.0179(11) Uani 1 1 d . . . H1H H -0.276(4) -0.569(4) -0.685(2) 0.020(14) Uiso 1 1 d . . . H2H H -0.348(5) -0.361(5) -0.831(3) 0.033(19) Uiso 1 1 d . . . N1S N -0.2446(4) -0.1388(6) -0.1535(3) 0.0600(18) Uani 1 1 d . . . C10S C -0.2595(5) -0.0772(6) -0.1940(3) 0.0422(17) Uani 1 1 d . . . C11S C -0.2754(5) -0.0055(5) -0.2455(3) 0.0487(19) Uani 1 1 d . . . H11J H -0.2147 -0.0082 -0.2730 0.073 Uiso 1 1 calc R . . H11K H -0.2835 0.0656 -0.2293 0.073 Uiso 1 1 calc R . . H11L H -0.3386 -0.0254 -0.2690 0.073 Uiso 1 1 calc R . . N2S N -0.1767(5) -0.6866(5) -0.3269(3) 0.0597(18) Uani 1 1 d . . . C20S C -0.1068(6) -0.7310(6) -0.3226(3) 0.051(2) Uani 1 1 d . . . C21S C -0.0116(6) -0.7929(6) -0.3173(4) 0.068(2) Uani 1 1 d . . . H21J H 0.0201 -0.7827 -0.2758 0.102 Uiso 1 1 calc R . . H21K H 0.0379 -0.7708 -0.3492 0.102 Uiso 1 1 calc R . . H21L H -0.0286 -0.8670 -0.3231 0.102 Uiso 1 1 calc R . . O1S O -0.8254(3) -0.7899(3) -0.43984(16) 0.0216(8) Uani 1 1 d . . . H1S H -0.7858 -0.8399 -0.4492 0.032 Uiso 1 1 calc R . . C1S C -0.9228(5) -0.8008(5) -0.4723(3) 0.0397(16) Uani 1 1 d . . . H1S1 H -0.9594 -0.8629 -0.4570 0.060 Uiso 1 1 calc R . . H1S2 H -0.9101 -0.8085 -0.5170 0.060 Uiso 1 1 calc R . . H1S3 H -0.9659 -0.7387 -0.4652 0.060 Uiso 1 1 calc R . . O2S O -0.1402(4) -0.3424(5) -0.1285(3) 0.0759(17) Uiso 1 1 d . . . H2S H -0.1709 -0.2853 -0.1222 0.114 Uiso 1 1 calc R . . C2S C -0.2153(6) -0.4229(7) -0.1357(4) 0.074(2) Uiso 1 1 d . . . H2S1 H -0.1859 -0.4888 -0.1201 0.110 Uiso 1 1 calc R . . H2S2 H -0.2341 -0.4304 -0.1799 0.110 Uiso 1 1 calc R . . H2S3 H -0.2780 -0.4053 -0.1120 0.110 Uiso 1 1 calc R . . O1W O -0.6400(4) -1.2557(4) -0.7352(2) 0.0357(11) Uani 1 1 d . . . H1W1 H -0.609(6) -1.213(6) -0.745(4) 0.06(3) Uiso 1 1 d . . . H1W2 H -0.712(4) -1.240(4) -0.715(2) 0.015(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni11 0.0167(3) 0.0099(3) 0.0111(3) 0.0005(3) 0.0018(2) 0.0001(3) Ni12 0.0175(3) 0.0103(3) 0.0106(3) -0.0010(3) 0.0016(2) 0.0000(3) Ni13 0.0154(3) 0.0096(3) 0.0108(3) -0.0001(3) 0.0020(2) 0.0000(3) Ni21 0.0151(3) 0.0126(3) 0.0121(3) 0.0009(3) 0.0034(3) -0.0006(3) Ni22 0.0137(3) 0.0136(3) 0.0109(3) -0.0001(3) 0.0021(2) 0.0018(3) Ni23 0.0145(3) 0.0102(3) 0.0110(3) 0.0013(3) 0.0028(3) 0.0008(3) N101 0.019(2) 0.012(2) 0.009(2) 0.0005(17) -0.0004(17) -0.0038(17) N102 0.022(2) 0.010(2) 0.013(2) -0.0011(17) 0.0030(18) 0.0000(17) N103 0.016(2) 0.012(2) 0.015(2) -0.0001(17) 0.0000(17) 0.0000(18) N104 0.017(2) 0.015(2) 0.013(2) 0.0004(17) 0.0052(17) -0.0005(18) N201 0.013(2) 0.015(2) 0.019(2) 0.0075(18) 0.0055(18) 0.0024(18) N202 0.017(2) 0.015(2) 0.019(2) -0.0015(19) 0.0025(19) 0.0002(19) N203 0.013(2) 0.017(2) 0.0091(19) 0.0028(17) 0.0033(16) -0.0028(17) N204 0.014(2) 0.017(2) 0.014(2) 0.0024(19) 0.0037(16) -0.0015(19) N1 0.017(2) 0.014(2) 0.014(2) -0.0048(18) 0.0030(18) 0.0019(18) N2 0.031(3) 0.022(2) 0.024(2) -0.001(2) 0.011(2) -0.011(2) N3 0.074(4) 0.025(3) 0.043(3) -0.014(3) 0.040(3) -0.016(3) O101 0.019(2) 0.0127(18) 0.0174(18) -0.0021(14) 0.0046(15) -0.0017(15) O102 0.0187(18) 0.0120(18) 0.0094(17) 0.0016(14) -0.0013(14) 0.0013(14) O103 0.0179(17) 0.0096(18) 0.0120(17) -0.0003(13) 0.0023(14) 0.0000(13) O201 0.0187(17) 0.0139(17) 0.0160(17) 0.0003(16) 0.0031(14) -0.0067(16) O202 0.0184(18) 0.020(2) 0.0113(17) -0.0006(14) 0.0012(14) 0.0066(15) O203 0.0127(18) 0.0180(19) 0.0125(18) -0.0014(14) 0.0043(14) -0.0013(15) O1H 0.0154(19) 0.0125(19) 0.0125(18) -0.0010(14) 0.0020(14) 0.0000(14) O2H 0.0127(19) 0.017(2) 0.0159(19) -0.0004(15) -0.0002(16) -0.0021(15) O3W 0.0160(18) 0.0152(18) 0.0090(17) -0.0026(14) 0.0019(14) 0.0008(15) O4W 0.0174(18) 0.0045(16) 0.0135(17) -0.0027(13) -0.0007(14) 0.0037(13) O11 0.0256(19) 0.0110(19) 0.0145(17) 0.0008(14) 0.0004(14) -0.0019(15) O13 0.0228(19) 0.0151(19) 0.0112(17) 0.0014(14) -0.0004(14) 0.0006(14) O23 0.0190(18) 0.0122(18) 0.0143(17) 0.0051(14) 0.0055(14) 0.0039(14) O21 0.0165(17) 0.0156(19) 0.0171(17) 0.0027(15) 0.0023(14) 0.0025(15) O31 0.025(2) 0.0107(18) 0.0150(18) -0.0010(14) 0.0052(15) 0.0016(15) O33 0.0252(19) 0.0084(18) 0.0120(17) 0.0001(13) 0.0053(14) 0.0009(14) C10 0.016(3) 0.019(3) 0.014(3) -0.001(2) 0.003(2) 0.000(2) C11 0.031(3) 0.024(3) 0.019(3) 0.005(2) -0.008(2) -0.002(2) C20 0.017(3) 0.010(3) 0.016(2) 0.001(2) 0.000(2) -0.002(2) C21 0.018(3) 0.016(3) 0.016(3) 0.002(2) -0.004(2) -0.001(2) C30 0.017(3) 0.012(2) 0.016(3) 0.001(2) 0.002(2) 0.000(2) C31 0.031(3) 0.014(3) 0.021(3) 0.002(2) 0.009(2) 0.008(2) C100 0.015(3) 0.017(3) 0.010(2) -0.004(2) 0.001(2) -0.002(2) C101 0.023(3) 0.017(3) 0.013(2) 0.004(2) 0.004(2) -0.002(2) C102 0.024(3) 0.016(3) 0.022(3) 0.001(2) -0.002(2) 0.005(2) C103 0.012(3) 0.029(3) 0.028(3) 0.002(2) 0.006(2) 0.007(2) C104 0.021(3) 0.020(3) 0.026(3) 0.004(2) 0.002(2) -0.006(2) C105 0.015(3) 0.014(3) 0.014(3) 0.003(2) -0.002(2) 0.001(2) C106 0.015(3) 0.017(3) 0.016(3) 0.005(2) 0.003(2) -0.006(2) C107 0.026(3) 0.011(3) 0.016(3) -0.001(2) 0.004(2) 0.001(2) C108 0.031(3) 0.013(3) 0.018(3) 0.003(2) -0.002(2) 0.001(2) C109 0.014(3) 0.018(3) 0.028(3) -0.003(2) -0.002(2) 0.004(2) C110 0.012(2) 0.017(3) 0.024(3) 0.000(2) 0.005(2) 0.002(2) C111 0.028(3) 0.014(3) 0.015(3) -0.002(2) 0.005(2) 0.005(2) C112 0.040(3) 0.012(3) 0.012(3) -0.003(2) 0.002(2) -0.004(2) C113 0.018(3) 0.017(3) 0.012(2) -0.005(2) 0.001(2) -0.002(2) C114 0.017(3) 0.018(3) 0.013(3) -0.001(2) 0.002(2) -0.002(2) C115 0.020(3) 0.025(3) 0.014(3) -0.003(2) -0.002(2) -0.004(2) C116 0.017(3) 0.026(3) 0.015(3) 0.006(2) -0.001(2) 0.000(2) C117 0.014(3) 0.020(3) 0.020(3) 0.006(2) -0.001(2) -0.003(2) C118 0.016(3) 0.018(3) 0.015(3) 0.002(2) 0.005(2) 0.003(2) C119 0.006(2) 0.019(3) 0.013(2) 0.001(2) 0.0011(19) -0.003(2) C120 0.019(3) 0.009(2) 0.009(2) 0.001(2) 0.004(2) 0.001(2) C121 0.017(3) 0.017(3) 0.010(2) 0.000(2) 0.007(2) 0.002(2) C122 0.027(3) 0.009(3) 0.014(3) -0.0015(19) 0.003(2) 0.004(2) C123 0.029(3) 0.015(3) 0.026(3) -0.005(2) -0.001(2) -0.008(2) C124 0.019(3) 0.024(3) 0.024(3) 0.002(2) 0.001(2) -0.004(2) C125 0.019(3) 0.012(3) 0.022(3) 0.002(2) -0.001(2) 0.005(2) C126 0.020(3) 0.010(3) 0.008(2) 0.0007(19) 0.0027(19) -0.002(2) C200 0.016(3) 0.010(3) 0.018(3) -0.002(2) 0.001(2) 0.006(2) C201 0.027(3) 0.016(3) 0.020(3) 0.000(2) -0.001(2) -0.004(2) C202 0.032(3) 0.026(3) 0.016(3) -0.006(2) -0.001(2) -0.002(3) C203 0.031(3) 0.030(3) 0.025(3) -0.003(3) -0.006(3) -0.010(3) C204 0.021(3) 0.023(3) 0.027(3) -0.002(2) 0.005(2) -0.008(2) C205 0.018(3) 0.015(3) 0.021(3) 0.003(2) 0.004(2) -0.001(2) C206 0.021(3) 0.013(3) 0.022(3) -0.003(2) 0.007(2) -0.004(2) C207 0.029(3) 0.017(3) 0.016(3) 0.004(2) 0.003(2) -0.002(2) C208 0.020(3) 0.018(3) 0.015(2) 0.007(2) -0.001(2) 0.001(2) C209 0.017(3) 0.022(3) 0.015(3) 0.001(2) -0.001(2) 0.001(2) C210 0.020(3) 0.021(3) 0.011(2) 0.001(2) 0.005(2) -0.001(2) C211 0.030(3) 0.014(3) 0.016(3) -0.005(2) 0.003(2) -0.002(2) C212 0.023(3) 0.017(3) 0.015(3) 0.000(2) 0.007(2) 0.005(2) C213 0.013(3) 0.017(3) 0.017(3) -0.001(2) 0.003(2) 0.002(2) C214 0.016(3) 0.013(3) 0.016(3) -0.001(2) 0.003(2) -0.001(2) C215 0.015(3) 0.020(3) 0.026(3) 0.002(2) 0.001(2) 0.005(2) C216 0.014(3) 0.027(3) 0.027(3) 0.008(2) -0.006(2) 0.005(2) C217 0.029(3) 0.026(3) 0.016(3) 0.005(2) -0.003(2) 0.000(2) C218 0.018(3) 0.016(3) 0.018(3) -0.003(2) 0.004(2) 0.005(2) C219 0.009(3) 0.014(3) 0.020(3) 0.000(2) -0.004(2) -0.002(2) C220 0.015(3) 0.023(3) 0.009(3) 0.000(2) 0.005(2) 0.001(2) C221 0.012(2) 0.015(3) 0.020(3) 0.000(2) 0.001(2) 0.003(2) C222 0.020(3) 0.023(3) 0.017(3) 0.007(2) 0.005(2) 0.005(2) C223 0.017(3) 0.042(4) 0.024(3) 0.010(3) 0.007(2) 0.002(3) C224 0.016(3) 0.051(4) 0.028(3) 0.007(3) 0.001(2) -0.010(3) C225 0.016(3) 0.041(3) 0.023(3) 0.002(3) -0.004(2) -0.001(3) C226 0.017(3) 0.015(3) 0.022(3) 0.003(2) 0.002(2) 0.003(2) N1S 0.028(3) 0.101(6) 0.051(4) -0.016(4) 0.005(3) 0.006(4) C10S 0.021(3) 0.064(5) 0.042(4) -0.017(4) 0.013(3) 0.006(3) C11S 0.032(4) 0.035(4) 0.079(6) -0.009(4) 0.011(4) 0.012(3) N2S 0.064(4) 0.050(4) 0.066(5) -0.006(3) 0.016(4) -0.004(4) C20S 0.059(5) 0.051(5) 0.042(4) 0.002(4) -0.009(4) -0.013(4) C21S 0.076(6) 0.047(5) 0.081(6) 0.005(4) 0.014(5) 0.013(4) O1S 0.0218(19) 0.020(2) 0.023(2) 0.0032(16) -0.0024(16) 0.0033(16) C1S 0.031(3) 0.041(4) 0.047(4) 0.015(3) -0.016(3) 0.006(3) O1W 0.031(3) 0.025(2) 0.051(3) 0.008(2) 0.007(2) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni11 N101 1.999(4) . ? Ni11 O101 2.009(3) . ? Ni11 O1H 2.067(3) . ? Ni11 O103 2.074(3) . ? Ni11 O11 2.089(3) . ? Ni11 N103 2.118(4) . ? Ni11 Ni13 2.9499(10) . ? Ni12 N102 2.011(4) . ? Ni12 O102 2.023(3) . ? Ni12 O103 2.055(3) . ? Ni12 O1H 2.069(3) . ? Ni12 N104 2.234(4) . ? Ni12 N1 2.292(4) . ? Ni13 O31 2.012(3) . ? Ni13 O101 2.034(3) . ? Ni13 O13 2.058(3) . ? Ni13 O4W 2.079(3) . ? Ni13 O1H 2.082(3) . ? Ni13 O3W 2.129(3) . ? Ni21 N201 1.998(4) . ? Ni21 O201 1.999(3) . ? Ni21 O2H 2.052(4) . ? Ni21 O203 2.093(3) . ? Ni21 O21 2.102(3) . ? Ni21 N203 2.112(4) . ? Ni21 Ni23 2.9667(10) . ? Ni22 N202 2.014(4) . ? Ni22 O202 2.020(3) . ? Ni22 O2H 2.066(3) . ? Ni22 O203 2.076(3) . ? Ni22 N204 2.256(4) . ? Ni22 N1 2.284(4) . ? Ni23 O33 2.022(3) . ? Ni23 O201 2.031(3) . ? Ni23 O23 2.046(3) . ? Ni23 O3W 2.070(3) . ? Ni23 O2H 2.081(3) . ? Ni23 O4W 2.116(3) . ? N101 C106 1.263(6) . ? N101 C107 1.480(6) . ? N102 C113 1.291(6) . ? N102 C112 1.468(6) . ? N103 C120 1.475(6) . ? N103 C108 1.484(6) . ? N103 C109 1.490(6) . ? N104 C111 1.483(6) . ? N104 C110 1.490(6) . ? N104 C120 1.495(6) . ? N201 C206 1.276(6) . ? N201 C207 1.467(6) . ? N202 C213 1.284(6) . ? N202 C212 1.459(6) . ? N203 C220 1.471(6) . ? N203 C209 1.491(6) . ? N203 C208 1.495(6) . ? N204 C211 1.483(6) . ? N204 C220 1.489(6) . ? N204 C210 1.488(6) . ? N1 N2 1.202(6) . ? N2 N3 1.163(6) . ? O101 C100 1.310(6) . ? O102 C119 1.309(5) . ? O103 C126 1.349(5) . ? O201 C200 1.318(6) . ? O202 C219 1.305(6) . ? O203 C226 1.335(6) . ? O1H H1H 0.98(5) . ? O2H H2H 0.81(6) . ? O3W H3W1 0.8003 . ? O3W H3W2 0.8609 . ? O4W H4W1 0.8153 . ? O4W H4W2 0.8318 . ? O11 C10 1.239(6) . ? O13 C10 1.270(6) . ? O23 C20 1.259(5) . ? O21 C20 1.257(5) . ? O31 C30 1.268(6) . ? O33 C30 1.268(5) . ? C10 C11 1.516(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C20 C21 1.502(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C30 C31 1.494(7) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C100 C101 1.413(7) . ? C100 C105 1.429(7) . ? C101 C102 1.370(7) . ? C101 H101 0.9500 . ? C102 C103 1.396(7) . ? C102 H102 0.9500 . ? C103 C104 1.371(7) . ? C103 H103 0.9500 . ? C104 C105 1.401(7) . ? C104 H104 0.9500 . ? C105 C106 1.464(7) . ? C106 H106 0.9500 . ? C107 C108 1.519(7) . ? C107 H10A 0.9900 . ? C107 H10B 0.9900 . ? C108 H10C 0.9900 . ? C108 H10D 0.9900 . ? C109 C110 1.538(7) . ? C109 H10E 0.9900 . ? C109 H10F 0.9900 . ? C110 H11D 0.9900 . ? C110 H11E 0.9900 . ? C111 C112 1.510(7) . ? C111 H11F 0.9900 . ? C111 H11G 0.9900 . ? C112 H11H 0.9900 . ? C112 H11I 0.9900 . ? C113 C114 1.452(7) . ? C113 H113 0.9500 . ? C114 C115 1.392(7) . ? C114 C119 1.418(7) . ? C115 C116 1.373(7) . ? C115 H115 0.9500 . ? C116 C117 1.396(7) . ? C116 H116 0.9500 . ? C117 C118 1.380(7) . ? C117 H117 0.9500 . ? C118 C119 1.424(6) . ? C118 H118 0.9500 . ? C120 C121 1.500(7) . ? C120 H120 1.0000 . ? C121 C122 1.403(7) . ? C121 C126 1.406(6) . ? C122 C123 1.379(7) . ? C122 H122 0.9500 . ? C123 C124 1.383(7) . ? C123 H123 0.9500 . ? C124 C125 1.384(7) . ? C124 H124 0.9500 . ? C125 C126 1.387(7) . ? C125 H125 0.9500 . ? C200 C201 1.402(7) . ? C200 C205 1.428(7) . ? C201 C202 1.380(7) . ? C201 H201 0.9500 . ? C202 C203 1.395(8) . ? C202 H202 0.9500 . ? C203 C204 1.371(7) . ? C203 H203 0.9500 . ? C204 C205 1.410(7) . ? C204 H204 0.9500 . ? C205 C206 1.451(7) . ? C206 H206 0.9500 . ? C207 C208 1.525(7) . ? C207 H20A 0.9900 . ? C207 H20B 0.9900 . ? C208 H20C 0.9900 . ? C208 H20D 0.9900 . ? C209 C210 1.539(7) . ? C209 H20E 0.9900 . ? C209 H20F 0.9900 . ? C210 H21D 0.9900 . ? C210 H21E 0.9900 . ? C211 C212 1.526(7) . ? C211 H21F 0.9900 . ? C211 H21G 0.9900 . ? C212 H21H 0.9900 . ? C212 H21I 0.9900 . ? C213 C214 1.444(6) . ? C213 H213 0.9500 . ? C214 C215 1.402(7) . ? C215 C216 1.378(7) . ? C215 H215 0.9500 . ? C216 C217 1.380(7) . ? C216 H216 0.9500 . ? C217 C218 1.386(7) . ? C217 H217 0.9500 . ? C218 H218 0.9500 . ? C219 C218 1.412(7) . ? C219 C214 1.433(7) . ? C220 C221 1.490(7) . ? C220 H220 1.0000 . ? C221 C222 1.385(7) . ? C221 C226 1.423(7) . ? C222 C223 1.387(7) . ? C222 H222 0.9500 . ? C223 C224 1.388(7) . ? C223 H223 0.9500 . ? C224 C225 1.371(7) . ? C224 H224 0.9500 . ? C225 C226 1.407(7) . ? C225 H225 0.9500 . ? N1S C10S 1.187(9) . ? C10S C11S 1.447(10) . ? C11S H11J 0.9800 . ? C11S H11K 0.9800 . ? C11S H11L 0.9800 . ? N2S C20S 1.060(9) . ? C20S C21S 1.455(11) . ? C21S H21J 0.9800 . ? C21S H21K 0.9800 . ? C21S H21L 0.9800 . ? O1S C1S 1.423(6) . ? O1S H1S 0.8400 . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? O2S C2S 1.414(9) . ? O2S H2S 0.8400 . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? O1W H1W1 0.71(7) . ? O1W H1W2 1.04(5) . ? 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 N101 Ni11 O101 91.05(15) . . ? N101 Ni11 O1H 172.76(15) . . ? O101 Ni11 O1H 83.99(13) . . ? N101 Ni11 O103 95.02(14) . . ? O101 Ni11 O103 90.39(13) . . ? O1H Ni11 O103 79.78(13) . . ? N101 Ni11 O11 90.69(14) . . ? O101 Ni11 O11 92.38(13) . . ? O1H Ni11 O11 94.78(13) . . ? O103 Ni11 O11 173.60(13) . . ? N101 Ni11 N103 84.03(16) . . ? O101 Ni11 N103 174.91(15) . . ? O1H Ni11 N103 101.03(14) . . ? O103 Ni11 N103 91.33(14) . . ? O11 Ni11 N103 86.39(14) . . ? N101 Ni11 Ni13 132.11(12) . . ? O101 Ni11 Ni13 43.46(9) . . ? O1H Ni11 Ni13 44.89(9) . . ? O103 Ni11 Ni13 98.58(9) . . ? O11 Ni11 Ni13 79.60(9) . . ? N103 Ni11 Ni13 140.78(11) . . ? N102 Ni12 O102 89.45(14) . . ? N102 Ni12 O103 100.59(14) . . ? O102 Ni12 O103 90.89(12) . . ? N102 Ni12 O1H 177.25(15) . . ? O102 Ni12 O1H 93.19(13) . . ? O103 Ni12 O1H 80.18(13) . . ? N102 Ni12 N104 80.68(15) . . ? O102 Ni12 N104 169.64(14) . . ? O103 Ni12 N104 87.84(13) . . ? O1H Ni12 N104 96.73(14) . . ? N102 Ni12 N1 87.14(15) . . ? O102 Ni12 N1 84.95(14) . . ? O103 Ni12 N1 171.21(14) . . ? O1H Ni12 N1 92.30(14) . . ? N104 Ni12 N1 97.63(14) . . ? O31 Ni13 O101 94.83(13) . . ? O31 Ni13 O13 86.65(13) . . ? O101 Ni13 O13 92.76(13) . . ? O31 Ni13 O4W 89.02(13) . . ? O101 Ni13 O4W 98.01(13) . . ? O13 Ni13 O4W 168.69(13) . . ? O31 Ni13 O1H 177.12(14) . . ? O101 Ni13 O1H 82.98(13) . . ? O13 Ni13 O1H 95.32(13) . . ? O4W Ni13 O1H 89.42(13) . . ? O31 Ni13 O3W 90.34(13) . . ? O101 Ni13 O3W 174.77(13) . . ? O13 Ni13 O3W 88.29(13) . . ? O4W Ni13 O3W 81.29(12) . . ? O1H Ni13 O3W 91.82(13) . . ? O31 Ni13 Ni11 134.14(10) . . ? O101 Ni13 Ni11 42.80(9) . . ? O13 Ni13 Ni11 80.44(9) . . ? O4W Ni13 Ni11 109.89(9) . . ? O1H Ni13 Ni11 44.47(9) . . ? O3W Ni13 Ni11 132.55(9) . . ? N201 Ni21 O201 89.94(15) . . ? N201 Ni21 O2H 169.64(16) . . ? O201 Ni21 O2H 83.99(13) . . ? N201 Ni21 O203 91.84(14) . . ? O201 Ni21 O203 93.23(13) . . ? O2H Ni21 O203 80.16(13) . . ? N201 Ni21 O21 93.03(15) . . ? O201 Ni21 O21 90.24(13) . . ? O2H Ni21 O21 95.38(14) . . ? O203 Ni21 O21 174.02(13) . . ? N201 Ni21 N203 83.93(16) . . ? O201 Ni21 N203 172.88(15) . . ? O2H Ni21 N203 102.60(15) . . ? O203 Ni21 N203 90.59(14) . . ? O21 Ni21 N203 86.49(14) . . ? N201 Ni21 Ni23 131.83(12) . . ? O201 Ni21 Ni23 43.03(9) . . ? O2H Ni21 Ni23 44.52(10) . . ? O203 Ni21 Ni23 99.19(9) . . ? O21 Ni21 Ni23 80.08(9) . . ? N203 Ni21 Ni23 142.00(11) . . ? N202 Ni22 O202 90.23(15) . . ? N202 Ni22 O2H 176.77(16) . . ? O202 Ni22 O2H 93.00(13) . . ? N202 Ni22 O203 99.51(16) . . ? O202 Ni22 O203 91.06(13) . . ? O2H Ni22 O203 80.24(14) . . ? N202 Ni22 N204 80.92(16) . . ? O202 Ni22 N204 170.32(14) . . ? O2H Ni22 N204 95.85(14) . . ? O203 Ni22 N204 86.59(14) . . ? N202 Ni22 N1 86.72(16) . . ? O202 Ni22 N1 85.59(14) . . ? O2H Ni22 N1 93.73(15) . . ? O203 Ni22 N1 172.95(14) . . ? N204 Ni22 N1 97.72(15) . . ? O33 Ni23 O201 97.48(13) . . ? O33 Ni23 O23 85.37(13) . . ? O201 Ni23 O23 91.47(13) . . ? O33 Ni23 O3W 91.75(13) . . ? O201 Ni23 O3W 98.31(13) . . ? O23 Ni23 O3W 170.09(13) . . ? O33 Ni23 O2H 178.09(14) . . ? O201 Ni23 O2H 82.48(13) . . ? O23 Ni23 O2H 92.72(13) . . ? O3W Ni23 O2H 90.15(13) . . ? O33 Ni23 O4W 89.05(12) . . ? O201 Ni23 O4W 173.46(13) . . ? O23 Ni23 O4W 88.65(12) . . ? O3W Ni23 O4W 81.81(12) . . ? O2H Ni23 O4W 90.98(13) . . ? O33 Ni23 Ni21 135.56(9) . . ? O201 Ni23 Ni21 42.19(9) . . ? O23 Ni23 Ni21 79.47(9) . . ? O3W Ni23 Ni21 108.93(9) . . ? O2H Ni23 Ni21 43.74(10) . . ? O4W Ni23 Ni21 131.57(9) . . ? C106 N101 C107 119.6(4) . . ? C106 N101 Ni11 126.1(3) . . ? C107 N101 Ni11 114.0(3) . . ? C113 N102 C112 117.6(4) . . ? C113 N102 Ni12 125.4(3) . . ? C112 N102 Ni12 116.2(3) . . ? C120 N103 C108 113.7(4) . . ? C120 N103 C109 102.9(4) . . ? C108 N103 C109 110.4(4) . . ? C120 N103 Ni11 114.0(3) . . ? C108 N103 Ni11 103.3(3) . . ? C109 N103 Ni11 112.9(3) . . ? C111 N104 C110 111.0(4) . . ? C111 N104 C120 110.9(4) . . ? C110 N104 C120 102.7(4) . . ? C111 N104 Ni12 105.2(3) . . ? C110 N104 Ni12 112.9(3) . . ? C120 N104 Ni12 114.4(3) . . ? C206 N201 C207 119.9(4) . . ? C206 N201 Ni21 123.5(4) . . ? C207 N201 Ni21 114.4(3) . . ? C213 N202 C212 117.0(4) . . ? C213 N202 Ni22 125.0(3) . . ? C212 N202 Ni22 116.9(3) . . ? C220 N203 C209 102.3(4) . . ? C220 N203 C208 114.3(4) . . ? C209 N203 C208 110.4(4) . . ? C220 N203 Ni21 114.1(3) . . ? C209 N203 Ni21 113.1(3) . . ? C208 N203 Ni21 103.1(3) . . ? C211 N204 C220 111.8(4) . . ? C211 N204 C210 112.0(4) . . ? C220 N204 C210 102.7(4) . . ? C211 N204 Ni22 104.2(3) . . ? C220 N204 Ni22 114.4(3) . . ? C210 N204 Ni22 112.1(3) . . ? N2 N1 Ni22 111.8(3) . . ? N2 N1 Ni12 111.0(3) . . ? Ni22 N1 Ni12 137.21(19) . . ? N3 N2 N1 178.8(6) . . ? C100 O101 Ni11 126.9(3) . . ? C100 O101 Ni13 139.3(3) . . ? Ni11 O101 Ni13 93.73(14) . . ? C119 O102 Ni12 126.5(3) . . ? C126 O103 Ni12 121.3(3) . . ? C126 O103 Ni11 111.6(3) . . ? Ni12 O103 Ni11 95.21(13) . . ? C200 O201 Ni21 125.4(3) . . ? C200 O201 Ni23 135.6(3) . . ? Ni21 O201 Ni23 94.78(13) . . ? C219 O202 Ni22 127.5(3) . . ? C226 O203 Ni22 116.8(3) . . ? C226 O203 Ni21 117.3(3) . . ? Ni22 O203 Ni21 94.32(13) . . ? Ni11 O1H Ni12 95.01(14) . . ? Ni11 O1H Ni13 90.64(13) . . ? Ni12 O1H Ni13 136.35(18) . . ? Ni11 O1H H1H 118(3) . . ? Ni12 O1H H1H 108(3) . . ? Ni13 O1H H1H 107(3) . . ? Ni21 O2H Ni22 95.87(14) . . ? Ni21 O2H Ni23 91.74(14) . . ? Ni22 O2H Ni23 136.53(19) . . ? Ni21 O2H H2H 119(4) . . ? Ni22 O2H H2H 108(4) . . ? Ni23 O2H H2H 106(4) . . ? Ni23 O3W Ni13 95.37(13) . . ? Ni23 O3W H3W1 126.7 . . ? Ni13 O3W H3W1 115.4 . . ? Ni23 O3W H3W2 106.0 . . ? Ni13 O3W H3W2 120.9 . . ? H3W1 O3W H3W2 94.4 . . ? Ni13 O4W Ni23 95.51(13) . . ? Ni13 O4W H4W1 117.5 . . ? Ni23 O4W H4W1 100.6 . . ? Ni13 O4W H4W2 99.6 . . ? Ni23 O4W H4W2 131.9 . . ? H4W1 O4W H4W2 111.8 . . ? C10 O11 Ni11 127.2(3) . . ? C10 O13 Ni13 126.9(3) . . ? C20 O23 Ni23 129.3(3) . . ? C20 O21 Ni21 125.7(3) . . ? C30 O31 Ni13 129.3(3) . . ? C30 O33 Ni23 127.8(3) . . ? O11 C10 O13 125.6(4) . . ? O11 C10 C11 118.0(5) . . ? O13 C10 C11 116.3(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O21 C20 O23 125.2(4) . . ? O21 C20 C21 118.5(4) . . ? O23 C20 C21 116.2(4) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O31 C30 O33 125.0(4) . . ? O31 C30 C31 117.1(4) . . ? O33 C30 C31 117.8(4) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O101 C100 C101 120.3(4) . . ? O101 C100 C105 122.5(4) . . ? C101 C100 C105 117.2(4) . . ? C102 C101 C100 121.4(4) . . ? C102 C101 H101 119.3 . . ? C100 C101 H101 119.3 . . ? C101 C102 C103 121.6(5) . . ? C101 C102 H102 119.2 . . ? C103 C102 H102 119.2 . . ? C104 C103 C102 118.0(5) . . ? C104 C103 H103 121.0 . . ? C102 C103 H103 121.0 . . ? C103 C104 C105 122.7(5) . . ? C103 C104 H104 118.7 . . ? C105 C104 H104 118.7 . . ? C104 C105 C100 119.1(4) . . ? C104 C105 C106 116.3(4) . . ? C100 C105 C106 124.6(4) . . ? N101 C106 C105 126.0(4) . . ? N101 C106 H106 117.0 . . ? C105 C106 H106 117.0 . . ? N101 C107 C108 108.8(4) . . ? N101 C107 H10A 109.9 . . ? C108 C107 H10A 109.9 . . ? N101 C107 H10B 109.9 . . ? C108 C107 H10B 109.9 . . ? H10A C107 H10B 108.3 . . ? N103 C108 C107 112.9(4) . . ? N103 C108 H10C 109.0 . . ? C107 C108 H10C 109.0 . . ? N103 C108 H10D 109.0 . . ? C107 C108 H10D 109.0 . . ? H10C C108 H10D 107.8 . . ? N103 C109 C110 104.6(4) . . ? N103 C109 H10E 110.8 . . ? C110 C109 H10E 110.8 . . ? N103 C109 H10F 110.8 . . ? C110 C109 H10F 110.8 . . ? H10E C109 H10F 108.9 . . ? N104 C110 C109 104.7(4) . . ? N104 C110 H11D 110.8 . . ? C109 C110 H11D 110.8 . . ? N104 C110 H11E 110.8 . . ? C109 C110 H11E 110.8 . . ? H11D C110 H11E 108.9 . . ? N104 C111 C112 111.3(4) . . ? N104 C111 H11F 109.4 . . ? C112 C111 H11F 109.4 . . ? N104 C111 H11G 109.4 . . ? C112 C111 H11G 109.4 . . ? H11F C111 H11G 108.0 . . ? N102 C112 C111 108.8(4) . . ? N102 C112 H11H 109.9 . . ? C111 C112 H11H 109.9 . . ? N102 C112 H11I 109.9 . . ? C111 C112 H11I 109.9 . . ? H11H C112 H11I 108.3 . . ? N102 C113 C114 126.4(4) . . ? N102 C113 H113 116.8 . . ? C114 C113 H113 116.8 . . ? C115 C114 C119 120.2(5) . . ? C115 C114 C113 116.6(4) . . ? C119 C114 C113 123.2(4) . . ? C116 C115 C114 122.3(5) . . ? C116 C115 H115 118.8 . . ? C114 C115 H115 118.8 . . ? C115 C116 C117 118.7(5) . . ? C115 C116 H116 120.6 . . ? C117 C116 H116 120.6 . . ? C118 C117 C116 120.2(5) . . ? C118 C117 H117 119.9 . . ? C116 C117 H117 119.9 . . ? C117 C118 C119 122.2(5) . . ? C117 C118 H118 118.9 . . ? C119 C118 H118 118.9 . . ? O102 C119 C114 124.2(4) . . ? O102 C119 C118 119.5(4) . . ? C114 C119 C118 116.3(4) . . ? N103 C120 N104 101.0(4) . . ? N103 C120 C121 114.1(4) . . ? N104 C120 C121 115.0(4) . . ? N103 C120 H120 108.8 . . ? N104 C120 H120 108.8 . . ? C121 C120 H120 108.8 . . ? C122 C121 C126 119.4(4) . . ? C122 C121 C120 119.3(4) . . ? C126 C121 C120 121.1(4) . . ? C123 C122 C121 120.8(4) . . ? C123 C122 H122 119.6 . . ? C121 C122 H122 119.6 . . ? C122 C123 C124 119.0(5) . . ? C122 C123 H123 120.5 . . ? C124 C123 H123 120.5 . . ? C125 C124 C123 121.4(5) . . ? C125 C124 H124 119.3 . . ? C123 C124 H124 119.3 . . ? C124 C125 C126 120.1(5) . . ? C124 C125 H125 119.9 . . ? C126 C125 H125 119.9 . . ? O103 C126 C125 120.9(4) . . ? O103 C126 C121 119.9(4) . . ? C125 C126 C121 119.1(4) . . ? O201 C200 C201 121.1(4) . . ? O201 C200 C205 121.3(4) . . ? C201 C200 C205 117.6(4) . . ? C202 C201 C200 121.9(5) . . ? C202 C201 H201 119.0 . . ? C200 C201 H201 119.0 . . ? C201 C202 C203 120.4(5) . . ? C201 C202 H202 119.8 . . ? C203 C202 H202 119.8 . . ? C204 C203 C202 119.1(5) . . ? C204 C203 H203 120.5 . . ? C202 C203 H203 120.5 . . ? C203 C204 C205 122.0(5) . . ? C203 C204 H204 119.0 . . ? C205 C204 H204 119.0 . . ? C204 C205 C200 118.8(5) . . ? C204 C205 C206 116.6(5) . . ? C200 C205 C206 124.6(5) . . ? N201 C206 C205 126.2(5) . . ? N201 C206 H206 116.9 . . ? C205 C206 H206 116.9 . . ? N201 C207 C208 108.9(4) . . ? N201 C207 H20A 109.9 . . ? C208 C207 H20A 109.9 . . ? N201 C207 H20B 109.9 . . ? C208 C207 H20B 109.9 . . ? H20A C207 H20B 108.3 . . ? N203 C208 C207 112.4(4) . . ? N203 C208 H20C 109.1 . . ? C207 C208 H20C 109.1 . . ? N203 C208 H20D 109.1 . . ? C207 C208 H20D 109.1 . . ? H20C C208 H20D 107.9 . . ? N203 C209 C210 103.7(4) . . ? N203 C209 H20E 111.0 . . ? C210 C209 H20E 111.0 . . ? N203 C209 H20F 111.0 . . ? C210 C209 H20F 111.0 . . ? H20E C209 H20F 109.0 . . ? N204 C210 C209 105.5(4) . . ? N204 C210 H21D 110.6 . . ? C209 C210 H21D 110.6 . . ? N204 C210 H21E 110.6 . . ? C209 C210 H21E 110.6 . . ? H21D C210 H21E 108.8 . . ? N204 C211 C212 112.3(4) . . ? N204 C211 H21F 109.1 . . ? C212 C211 H21F 109.1 . . ? N204 C211 H21G 109.1 . . ? C212 C211 H21G 109.1 . . ? H21F C211 H21G 107.9 . . ? N202 C212 C211 109.5(4) . . ? N202 C212 H21H 109.8 . . ? C211 C212 H21H 109.8 . . ? N202 C212 H21I 109.8 . . ? C211 C212 H21I 109.8 . . ? H21H C212 H21I 108.2 . . ? N202 C213 C214 126.6(5) . . ? N202 C213 H213 116.7 . . ? C214 C213 H213 116.7 . . ? C215 C214 C219 119.1(5) . . ? C215 C214 C213 116.8(4) . . ? C219 C214 C213 124.0(4) . . ? C216 C215 C214 122.7(5) . . ? C216 C215 H215 118.7 . . ? C214 C215 H215 118.7 . . ? C215 C216 C217 118.7(5) . . ? C215 C216 H216 120.7 . . ? C217 C216 H216 120.7 . . ? C216 C217 C218 120.6(5) . . ? C216 C217 H217 119.7 . . ? C218 C217 H217 119.7 . . ? C217 C218 C219 122.4(5) . . ? C217 C218 H218 118.8 . . ? C219 C218 H218 118.8 . . ? O202 C219 C218 120.0(4) . . ? O202 C219 C214 123.4(4) . . ? C218 C219 C214 116.5(4) . . ? N203 C220 N204 101.6(4) . . ? N203 C220 C221 116.1(4) . . ? N204 C220 C221 114.5(4) . . ? N203 C220 H220 108.0 . . ? N204 C220 H220 108.0 . . ? C221 C220 H220 108.0 . . ? C222 C221 C226 120.2(4) . . ? C222 C221 C220 120.4(5) . . ? C226 C221 C220 119.4(4) . . ? C221 C222 C223 121.5(5) . . ? C221 C222 H222 119.2 . . ? C223 C222 H222 119.2 . . ? C222 C223 C224 118.0(5) . . ? C222 C223 H223 121.0 . . ? C224 C223 H223 121.0 . . ? C225 C224 C223 122.1(5) . . ? C225 C224 H224 118.9 . . ? C223 C224 H224 118.9 . . ? C224 C225 C226 120.7(5) . . ? C224 C225 H225 119.7 . . ? C226 C225 H225 119.7 . . ? O203 C226 C225 121.8(5) . . ? O203 C226 C221 120.8(4) . . ? C225 C226 C221 117.4(4) . . ? N1S C10S C11S 177.3(7) . . ? C10S C11S H11J 109.5 . . ? C10S C11S H11K 109.5 . . ? H11J C11S H11K 109.5 . . ? C10S C11S H11L 109.5 . . ? H11J C11S H11L 109.5 . . ? H11K C11S H11L 109.5 . . ? N2S C20S C21S 179.3(10) . . ? C20S C21S H21J 109.5 . . ? C20S C21S H21K 109.5 . . ? H21J C21S H21K 109.5 . . ? C20S C21S H21L 109.5 . . ? H21J C21S H21L 109.5 . . ? H21K C21S H21L 109.5 . . ? C1S O1S H1S 109.5 . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C2S O2S H2S 109.5 . . ? O2S C2S H2S1 109.5 . . ? O2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? O2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? H1W1 O1W H1W2 118(7) . . ? 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 N101 Ni11 Ni13 O31 5.5(2) . . . . ? O101 Ni11 Ni13 O31 28.94(19) . . . . ? O1H Ni11 Ni13 O31 176.4(2) . . . . ? O103 Ni11 Ni13 O31 110.37(16) . . . . ? O11 Ni11 Ni13 O31 -75.85(17) . . . . ? N103 Ni11 Ni13 O31 -146.8(2) . . . . ? N101 Ni11 Ni13 O101 -23.4(2) . . . . ? O1H Ni11 Ni13 O101 147.50(19) . . . . ? O103 Ni11 Ni13 O101 81.43(16) . . . . ? O11 Ni11 Ni13 O101 -104.79(16) . . . . ? N103 Ni11 Ni13 O101 -175.8(2) . . . . ? N101 Ni11 Ni13 O13 81.30(18) . . . . ? O101 Ni11 Ni13 O13 104.69(17) . . . . ? O1H Ni11 Ni13 O13 -107.81(17) . . . . ? O103 Ni11 Ni13 O13 -173.88(13) . . . . ? O11 Ni11 Ni13 O13 -0.09(13) . . . . ? N103 Ni11 Ni13 O13 -71.1(2) . . . . ? N101 Ni11 Ni13 O4W -103.46(18) . . . . ? O101 Ni11 Ni13 O4W -80.07(17) . . . . ? O1H Ni11 Ni13 O4W 67.43(17) . . . . ? O103 Ni11 Ni13 O4W 1.36(13) . . . . ? O11 Ni11 Ni13 O4W 175.14(13) . . . . ? N103 Ni11 Ni13 O4W 104.2(2) . . . . ? N101 Ni11 Ni13 O1H -170.9(2) . . . . ? O101 Ni11 Ni13 O1H -147.50(19) . . . . ? O103 Ni11 Ni13 O1H -66.07(16) . . . . ? O11 Ni11 Ni13 O1H 107.71(16) . . . . ? N103 Ni11 Ni13 O1H 36.7(2) . . . . ? N101 Ni11 Ni13 O3W 160.02(19) . . . . ? O101 Ni11 Ni13 O3W -176.59(19) . . . . ? O1H Ni11 Ni13 O3W -29.09(18) . . . . ? O103 Ni11 Ni13 O3W -95.16(15) . . . . ? O11 Ni11 Ni13 O3W 78.62(15) . . . . ? N103 Ni11 Ni13 O3W 7.7(2) . . . . ? N201 Ni21 Ni23 O33 16.0(2) . . . . ? O201 Ni21 Ni23 O33 32.0(2) . . . . ? O2H Ni21 Ni23 O33 -177.4(2) . . . . ? O203 Ni21 Ni23 O33 116.85(16) . . . . ? O21 Ni21 Ni23 O33 -69.17(17) . . . . ? N203 Ni21 Ni23 O33 -140.2(2) . . . . ? N201 Ni21 Ni23 O201 -16.0(2) . . . . ? O2H Ni21 Ni23 O201 150.6(2) . . . . ? O203 Ni21 Ni23 O201 84.86(17) . . . . ? O21 Ni21 Ni23 O201 -101.16(17) . . . . ? N203 Ni21 Ni23 O201 -172.2(2) . . . . ? N201 Ni21 Ni23 O23 88.12(18) . . . . ? O201 Ni21 Ni23 O23 104.12(17) . . . . ? O2H Ni21 Ni23 O23 -105.31(17) . . . . ? O203 Ni21 Ni23 O23 -171.02(13) . . . . ? O21 Ni21 Ni23 O23 2.96(13) . . . . ? N203 Ni21 Ni23 O23 -68.1(2) . . . . ? N201 Ni21 Ni23 O3W -97.32(18) . . . . ? O201 Ni21 Ni23 O3W -81.32(17) . . . . ? O2H Ni21 Ni23 O3W 69.24(17) . . . . ? O203 Ni21 Ni23 O3W 3.54(13) . . . . ? O21 Ni21 Ni23 O3W 177.52(13) . . . . ? N203 Ni21 Ni23 O3W 106.5(2) . . . . ? N201 Ni21 Ni23 O2H -166.6(2) . . . . ? O201 Ni21 Ni23 O2H -150.6(2) . . . . ? O203 Ni21 Ni23 O2H -65.71(17) . . . . ? O21 Ni21 Ni23 O2H 108.27(17) . . . . ? N203 Ni21 Ni23 O2H 37.2(2) . . . . ? N201 Ni21 Ni23 O4W 166.77(19) . . . . ? O201 Ni21 Ni23 O4W -177.23(18) . . . . ? O2H Ni21 Ni23 O4W -26.66(19) . . . . ? O203 Ni21 Ni23 O4W -92.37(14) . . . . ? O21 Ni21 Ni23 O4W 81.61(15) . . . . ? N203 Ni21 Ni23 O4W 10.6(2) . . . . ? O101 Ni11 N101 C106 12.2(4) . . . . ? O103 Ni11 N101 C106 -78.3(4) . . . . ? O11 Ni11 N101 C106 104.6(4) . . . . ? N103 Ni11 N101 C106 -169.1(4) . . . . ? Ni13 Ni11 N101 C106 28.1(5) . . . . ? O101 Ni11 N101 C107 -173.6(3) . . . . ? O11 Ni11 N101 C107 -81.2(3) . . . . ? N103 Ni11 N101 C107 5.1(3) . . . . ? Ni13 Ni11 N101 C107 -157.7(2) . . . . ? O102 Ni12 N102 C113 20.6(4) . . . . ? O103 Ni12 N102 C113 111.4(4) . . . . ? N104 Ni12 N102 C113 -162.5(4) . . . . ? N1 Ni12 N102 C113 -64.3(4) . . . . ? O102 Ni12 N102 C112 -169.9(3) . . . . ? O103 Ni12 N102 C112 -79.1(4) . . . . ? N104 Ni12 N102 C112 6.9(3) . . . . ? N1 Ni12 N102 C112 105.1(4) . . . . ? N101 Ni11 N103 C120 97.7(3) . . . . ? O1H Ni11 N103 C120 -77.0(3) . . . . ? O103 Ni11 N103 C120 2.8(3) . . . . ? O11 Ni11 N103 C120 -171.2(3) . . . . ? Ni13 Ni11 N103 C120 -102.5(3) . . . . ? N101 Ni11 N103 C108 -26.1(3) . . . . ? O1H Ni11 N103 C108 159.2(3) . . . . ? O103 Ni11 N103 C108 -121.0(3) . . . . ? O11 Ni11 N103 C108 65.0(3) . . . . ? Ni13 Ni11 N103 C108 133.7(3) . . . . ? N101 Ni11 N103 C109 -145.3(3) . . . . ? O1H Ni11 N103 C109 39.9(3) . . . . ? O103 Ni11 N103 C109 119.7(3) . . . . ? O11 Ni11 N103 C109 -54.3(3) . . . . ? Ni13 Ni11 N103 C109 14.4(4) . . . . ? N102 Ni12 N104 C111 18.0(3) . . . . ? O102 Ni12 N104 C111 35.9(9) . . . . ? O103 Ni12 N104 C111 119.1(3) . . . . ? O1H Ni12 N104 C111 -161.1(3) . . . . ? N1 Ni12 N104 C111 -67.8(3) . . . . ? N102 Ni12 N104 C110 139.1(3) . . . . ? O102 Ni12 N104 C110 157.1(7) . . . . ? O103 Ni12 N104 C110 -119.8(3) . . . . ? O1H Ni12 N104 C110 -40.0(3) . . . . ? N1 Ni12 N104 C110 53.3(3) . . . . ? N102 Ni12 N104 C120 -103.9(3) . . . . ? O102 Ni12 N104 C120 -85.9(8) . . . . ? O103 Ni12 N104 C120 -2.8(3) . . . . ? O1H Ni12 N104 C120 77.0(3) . . . . ? N1 Ni12 N104 C120 170.3(3) . . . . ? O201 Ni21 N201 C206 26.9(4) . . . . ? O203 Ni21 N201 C206 -66.4(4) . . . . ? O21 Ni21 N201 C206 117.1(4) . . . . ? N203 Ni21 N201 C206 -156.7(4) . . . . ? Ni23 Ni21 N201 C206 37.7(5) . . . . ? O201 Ni21 N201 C207 -169.9(3) . . . . ? O2H Ni21 N201 C207 136.1(8) . . . . ? O203 Ni21 N201 C207 96.8(3) . . . . ? O21 Ni21 N201 C207 -79.7(3) . . . . ? N203 Ni21 N201 C207 6.5(3) . . . . ? Ni23 Ni21 N201 C207 -159.1(3) . . . . ? O202 Ni22 N202 C213 19.1(4) . . . . ? O203 Ni22 N202 C213 110.2(4) . . . . ? N204 Ni22 N202 C213 -164.8(4) . . . . ? N1 Ni22 N202 C213 -66.4(4) . . . . ? O202 Ni22 N202 C212 -173.0(4) . . . . ? O203 Ni22 N202 C212 -81.9(4) . . . . ? N204 Ni22 N202 C212 3.1(4) . . . . ? N1 Ni22 N202 C212 101.5(4) . . . . ? N201 Ni21 N203 C220 97.4(3) . . . . ? O2H Ni21 N203 C220 -74.4(3) . . . . ? O203 Ni21 N203 C220 5.6(3) . . . . ? O21 Ni21 N203 C220 -169.2(3) . . . . ? Ni23 Ni21 N203 C220 -100.2(3) . . . . ? N201 Ni21 N203 C209 -146.2(3) . . . . ? O2H Ni21 N203 C209 41.9(3) . . . . ? O203 Ni21 N203 C209 122.0(3) . . . . ? O21 Ni21 N203 C209 -52.8(3) . . . . ? Ni23 Ni21 N203 C209 16.2(4) . . . . ? N201 Ni21 N203 C208 -27.1(3) . . . . ? O2H Ni21 N203 C208 161.1(3) . . . . ? O203 Ni21 N203 C208 -118.9(3) . . . . ? O21 Ni21 N203 C208 66.4(3) . . . . ? Ni23 Ni21 N203 C208 135.3(2) . . . . ? N202 Ni22 N204 C211 19.9(3) . . . . ? O2H Ni22 N204 C211 -160.1(3) . . . . ? O203 Ni22 N204 C211 120.1(3) . . . . ? N1 Ni22 N204 C211 -65.5(3) . . . . ? N202 Ni22 N204 C220 -102.4(3) . . . . ? O2H Ni22 N204 C220 77.6(3) . . . . ? O203 Ni22 N204 C220 -2.2(3) . . . . ? N1 Ni22 N204 C220 172.2(3) . . . . ? N202 Ni22 N204 C210 141.1(3) . . . . ? O2H Ni22 N204 C210 -38.8(3) . . . . ? O203 Ni22 N204 C210 -118.7(3) . . . . ? N1 Ni22 N204 C210 55.7(3) . . . . ? N202 Ni22 N1 N2 -33.9(4) . . . . ? O202 Ni22 N1 N2 -124.4(4) . . . . ? O2H Ni22 N1 N2 142.9(4) . . . . ? N204 Ni22 N1 N2 46.5(4) . . . . ? N202 Ni22 N1 Ni12 145.4(3) . . . . ? O202 Ni22 N1 Ni12 54.9(3) . . . . ? O2H Ni22 N1 Ni12 -37.8(3) . . . . ? N204 Ni22 N1 Ni12 -134.2(3) . . . . ? N102 Ni12 N1 N2 -32.1(4) . . . . ? O102 Ni12 N1 N2 -121.8(4) . . . . ? O1H Ni12 N1 N2 145.2(4) . . . . ? N104 Ni12 N1 N2 48.1(4) . . . . ? N102 Ni12 N1 Ni22 148.6(3) . . . . ? O102 Ni12 N1 Ni22 58.9(3) . . . . ? O1H Ni12 N1 Ni22 -34.1(3) . . . . ? N104 Ni12 N1 Ni22 -131.2(3) . . . . ? N101 Ni11 O101 C100 -18.9(4) . . . . ? O1H Ni11 O101 C100 155.8(4) . . . . ? O103 Ni11 O101 C100 76.1(4) . . . . ? O11 Ni11 O101 C100 -109.7(4) . . . . ? Ni13 Ni11 O101 C100 178.2(4) . . . . ? N101 Ni11 O101 Ni13 162.87(15) . . . . ? O1H Ni11 O101 Ni13 -22.41(13) . . . . ? O103 Ni11 O101 Ni13 -102.10(13) . . . . ? O11 Ni11 O101 Ni13 72.14(13) . . . . ? O31 Ni13 O101 C100 22.6(5) . . . . ? O13 Ni13 O101 C100 109.5(5) . . . . ? O4W Ni13 O101 C100 -67.1(5) . . . . ? O1H Ni13 O101 C100 -155.5(5) . . . . ? Ni11 Ni13 O101 C100 -177.8(5) . . . . ? O31 Ni13 O101 Ni11 -159.61(13) . . . . ? O13 Ni13 O101 Ni11 -72.74(14) . . . . ? O4W Ni13 O101 Ni11 110.70(13) . . . . ? O1H Ni13 O101 Ni11 22.28(13) . . . . ? N102 Ni12 O102 C119 -22.8(4) . . . . ? O103 Ni12 O102 C119 -123.4(3) . . . . ? O1H Ni12 O102 C119 156.4(3) . . . . ? N1 Ni12 O102 C119 64.4(4) . . . . ? N102 Ni12 O103 C126 34.6(3) . . . . ? O102 Ni12 O103 C126 124.2(3) . . . . ? O1H Ni12 O103 C126 -142.7(3) . . . . ? N104 Ni12 O103 C126 -45.5(3) . . . . ? N102 Ni12 O103 Ni11 153.83(14) . . . . ? O102 Ni12 O103 Ni11 -116.56(12) . . . . ? O1H Ni12 O103 Ni11 -23.48(12) . . . . ? N104 Ni12 O103 Ni11 73.73(14) . . . . ? N101 Ni11 O103 C126 -34.9(3) . . . . ? O101 Ni11 O103 C126 -126.0(3) . . . . ? O1H Ni11 O103 C126 150.2(3) . . . . ? N103 Ni11 O103 C126 49.2(3) . . . . ? Ni13 Ni11 O103 C126 -168.9(3) . . . . ? N101 Ni11 O103 Ni12 -161.54(14) . . . . ? O101 Ni11 O103 Ni12 107.37(13) . . . . ? O1H Ni11 O103 Ni12 23.54(12) . . . . ? N103 Ni11 O103 Ni12 -77.42(14) . . . . ? Ni13 Ni11 O103 Ni12 64.50(10) . . . . ? N201 Ni21 O201 C200 -32.0(4) . . . . ? O2H Ni21 O201 C200 139.6(4) . . . . ? O203 Ni21 O201 C200 59.8(4) . . . . ? O21 Ni21 O201 C200 -125.0(4) . . . . ? Ni23 Ni21 O201 C200 159.9(4) . . . . ? N201 Ni21 O201 Ni23 168.15(15) . . . . ? O2H Ni21 O201 Ni23 -20.27(13) . . . . ? O203 Ni21 O201 Ni23 -100.01(14) . . . . ? O21 Ni21 O201 Ni23 75.11(14) . . . . ? O33 Ni23 O201 C200 45.6(4) . . . . ? O23 Ni23 O201 C200 131.1(4) . . . . ? O3W Ni23 O201 C200 -47.3(4) . . . . ? O2H Ni23 O201 C200 -136.3(4) . . . . ? Ni21 Ni23 O201 C200 -156.4(5) . . . . ? O33 Ni23 O201 Ni21 -158.03(13) . . . . ? O23 Ni23 O201 Ni21 -72.51(14) . . . . ? O3W Ni23 O201 Ni21 109.09(13) . . . . ? O2H Ni23 O201 Ni21 20.04(13) . . . . ? N202 Ni22 O202 C219 -16.3(4) . . . . ? O2H Ni22 O202 C219 163.9(4) . . . . ? O203 Ni22 O202 C219 -115.8(4) . . . . ? N1 Ni22 O202 C219 70.4(4) . . . . ? N202 Ni22 O203 C226 30.4(3) . . . . ? O202 Ni22 O203 C226 120.9(3) . . . . ? O2H Ni22 O203 C226 -146.3(3) . . . . ? N204 Ni22 O203 C226 -49.8(3) . . . . ? N202 Ni22 O203 Ni21 153.98(14) . . . . ? O202 Ni22 O203 Ni21 -115.61(13) . . . . ? O2H Ni22 O203 Ni21 -22.75(13) . . . . ? N204 Ni22 O203 Ni21 73.79(14) . . . . ? N201 Ni21 O203 C226 -40.5(3) . . . . ? O201 Ni21 O203 C226 -130.6(3) . . . . ? O2H Ni21 O203 C226 146.1(3) . . . . ? N203 Ni21 O203 C226 43.4(3) . . . . ? Ni23 Ni21 O203 C226 -173.5(3) . . . . ? N201 Ni21 O203 Ni22 -163.71(15) . . . . ? O201 Ni21 O203 Ni22 106.25(13) . . . . ? O2H Ni21 O203 Ni22 22.92(13) . . . . ? N203 Ni21 O203 Ni22 -79.77(14) . . . . ? Ni23 Ni21 O203 Ni22 63.35(11) . . . . ? O101 Ni11 O1H Ni12 -114.85(15) . . . . ? O103 Ni11 O1H Ni12 -23.36(12) . . . . ? O11 Ni11 O1H Ni12 153.24(13) . . . . ? N103 Ni11 O1H Ni12 66.00(16) . . . . ? Ni13 Ni11 O1H Ni12 -136.67(19) . . . . ? O101 Ni11 O1H Ni13 21.82(13) . . . . ? O103 Ni11 O1H Ni13 113.31(14) . . . . ? O11 Ni11 O1H Ni13 -70.09(14) . . . . ? N103 Ni11 O1H Ni13 -157.33(14) . . . . ? O102 Ni12 O1H Ni11 113.92(14) . . . . ? O103 Ni12 O1H Ni11 23.57(12) . . . . ? N104 Ni12 O1H Ni11 -63.06(15) . . . . ? N1 Ni12 O1H Ni11 -161.02(14) . . . . ? O102 Ni12 O1H Ni13 17.7(2) . . . . ? O103 Ni12 O1H Ni13 -72.6(2) . . . . ? N104 Ni12 O1H Ni13 -159.3(2) . . . . ? N1 Ni12 O1H Ni13 102.8(2) . . . . ? O101 Ni13 O1H Ni11 -21.58(13) . . . . ? O13 Ni13 O1H Ni11 70.55(14) . . . . ? O4W Ni13 O1H Ni11 -119.73(13) . . . . ? O3W Ni13 O1H Ni11 159.00(13) . . . . ? O101 Ni13 O1H Ni12 76.4(2) . . . . ? O13 Ni13 O1H Ni12 168.5(2) . . . . ? O4W Ni13 O1H Ni12 -21.8(2) . . . . ? O3W Ni13 O1H Ni12 -103.1(2) . . . . ? Ni11 Ni13 O1H Ni12 97.9(3) . . . . ? O201 Ni21 O2H Ni22 -117.44(15) . . . . ? O203 Ni21 O2H Ni22 -23.10(13) . . . . ? O21 Ni21 O2H Ni22 152.89(14) . . . . ? N203 Ni21 O2H Ni22 65.29(16) . . . . ? Ni23 Ni21 O2H Ni22 -137.1(2) . . . . ? N201 Ni21 O2H Ni23 74.2(9) . . . . ? O201 Ni21 O2H Ni23 19.70(13) . . . . ? O203 Ni21 O2H Ni23 114.05(15) . . . . ? O21 Ni21 O2H Ni23 -69.97(14) . . . . ? N203 Ni21 O2H Ni23 -157.56(14) . . . . ? O202 Ni22 O2H Ni21 113.85(15) . . . . ? O203 Ni22 O2H Ni21 23.29(13) . . . . ? N204 Ni22 O2H Ni21 -62.22(16) . . . . ? N1 Ni22 O2H Ni21 -160.38(15) . . . . ? O202 Ni22 O2H Ni23 15.1(3) . . . . ? O203 Ni22 O2H Ni23 -75.5(3) . . . . ? N204 Ni22 O2H Ni23 -161.0(3) . . . . ? N1 Ni22 O2H Ni23 100.8(3) . . . . ? O201 Ni23 O2H Ni21 -19.44(13) . . . . ? O23 Ni23 O2H Ni21 71.68(14) . . . . ? O3W Ni23 O2H Ni21 -117.80(14) . . . . ? O4W Ni23 O2H Ni21 160.38(13) . . . . ? O201 Ni23 O2H Ni22 81.0(3) . . . . ? O23 Ni23 O2H Ni22 172.1(3) . . . . ? O3W Ni23 O2H Ni22 -17.4(3) . . . . ? O4W Ni23 O2H Ni22 -99.2(3) . . . . ? Ni21 Ni23 O2H Ni22 100.4(3) . . . . ? O33 Ni23 O3W Ni13 70.52(13) . . . . ? O201 Ni23 O3W Ni13 168.34(12) . . . . ? O2H Ni23 O3W Ni13 -109.24(14) . . . . ? O4W Ni23 O3W Ni13 -18.27(12) . . . . ? Ni21 Ni23 O3W Ni13 -149.52(7) . . . . ? O31 Ni13 O3W Ni23 -70.32(14) . . . . ? O13 Ni13 O3W Ni23 -156.96(13) . . . . ? O4W Ni13 O3W Ni23 18.63(12) . . . . ? O1H Ni13 O3W Ni23 107.77(13) . . . . ? Ni11 Ni13 O3W Ni23 127.69(9) . . . . ? O31 Ni13 O4W Ni23 72.28(13) . . . . ? O101 Ni13 O4W Ni23 167.02(12) . . . . ? O13 Ni13 O4W Ni23 4.9(7) . . . . ? O1H Ni13 O4W Ni23 -110.15(13) . . . . ? O3W Ni13 O4W Ni23 -18.22(12) . . . . ? Ni11 Ni13 O4W Ni23 -150.46(7) . . . . ? O33 Ni23 O4W Ni13 -73.17(13) . . . . ? O23 Ni23 O4W Ni13 -158.56(13) . . . . ? O3W Ni23 O4W Ni13 18.73(12) . . . . ? O2H Ni23 O4W Ni13 108.74(14) . . . . ? Ni21 Ni23 O4W Ni13 126.82(8) . . . . ? N101 Ni11 O11 C10 -129.3(4) . . . . ? O101 Ni11 O11 C10 -38.2(4) . . . . ? O1H Ni11 O11 C10 45.9(4) . . . . ? N103 Ni11 O11 C10 146.7(4) . . . . ? Ni13 Ni11 O11 C10 3.5(4) . . . . ? O31 Ni13 O13 C10 132.7(4) . . . . ? O101 Ni13 O13 C10 38.0(4) . . . . ? O4W Ni13 O13 C10 -159.7(6) . . . . ? O1H Ni13 O13 C10 -45.2(4) . . . . ? O3W Ni13 O13 C10 -136.9(4) . . . . ? Ni11 Ni13 O13 C10 -3.2(4) . . . . ? O33 Ni23 O23 C20 133.8(4) . . . . ? O201 Ni23 O23 C20 36.4(4) . . . . ? O2H Ni23 O23 C20 -46.1(4) . . . . ? O4W Ni23 O23 C20 -137.0(4) . . . . ? Ni21 Ni23 O23 C20 -4.2(4) . . . . ? N201 Ni21 O21 C20 -135.5(4) . . . . ? O201 Ni21 O21 C20 -45.6(4) . . . . ? O2H Ni21 O21 C20 38.4(4) . . . . ? N203 Ni21 O21 C20 140.7(4) . . . . ? Ni23 Ni21 O21 C20 -3.6(4) . . . . ? O101 Ni13 O31 C30 -129.8(4) . . . . ? O13 Ni13 O31 C30 137.7(4) . . . . ? O4W Ni13 O31 C30 -31.9(4) . . . . ? O3W Ni13 O31 C30 49.4(4) . . . . ? Ni11 Ni13 O31 C30 -149.1(3) . . . . ? O201 Ni23 O33 C30 -147.9(4) . . . . ? O23 Ni23 O33 C30 121.2(4) . . . . ? O3W Ni23 O33 C30 -49.3(4) . . . . ? O4W Ni23 O33 C30 32.5(4) . . . . ? Ni21 Ni23 O33 C30 -168.9(3) . . . . ? Ni11 O11 C10 O13 -7.3(7) . . . . ? Ni11 O11 C10 C11 175.6(3) . . . . ? Ni13 O13 C10 O11 7.1(7) . . . . ? Ni13 O13 C10 C11 -175.8(3) . . . . ? Ni21 O21 C20 O23 1.9(7) . . . . ? Ni21 O21 C20 C21 -175.9(3) . . . . ? Ni23 O23 C20 O21 3.1(7) . . . . ? Ni23 O23 C20 C21 -179.2(3) . . . . ? Ni13 O31 C30 O33 -19.6(7) . . . . ? Ni13 O31 C30 C31 158.8(3) . . . . ? Ni23 O33 C30 O31 18.5(7) . . . . ? Ni23 O33 C30 C31 -159.9(3) . . . . ? Ni11 O101 C100 C101 -163.0(3) . . . . ? Ni13 O101 C100 C101 14.2(7) . . . . ? Ni11 O101 C100 C105 16.5(6) . . . . ? Ni13 O101 C100 C105 -166.3(3) . . . . ? O101 C100 C101 C102 -177.8(5) . . . . ? C105 C100 C101 C102 2.6(7) . . . . ? C100 C101 C102 C103 -0.5(8) . . . . ? C101 C102 C103 C104 -0.4(8) . . . . ? C102 C103 C104 C105 -1.0(8) . . . . ? C103 C104 C105 C100 3.2(8) . . . . ? C103 C104 C105 C106 -178.4(5) . . . . ? O101 C100 C105 C104 176.6(4) . . . . ? C101 C100 C105 C104 -3.9(7) . . . . ? O101 C100 C105 C106 -1.6(7) . . . . ? C101 C100 C105 C106 177.9(4) . . . . ? C107 N101 C106 C105 -177.4(4) . . . . ? Ni11 N101 C106 C105 -3.5(7) . . . . ? C104 C105 C106 N101 176.4(5) . . . . ? C100 C105 C106 N101 -5.4(8) . . . . ? C106 N101 C107 C108 -168.2(4) . . . . ? Ni11 N101 C107 C108 17.2(5) . . . . ? C120 N103 C108 C107 -80.3(5) . . . . ? C109 N103 C108 C107 164.7(4) . . . . ? Ni11 N103 C108 C107 43.7(5) . . . . ? N101 C107 C108 N103 -41.9(5) . . . . ? C120 N103 C109 C110 29.9(5) . . . . ? C108 N103 C109 C110 151.5(4) . . . . ? Ni11 N103 C109 C110 -93.5(4) . . . . ? C111 N104 C110 C109 -146.0(4) . . . . ? C120 N104 C110 C109 -27.5(5) . . . . ? Ni12 N104 C110 C109 96.2(4) . . . . ? N103 C109 C110 N104 -1.2(5) . . . . ? C110 N104 C111 C112 -161.9(4) . . . . ? C120 N104 C111 C112 84.6(5) . . . . ? Ni12 N104 C111 C112 -39.5(4) . . . . ? C113 N102 C112 C111 139.9(4) . . . . ? Ni12 N102 C112 C111 -30.4(5) . . . . ? N104 C111 C112 N102 46.9(5) . . . . ? C112 N102 C113 C114 178.7(5) . . . . ? Ni12 N102 C113 C114 -12.0(7) . . . . ? N102 C113 C114 C115 177.5(5) . . . . ? N102 C113 C114 C119 -4.2(8) . . . . ? C119 C114 C115 C116 -1.7(7) . . . . ? C113 C114 C115 C116 176.7(5) . . . . ? C114 C115 C116 C117 0.6(8) . . . . ? C115 C116 C117 C118 0.2(7) . . . . ? C116 C117 C118 C119 0.2(7) . . . . ? Ni12 O102 C119 C114 15.6(6) . . . . ? Ni12 O102 C119 C118 -165.9(3) . . . . ? C115 C114 C119 O102 -179.5(4) . . . . ? C113 C114 C119 O102 2.3(7) . . . . ? C115 C114 C119 C118 2.0(7) . . . . ? C113 C114 C119 C118 -176.3(4) . . . . ? C117 C118 C119 O102 -179.9(4) . . . . ? C117 C118 C119 C114 -1.2(7) . . . . ? C108 N103 C120 N104 -166.7(4) . . . . ? C109 N103 C120 N104 -47.3(4) . . . . ? Ni11 N103 C120 N104 75.3(4) . . . . ? C108 N103 C120 C121 69.3(5) . . . . ? C109 N103 C120 C121 -171.3(4) . . . . ? Ni11 N103 C120 C121 -48.7(5) . . . . ? C111 N104 C120 N103 165.1(4) . . . . ? C110 N104 C120 N103 46.5(4) . . . . ? Ni12 N104 C120 N103 -76.2(4) . . . . ? C111 N104 C120 C121 -71.5(5) . . . . ? C110 N104 C120 C121 169.9(4) . . . . ? Ni12 N104 C120 C121 47.2(5) . . . . ? N103 C120 C121 C122 -119.4(5) . . . . ? N104 C120 C121 C122 124.6(5) . . . . ? N103 C120 C121 C126 55.8(6) . . . . ? N104 C120 C121 C126 -60.3(6) . . . . ? C126 C121 C122 C123 -3.9(7) . . . . ? C120 C121 C122 C123 171.4(4) . . . . ? C121 C122 C123 C124 0.0(7) . . . . ? C122 C123 C124 C125 2.4(8) . . . . ? C123 C124 C125 C126 -0.9(8) . . . . ? Ni12 O103 C126 C125 -132.9(4) . . . . ? Ni11 O103 C126 C125 116.3(4) . . . . ? Ni12 O103 C126 C121 50.1(5) . . . . ? Ni11 O103 C126 C121 -60.7(5) . . . . ? C124 C125 C126 O103 180.0(4) . . . . ? C124 C125 C126 C121 -3.0(7) . . . . ? C122 C121 C126 O103 -177.6(4) . . . . ? C120 C121 C126 O103 7.2(6) . . . . ? C122 C121 C126 C125 5.3(7) . . . . ? C120 C121 C126 C125 -169.8(4) . . . . ? Ni21 O201 C200 C201 -158.9(4) . . . . ? Ni23 O201 C200 C201 -8.2(7) . . . . ? Ni21 O201 C200 C205 22.7(6) . . . . ? Ni23 O201 C200 C205 173.3(3) . . . . ? O201 C200 C201 C202 176.5(5) . . . . ? C205 C200 C201 C202 -5.0(7) . . . . ? C200 C201 C202 C203 2.2(8) . . . . ? C201 C202 C203 C204 1.2(9) . . . . ? C202 C203 C204 C205 -1.6(9) . . . . ? C203 C204 C205 C200 -1.3(8) . . . . ? C203 C204 C205 C206 179.4(5) . . . . ? O201 C200 C205 C204 -177.0(4) . . . . ? C201 C200 C205 C204 4.5(7) . . . . ? O201 C200 C205 C206 2.2(8) . . . . ? C201 C200 C205 C206 -176.3(5) . . . . ? C207 N201 C206 C205 -176.3(5) . . . . ? Ni21 N201 C206 C205 -13.9(7) . . . . ? C204 C205 C206 N201 172.5(5) . . . . ? C200 C205 C206 N201 -6.8(8) . . . . ? C206 N201 C207 C208 180.0(5) . . . . ? Ni21 N201 C207 C208 16.1(5) . . . . ? C220 N203 C208 C207 -80.3(5) . . . . ? C209 N203 C208 C207 165.1(4) . . . . ? Ni21 N203 C208 C207 44.1(4) . . . . ? N201 C207 C208 N203 -41.4(6) . . . . ? C220 N203 C209 C210 33.2(4) . . . . ? C208 N203 C209 C210 155.2(4) . . . . ? Ni21 N203 C209 C210 -89.9(4) . . . . ? C211 N204 C210 C209 -143.5(4) . . . . ? C220 N204 C210 C209 -23.5(4) . . . . ? Ni22 N204 C210 C209 99.8(4) . . . . ? N203 C209 C210 N204 -5.8(5) . . . . ? C220 N204 C211 C212 84.7(5) . . . . ? C210 N204 C211 C212 -160.7(4) . . . . ? Ni22 N204 C211 C212 -39.3(4) . . . . ? C213 N202 C212 C211 143.5(4) . . . . ? Ni22 N202 C212 C211 -25.4(5) . . . . ? N204 C211 C212 N202 44.2(6) . . . . ? C212 N202 C213 C214 176.8(5) . . . . ? Ni22 N202 C213 C214 -15.3(7) . . . . ? O202 C219 C214 C215 -179.5(4) . . . . ? C218 C219 C214 C215 -0.7(7) . . . . ? O202 C219 C214 C213 3.1(8) . . . . ? C218 C219 C214 C213 -178.1(5) . . . . ? N202 C213 C214 C215 -176.7(5) . . . . ? N202 C213 C214 C219 0.7(8) . . . . ? C219 C214 C215 C216 -0.1(7) . . . . ? C213 C214 C215 C216 177.5(5) . . . . ? C214 C215 C216 C217 -0.4(8) . . . . ? C215 C216 C217 C218 1.6(8) . . . . ? C216 C217 C218 C219 -2.5(8) . . . . ? O202 C219 C218 C217 -179.1(5) . . . . ? C214 C219 C218 C217 2.0(7) . . . . ? Ni22 O202 C219 C218 -170.2(3) . . . . ? Ni22 O202 C219 C214 8.6(7) . . . . ? C209 N203 C220 N204 -48.7(4) . . . . ? C208 N203 C220 N204 -168.0(4) . . . . ? Ni21 N203 C220 N204 73.8(4) . . . . ? C209 N203 C220 C221 -173.7(4) . . . . ? C208 N203 C220 C221 67.0(5) . . . . ? Ni21 N203 C220 C221 -51.2(5) . . . . ? C211 N204 C220 N203 164.9(4) . . . . ? C210 N204 C220 N203 44.7(4) . . . . ? Ni22 N204 C220 N203 -77.0(4) . . . . ? C211 N204 C220 C221 -69.1(5) . . . . ? C210 N204 C220 C221 170.7(4) . . . . ? Ni22 N204 C220 C221 49.0(5) . . . . ? N203 C220 C221 C222 -122.2(5) . . . . ? N204 C220 C221 C222 119.7(5) . . . . ? N203 C220 C221 C226 59.5(6) . . . . ? N204 C220 C221 C226 -58.6(6) . . . . ? C226 C221 C222 C223 0.4(8) . . . . ? C220 C221 C222 C223 -177.9(5) . . . . ? C221 C222 C223 C224 0.3(8) . . . . ? C222 C223 C224 C225 -1.4(9) . . . . ? C223 C224 C225 C226 1.9(9) . . . . ? Ni22 O203 C226 C225 -119.7(5) . . . . ? Ni21 O203 C226 C225 129.5(4) . . . . ? Ni22 O203 C226 C221 59.9(5) . . . . ? Ni21 O203 C226 C221 -50.9(5) . . . . ? C224 C225 C226 O203 178.5(5) . . . . ? C224 C225 C226 C221 -1.1(8) . . . . ? C222 C221 C226 O203 -179.6(5) . . . . ? C220 C221 C226 O203 -1.3(7) . . . . ? C222 C221 C226 C225 0.0(7) . . . . ? C220 C221 C226 C225 178.3(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3W H3W1 O1S 0.80 2.12 2.840(5) 150 2_454 O3W H3W2 O202 0.86 1.65 2.504(4) 169 . O4W H4W1 O1W 0.82 1.91 2.697(5) 161 1_565 O4W H4W2 O102 0.83 1.72 2.511(4) 157 . O1H H1H O202 0.98(5) 2.54(5) 3.242(5) 129(4) . O2H H2H O102 0.81(6) 2.75(6) 3.345(5) 132(5) . O1S H1S O13 0.84 1.87 2.669(5) 159 2_444 O2S H2S N1S 0.84 2.20 2.971(10) 153 . O1W H1W1 O23 0.71(7) 2.16(7) 2.746(6) 141(8) 1_545 O1W H1W2 N2S 1.04(5) 1.82(5) 2.849(8) 167(4) 2_444 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.386 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.089 #END