Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_ifn232m _database_code_CSD 172114 _database_code_CSD 172114 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Adams, Harry' 'Clunas, Scott' 'Fenton, David E.' _publ_contact_author_name 'Prof David E Fenton' _publ_contact_author_address ; Prof David E Fenton Department of Chemistry The University of Sheffield Sheffield S3 7HF UK ; _publ_contact_author_email 'D.FENTON@SHEFFIELD.AC.UK' _publ_section_title ; A Tetranuclear nickel(II) complex assembled from an asymmetric compartmental ligand and bearing an intramolecular [H3O2]- bridge ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H83 Cl F12 N8 Ni4 O16 P2' _chemical_formula_weight 1540.41 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 11.337(6) _cell_length_b 22.608(11) _cell_length_c 11.892(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.706(9) _cell_angle_gamma 90.00 _cell_volume 3048(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 1.419 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.6594 _exptl_absorpt_correction_T_max 0.7644 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12274 _diffrn_reflns_av_R_equivalents 0.1430 _diffrn_reflns_av_sigmaI/netI 0.2023 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4109 _reflns_number_gt 1700 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0941P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4109 _refine_ls_number_parameters 403 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1799 _refine_ls_R_factor_gt 0.0787 _refine_ls_wR_factor_ref 0.2138 _refine_ls_wR_factor_gt 0.1794 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.940 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.67953(12) -0.18549(7) 0.24012(13) 0.0304(5) Uani 1 1 d . . . Ni2 Ni 0.35478(13) -0.18667(7) 0.19111(14) 0.0351(5) Uani 1 1 d . . . P1 P 0.0913(4) -0.0871(2) 0.7988(4) 0.0582(13) Uani 1 1 d . . . Cl1 Cl 0.5428(4) -0.2500 0.0311(4) 0.0510(15) Uani 1 2 d S . . O1 O 0.5160(7) -0.1467(3) 0.2171(7) 0.033(2) Uani 1 1 d . . . O2 O 0.6415(9) -0.2500 0.1228(8) 0.027(3) Uiso 1 2 d S . . O3 O 0.4186(10) -0.2500 0.0832(9) 0.031(3) Uiso 1 2 d S . . O4 O 0.5558(7) -0.1939(4) -0.0452(7) 0.046(2) Uiso 1 1 d . . . O5 O 0.8088(8) -0.2500 0.2671(7) 0.009(2) Uiso 1 2 d S . . H5A H 0.8369 -0.2500 0.3336 0.011 Uiso 1 2 d SR . . O6 O 0.2077(9) -0.2500 0.1662(9) 0.035(3) Uani 1 2 d S . . H6A H 0.1776 -0.2500 0.1004 0.042 Uiso 1 2 d SR . . O7 O 0.5981(10) -0.2500 0.3460(9) 0.038(3) Uiso 1 2 d S . . H1SA H 0.5234 -0.2500 0.3410 0.045 Uiso 1 2 d SR . . H1SB H 0.6238 -0.2500 0.4116 0.045 Uiso 1 2 d SR . . O8 O 0.3852(8) -0.2500 0.3070(7) 0.013(2) Uiso 1 2 d S . . H2SA H 0.3551 -0.2500 0.3589 0.015 Uiso 1 2 d SR . . N1 N 0.7281(10) -0.1247(5) 0.3651(9) 0.036(3) Uani 1 1 d . . . N2 N 0.7914(9) -0.1349(4) 0.1357(9) 0.039(3) Uani 1 1 d . . . N3 N 0.2967(8) -0.1237(4) 0.0755(9) 0.034(3) Uani 1 1 d . . . H3 H 0.2723 -0.1427 0.0099 0.041 Uiso 1 1 calc R . . N4 N 0.2676(8) -0.1348(5) 0.2997(10) 0.034(3) Uani 1 1 d . . . C1 C 0.4755(12) 0.1017(5) 0.2771(12) 0.056(4) Uani 1 1 d . . . H1A H 0.5120 0.1127 0.3493 0.084 Uiso 1 1 calc R . . H1B H 0.3933 0.1151 0.2752 0.084 Uiso 1 1 calc R . . H1C H 0.5188 0.1205 0.2158 0.084 Uiso 1 1 calc R . . C2 C 0.4794(12) 0.0352(6) 0.2632(13) 0.042(4) Uani 1 1 d . . . C3 C 0.5400(10) 0.0005(6) 0.3410(11) 0.042(4) Uani 1 1 d . . . H3A H 0.5736 0.0188 0.4058 0.051 Uiso 1 1 calc R . . C4 C 0.5528(11) -0.0603(6) 0.3267(12) 0.034(3) Uani 1 1 d . . . C5 C 0.5044(11) -0.0880(6) 0.2329(12) 0.032(3) Uani 1 1 d . . . C6 C 0.4443(11) -0.0524(7) 0.1530(13) 0.040(4) Uani 1 1 d . . . C7 C 0.4341(11) 0.0070(7) 0.1681(12) 0.044(4) Uani 1 1 d . . . H7 H 0.3950 0.0300 0.1121 0.053 Uiso 1 1 calc R . . C8 C 0.6218(11) -0.0961(6) 0.4127(10) 0.039(4) Uani 1 1 d . . . H8A H 0.6464 -0.0698 0.4754 0.047 Uiso 1 1 calc R . . H8B H 0.5698 -0.1270 0.4440 0.047 Uiso 1 1 calc R . . C9 C 0.7932(14) -0.1589(7) 0.4604(13) 0.047(5) Uani 1 1 d . . . H9A H 0.7377 -0.1881 0.4919 0.057 Uiso 1 1 calc R . . H9B H 0.8590 -0.1812 0.4267 0.057 Uiso 1 1 calc R . . C10 C 0.8425(13) -0.1222(6) 0.5565(12) 0.065(5) Uani 1 1 d . . . H10A H 0.8817 -0.1482 0.6112 0.097 Uiso 1 1 calc R . . H10B H 0.7781 -0.1009 0.5930 0.097 Uiso 1 1 calc R . . H10C H 0.8996 -0.0937 0.5273 0.097 Uiso 1 1 calc R . . C11 C 0.8090(11) -0.0797(6) 0.3135(12) 0.048(4) Uani 1 1 d . . . H11A H 0.8651 -0.0647 0.3712 0.058 Uiso 1 1 calc R . . H11B H 0.7623 -0.0459 0.2844 0.058 Uiso 1 1 calc R . . C12 C 0.8759(11) -0.1081(6) 0.2187(13) 0.049(4) Uani 1 1 d . . . H12A H 0.928(11) -0.077(5) 0.178(10) 0.059 Uiso 1 1 d . . . H12B H 0.760(17) -0.136(9) 0.423(15) 0.059 Uiso 1 1 d . . . C13 C 0.8621(11) -0.1720(6) 0.0588(11) 0.048(4) Uani 1 1 d . . . H13A H 0.9024 -0.2031 0.1021 0.072 Uiso 1 1 calc R . . H13B H 0.9208 -0.1473 0.0214 0.072 Uiso 1 1 calc R . . H13C H 0.8100 -0.1901 0.0023 0.072 Uiso 1 1 calc R . . C14 C 0.7325(11) -0.0890(6) 0.0689(11) 0.053(4) Uani 1 1 d . . . H14A H 0.6858 -0.0638 0.1184 0.079 Uiso 1 1 calc R . . H14B H 0.6804 -0.1076 0.0128 0.079 Uiso 1 1 calc R . . H14C H 0.7918 -0.0650 0.0307 0.079 Uiso 1 1 calc R . . C15 C 0.3926(10) -0.0821(6) 0.0486(11) 0.042(4) Uani 1 1 d . . . H15A H 0.3618 -0.0513 -0.0032 0.050 Uiso 1 1 calc R . . H15B H 0.4559 -0.1037 0.0094 0.050 Uiso 1 1 calc R . . C16 C 0.1930(11) -0.0934(6) 0.1266(12) 0.043(4) Uani 1 1 d . . . H16A H 0.1868 -0.0527 0.0963 0.052 Uiso 1 1 calc R . . H16B H 0.1200 -0.1149 0.1055 0.052 Uiso 1 1 calc R . . C17 C 0.2041(10) -0.0908(6) 0.2502(13) 0.038(4) Uani 1 1 d . . . C18 C 0.1492(12) -0.0479(6) 0.3148(15) 0.052(4) Uani 1 1 d . . . H18 H 0.1057 -0.0170 0.2797 0.062 Uiso 1 1 calc R . . C19 C 0.1589(14) -0.0506(7) 0.4337(16) 0.063(5) Uani 1 1 d . . . H19 H 0.1223 -0.0218 0.4797 0.075 Uiso 1 1 calc R . . C20 C 0.2241(13) -0.0972(7) 0.4812(13) 0.054(4) Uani 1 1 d . . . H20 H 0.2322 -0.1013 0.5605 0.065 Uiso 1 1 calc R . . C21 C 0.2759(11) -0.1369(6) 0.4095(14) 0.044(4) Uani 1 1 d . . . H21 H 0.3210 -0.1680 0.4420 0.053 Uiso 1 1 calc R . . F1 F 0.0812(17) -0.0406(6) 0.8832(11) 0.194(7) Uani 1 1 d . . . F2 F 0.2209(11) -0.0868(6) 0.7935(12) 0.165(5) Uani 1 1 d . . . F3 F 0.0713(8) -0.0499(4) 0.6960(8) 0.084(3) Uani 1 1 d . . . F4 F -0.0434(16) -0.0938(9) 0.8122(14) 0.227(8) Uani 1 1 d . . . F5 F 0.0852(14) -0.1449(7) 0.7220(14) 0.192(6) Uani 1 1 d . . . F6 F 0.0989(14) -0.1334(7) 0.8918(14) 0.188(6) Uani 1 1 d . . . O1W O 0.5546(15) -0.2500 0.5685(12) 0.091(5) Uani 1 2 d S . . O2W O 0.326(2) -0.2016(11) -0.166(2) 0.118(9) Uani 0.50 1 d P . . O3W O 0.139(2) -0.2500 -0.0498(15) 0.177(10) Uani 1 2 d S . . O4W O 1.324(4) -0.2500 0.639(2) 0.304(19) Uani 1 2 d S . . C1S C 1.063(4) -0.2500 0.4304(14) 0.17(2) Uiso 0.719(19) 2 d SPD A 1 H1S1 H 1.0395 -0.2119 0.4628 0.255 Uiso 0.360(9) 1 d PR A 1 H1S2 H 1.1475 -0.2561 0.4425 0.255 Uiso 0.360(9) 1 d PR A 1 H1S3 H 1.0188 -0.2819 0.4667 0.255 Uiso 0.360(9) 1 d PR A 1 O1S O 1.0367(11) -0.2500 0.3107(11) 0.015(5) Uiso 0.719(19) 2 d SPD A 1 H1S H 1.0454 -0.2158 0.2846 0.018 Uiso 0.360(9) 1 d PR A 1 C1S' C 1.017(12) -0.2500 0.664(8) 0.6(2) Uiso 0.281(19) 2 d SPD A 2 H1S4 H 0.9589 -0.2180 0.6590 0.871 Uiso 0.140(9) 1 d PR A 2 H1S5 H 1.0676 -0.2440 0.7305 0.871 Uiso 0.140(9) 1 d PR A 2 H1S6 H 0.9760 -0.2880 0.6702 0.871 Uiso 0.140(9) 1 d PR A 2 O2S O 1.082(4) -0.2500 0.560(4) 0.052(16) Uiso 0.281(19) 2 d SPD A 2 H2S H 1.0964 -0.2421 0.4922 0.062 Uiso 0.140(9) 1 d PR A 2 C2S C 0.678(2) -0.2500 0.759(2) 0.093(9) Uiso 1 2 d S . . H2S1 H 0.6404 -0.2340 0.8268 0.140 Uiso 0.50 1 d PR . . H2S2 H 0.6503 -0.2906 0.7466 0.140 Uiso 0.50 1 d PR . . H2S3 H 0.6567 -0.2254 0.6943 0.140 Uiso 0.50 1 d PR . . O3S O 0.793(3) -0.2500 0.774(3) 0.279(17) Uiso 1 2 d S . . H3S H 0.8190 -0.2159 0.7614 0.334 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0104(9) 0.0334(11) 0.0475(11) 0.0016(9) -0.0016(8) -0.0007(8) Ni2 0.0103(9) 0.0361(11) 0.0589(13) 0.0012(10) 0.0002(8) 0.0013(8) P1 0.050(3) 0.067(4) 0.058(3) 0.008(3) -0.006(2) -0.004(2) Cl1 0.027(3) 0.061(4) 0.065(4) 0.000 -0.001(3) 0.000 O1 0.021(5) 0.021(5) 0.056(6) 0.006(5) -0.004(4) -0.004(4) O6 0.022(7) 0.046(8) 0.037(8) 0.000 -0.016(6) 0.000 N1 0.019(7) 0.047(8) 0.042(9) 0.014(7) -0.007(6) 0.007(6) N2 0.035(8) 0.035(7) 0.048(8) 0.010(6) -0.003(6) -0.003(6) N3 0.013(6) 0.032(7) 0.057(8) -0.012(6) -0.003(6) 0.001(5) N4 0.012(6) 0.043(8) 0.048(8) 0.008(6) 0.004(6) -0.009(5) C1 0.048(10) 0.042(10) 0.078(11) 0.015(9) 0.003(8) 0.010(8) C2 0.022(8) 0.039(10) 0.063(11) 0.022(9) 0.008(8) 0.013(7) C3 0.013(8) 0.059(11) 0.055(10) 0.005(9) 0.002(7) 0.002(7) C4 0.020(8) 0.031(9) 0.052(10) 0.013(8) -0.001(7) -0.008(7) C5 0.018(8) 0.034(9) 0.043(9) -0.003(8) 0.008(7) -0.002(7) C6 0.013(8) 0.042(10) 0.065(11) 0.001(9) 0.009(8) -0.012(7) C7 0.024(9) 0.064(12) 0.046(10) 0.013(9) 0.005(7) 0.008(8) C8 0.030(9) 0.041(9) 0.046(9) -0.018(7) -0.017(7) 0.014(7) C9 0.035(11) 0.049(12) 0.057(12) 0.000(9) -0.015(8) 0.009(8) C10 0.056(12) 0.074(12) 0.064(11) -0.015(9) -0.017(9) -0.007(9) C11 0.016(8) 0.045(10) 0.083(12) 0.002(9) -0.012(8) -0.019(7) C12 0.012(8) 0.054(11) 0.081(12) 0.003(9) 0.008(8) -0.023(7) C13 0.023(8) 0.058(10) 0.064(10) 0.005(8) 0.017(7) -0.005(7) C14 0.021(8) 0.087(12) 0.050(10) 0.035(9) 0.000(7) 0.002(8) C15 0.011(8) 0.066(10) 0.048(9) 0.028(8) -0.003(7) -0.011(7) C16 0.019(8) 0.052(10) 0.058(11) 0.005(8) -0.007(7) 0.012(7) C17 0.002(7) 0.042(10) 0.069(12) 0.005(9) 0.000(7) 0.008(7) C18 0.029(9) 0.027(10) 0.099(14) 0.013(10) -0.002(9) 0.000(7) C19 0.058(12) 0.046(12) 0.084(15) -0.015(10) 0.017(10) -0.005(9) C20 0.059(12) 0.051(11) 0.053(11) -0.006(9) 0.005(9) -0.014(9) C21 0.028(9) 0.050(10) 0.056(11) -0.004(9) 0.009(8) 0.002(7) F1 0.33(2) 0.127(12) 0.126(11) -0.036(9) -0.042(13) 0.004(12) F2 0.067(9) 0.212(14) 0.216(14) 0.043(12) -0.041(9) -0.034(9) F3 0.073(7) 0.087(7) 0.093(7) 0.012(6) -0.009(6) 0.014(5) F4 0.161(17) 0.32(2) 0.203(16) 0.025(16) 0.008(14) -0.038(17) F5 0.185(16) 0.166(14) 0.221(17) -0.010(13) -0.085(13) 0.015(11) F6 0.168(16) 0.173(14) 0.225(17) 0.051(13) 0.049(13) 0.013(11) O1W 0.106(15) 0.097(12) 0.070(11) 0.000 0.017(10) 0.000 O2W 0.07(2) 0.15(2) 0.13(2) 0.046(18) 0.013(16) 0.010(16) O3W 0.14(2) 0.32(3) 0.069(14) 0.000 -0.011(13) 0.000 O4W 0.32(5) 0.41(5) 0.18(3) 0.000 -0.06(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O2 2.060(7) . ? Ni1 O1 2.066(8) . ? Ni1 O5 2.089(7) . ? Ni1 N1 2.093(12) . ? Ni1 N2 2.120(10) . ? Ni1 O7 2.144(8) . ? Ni1 Ni1 2.917(3) 4 ? Ni1 Ni2 3.720(3) . ? Ni2 N4 2.013(11) . ? Ni2 O8 2.014(6) . ? Ni2 O1 2.058(8) . ? Ni2 O3 2.060(8) . ? Ni2 N3 2.080(10) . ? Ni2 O6 2.215(8) . ? Ni2 Ni2 2.864(3) 4 ? P1 F1 1.459(13) . ? P1 F2 1.471(12) . ? P1 F3 1.500(9) . ? P1 F6 1.524(15) . ? P1 F4 1.545(17) . ? P1 F5 1.595(15) . ? Cl1 O3 1.546(11) . ? Cl1 O2 1.552(11) . ? Cl1 O4 1.567(8) 4 ? Cl1 O4 1.567(8) . ? O1 C5 1.348(13) . ? O2 Ni1 2.060(7) 4 ? O2 O3 2.565(16) . ? O3 Ni2 2.060(8) 4 ? O5 Ni1 2.089(7) 4 ? O6 Ni2 2.215(8) 4 ? O6 O3W 2.67(2) . ? O7 Ni1 2.144(8) 4 ? O7 O8 2.452(15) . ? O7 O1W 2.697(18) . ? O8 Ni2 2.014(6) 4 ? N1 C8 1.487(16) . ? N1 C11 1.504(16) . ? N1 C9 1.551(15) . ? N2 C14 1.463(14) . ? N2 C13 1.483(14) . ? N2 C12 1.495(16) . ? N3 C15 1.476(13) . ? N3 C16 1.496(14) . ? N4 C21 1.309(15) . ? N4 C17 1.358(15) . ? C1 C2 1.515(17) . ? C2 C7 1.390(17) . ? C2 C3 1.388(16) . ? C3 C4 1.393(16) . ? C4 C5 1.387(16) . ? C4 C8 1.514(16) . ? C5 C6 1.413(17) . ? C6 C7 1.362(17) . ? C6 C15 1.521(17) . ? C9 C10 1.513(19) . ? C11 C12 1.510(18) . ? C16 C17 1.475(17) . ? C17 C18 1.389(17) . ? C18 C19 1.418(19) . ? C19 C20 1.402(19) . ? C20 C21 1.374(17) . ? C1S O1S 1.450(2) . ? C1S' O2S 1.450(2) . ? C2S O3S 1.31(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ni1 O1 91.7(3) . . ? O2 Ni1 O5 75.6(3) . . ? O1 Ni1 O5 160.6(3) . . ? O2 Ni1 N1 175.4(4) . . ? O1 Ni1 N1 92.5(4) . . ? O5 Ni1 N1 99.9(4) . . ? O2 Ni1 N2 96.1(4) . . ? O1 Ni1 N2 103.6(4) . . ? O5 Ni1 N2 92.5(4) . . ? N1 Ni1 N2 84.7(4) . . ? O2 Ni1 O7 80.1(3) . . ? O1 Ni1 O7 88.5(3) . . ? O5 Ni1 O7 75.0(3) . . ? N1 Ni1 O7 98.1(4) . . ? N2 Ni1 O7 167.4(4) . . ? O2 Ni1 Ni1 44.9(2) . 4 ? O1 Ni1 Ni1 115.1(2) . 4 ? O5 Ni1 Ni1 45.73(17) . 4 ? N1 Ni1 Ni1 131.1(3) . 4 ? N2 Ni1 Ni1 122.6(3) . 4 ? O7 Ni1 Ni1 47.1(2) . 4 ? O2 Ni1 Ni2 72.0(3) . . ? O1 Ni1 Ni2 25.5(2) . . ? O5 Ni1 Ni2 135.23(18) . . ? N1 Ni1 Ni2 111.5(3) . . ? N2 Ni1 Ni2 120.7(3) . . ? O7 Ni1 Ni2 69.8(3) . . ? Ni1 Ni1 Ni2 89.59(4) 4 . ? N4 Ni2 O8 93.2(4) . . ? N4 Ni2 O1 95.2(4) . . ? O8 Ni2 O1 93.7(3) . . ? N4 Ni2 O3 169.6(4) . . ? O8 Ni2 O3 82.7(3) . . ? O1 Ni2 O3 94.6(4) . . ? N4 Ni2 N3 82.6(4) . . ? O8 Ni2 N3 171.4(4) . . ? O1 Ni2 N3 94.1(3) . . ? O3 Ni2 N3 100.1(4) . . ? N4 Ni2 O6 95.0(4) . . ? O8 Ni2 O6 75.8(3) . . ? O1 Ni2 O6 165.8(3) . . ? O3 Ni2 O6 74.7(4) . . ? N3 Ni2 O6 97.0(3) . . ? N4 Ni2 Ni2 125.6(3) . 4 ? O8 Ni2 Ni2 44.68(18) . 4 ? O1 Ni2 Ni2 116.0(2) . 4 ? O3 Ni2 Ni2 46.0(2) . 4 ? N3 Ni2 Ni2 133.2(3) . 4 ? O6 Ni2 Ni2 49.73(18) . 4 ? N4 Ni2 Ni1 112.8(3) . . ? O8 Ni2 Ni1 74.8(3) . . ? O1 Ni2 Ni1 25.6(2) . . ? O3 Ni2 Ni1 75.4(3) . . ? N3 Ni2 Ni1 113.8(3) . . ? O6 Ni2 Ni1 140.13(19) . . ? Ni2 Ni2 Ni1 90.41(4) 4 . ? F1 P1 F2 96.6(9) . . ? F1 P1 F3 98.3(7) . . ? F2 P1 F3 96.0(7) . . ? F1 P1 F6 90.0(8) . . ? F2 P1 F6 89.2(8) . . ? F3 P1 F6 169.7(8) . . ? F1 P1 F4 85.0(10) . . ? F2 P1 F4 173.6(10) . . ? F3 P1 F4 89.9(8) . . ? F6 P1 F4 84.5(8) . . ? F1 P1 F5 168.8(10) . . ? F2 P1 F5 90.9(9) . . ? F3 P1 F5 89.3(7) . . ? F6 P1 F5 81.7(8) . . ? F4 P1 F5 86.7(9) . . ? O3 Cl1 O2 111.8(6) . . ? O3 Cl1 O4 109.0(4) . 4 ? O2 Cl1 O4 109.5(4) . 4 ? O3 Cl1 O4 109.0(4) . . ? O2 Cl1 O4 109.5(4) . . ? O4 Cl1 O4 108.0(6) 4 . ? C5 O1 Ni2 111.5(7) . . ? C5 O1 Ni1 119.2(7) . . ? Ni2 O1 Ni1 128.8(4) . . ? Cl1 O2 Ni1 128.2(4) . . ? Cl1 O2 Ni1 128.2(4) . 4 ? Ni1 O2 Ni1 90.1(4) . 4 ? Cl1 O2 O3 34.0(4) . . ? Ni1 O2 O3 108.8(4) . . ? Ni1 O2 O3 108.8(4) 4 . ? Cl1 O3 Ni2 125.3(4) . 4 ? Cl1 O3 Ni2 125.3(4) . . ? Ni2 O3 Ni2 88.1(4) 4 . ? Cl1 O3 O2 34.2(4) . . ? Ni2 O3 O2 103.8(4) 4 . ? Ni2 O3 O2 103.8(4) . . ? Ni1 O5 Ni1 88.5(3) 4 . ? Ni2 O6 Ni2 80.5(4) . 4 ? Ni2 O6 O3W 109.7(5) . . ? Ni2 O6 O3W 109.7(5) 4 . ? Ni1 O7 Ni1 85.7(4) 4 . ? Ni1 O7 O8 108.6(4) 4 . ? Ni1 O7 O8 108.6(4) . . ? Ni1 O7 O1W 131.4(3) 4 . ? Ni1 O7 O1W 131.4(3) . . ? O8 O7 O1W 89.7(5) . . ? Ni2 O8 Ni2 90.6(4) 4 . ? Ni2 O8 O7 106.8(4) 4 . ? Ni2 O8 O7 106.8(4) . . ? C8 N1 C11 111.3(11) . . ? C8 N1 C9 108.5(10) . . ? C11 N1 C9 110.4(10) . . ? C8 N1 Ni1 110.4(8) . . ? C11 N1 Ni1 108.1(8) . . ? C9 N1 Ni1 108.1(7) . . ? C14 N2 C13 108.2(10) . . ? C14 N2 C12 110.9(10) . . ? C13 N2 C12 106.8(10) . . ? C14 N2 Ni1 115.4(8) . . ? C13 N2 Ni1 112.8(7) . . ? C12 N2 Ni1 102.4(8) . . ? C15 N3 C16 112.4(10) . . ? C15 N3 Ni2 110.6(7) . . ? C16 N3 Ni2 106.8(8) . . ? C21 N4 C17 119.3(12) . . ? C21 N4 Ni2 126.1(10) . . ? C17 N4 Ni2 114.2(10) . . ? C7 C2 C3 117.3(13) . . ? C7 C2 C1 122.2(13) . . ? C3 C2 C1 120.2(14) . . ? C4 C3 C2 121.8(14) . . ? C3 C4 C5 120.2(13) . . ? C3 C4 C8 119.9(13) . . ? C5 C4 C8 119.9(12) . . ? O1 C5 C4 121.2(13) . . ? O1 C5 C6 120.9(13) . . ? C4 C5 C6 117.9(12) . . ? C7 C6 C5 120.9(14) . . ? C7 C6 C15 120.7(14) . . ? C5 C6 C15 118.4(13) . . ? C6 C7 C2 121.9(14) . . ? N1 C8 C4 112.9(11) . . ? C10 C9 N1 116.5(12) . . ? N1 C11 C12 109.3(11) . . ? N2 C12 C11 110.0(11) . . ? N3 C15 C6 112.4(10) . . ? C17 C16 N3 111.4(11) . . ? N4 C17 C18 120.7(14) . . ? N4 C17 C16 116.2(12) . . ? C18 C17 C16 123.0(13) . . ? C17 C18 C19 119.4(14) . . ? C20 C19 C18 117.9(14) . . ? C21 C20 C19 117.9(15) . . ? N4 C21 C20 124.8(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Ni1 Ni2 N4 171.5(4) . . . . ? O1 Ni1 Ni2 N4 -49.3(6) . . . . ? O5 Ni1 Ni2 N4 126.0(5) . . . . ? N1 Ni1 Ni2 N4 -5.3(5) . . . . ? N2 Ni1 Ni2 N4 -102.1(5) . . . . ? O7 Ni1 Ni2 N4 85.7(4) . . . . ? Ni1 Ni1 Ni2 N4 129.4(3) 4 . . . ? O2 Ni1 Ni2 O8 84.5(3) . . . . ? O1 Ni1 Ni2 O8 -136.4(6) . . . . ? O5 Ni1 Ni2 O8 39.0(4) . . . . ? N1 Ni1 Ni2 O8 -92.3(4) . . . . ? N2 Ni1 Ni2 O8 170.9(4) . . . . ? O7 Ni1 Ni2 O8 -1.4(3) . . . . ? Ni1 Ni1 Ni2 O8 42.4(2) 4 . . . ? O2 Ni1 Ni2 O1 -139.1(6) . . . . ? O5 Ni1 Ni2 O1 175.4(6) . . . . ? N1 Ni1 Ni2 O1 44.1(6) . . . . ? N2 Ni1 Ni2 O1 -52.7(6) . . . . ? O7 Ni1 Ni2 O1 135.0(6) . . . . ? Ni1 Ni1 Ni2 O1 178.8(5) 4 . . . ? O2 Ni1 Ni2 O3 -1.8(3) . . . . ? O1 Ni1 Ni2 O3 137.3(6) . . . . ? O5 Ni1 Ni2 O3 -47.3(4) . . . . ? N1 Ni1 Ni2 O3 -178.6(4) . . . . ? N2 Ni1 Ni2 O3 84.6(4) . . . . ? O7 Ni1 Ni2 O3 -87.7(3) . . . . ? Ni1 Ni1 Ni2 O3 -43.9(2) 4 . . . ? O2 Ni1 Ni2 N3 -96.6(4) . . . . ? O1 Ni1 Ni2 N3 42.5(6) . . . . ? O5 Ni1 Ni2 N3 -142.1(5) . . . . ? N1 Ni1 Ni2 N3 86.6(4) . . . . ? N2 Ni1 Ni2 N3 -10.2(5) . . . . ? O7 Ni1 Ni2 N3 177.6(4) . . . . ? Ni1 Ni1 Ni2 N3 -138.7(3) 4 . . . ? O2 Ni1 Ni2 O6 40.8(5) . . . . ? O1 Ni1 Ni2 O6 180.0(7) . . . . ? O5 Ni1 Ni2 O6 -4.7(5) . . . . ? N1 Ni1 Ni2 O6 -136.0(6) . . . . ? N2 Ni1 Ni2 O6 127.2(6) . . . . ? O7 Ni1 Ni2 O6 -45.0(5) . . . . ? Ni1 Ni1 Ni2 O6 -1.3(4) 4 . . . ? O2 Ni1 Ni2 Ni2 42.1(2) . . . 4 ? O1 Ni1 Ni2 Ni2 -178.8(5) . . . 4 ? O5 Ni1 Ni2 Ni2 -3.4(3) . . . 4 ? N1 Ni1 Ni2 Ni2 -134.7(3) . . . 4 ? N2 Ni1 Ni2 Ni2 128.5(3) . . . 4 ? O7 Ni1 Ni2 Ni2 -43.8(2) . . . 4 ? Ni1 Ni1 Ni2 Ni2 0.0 4 . . 4 ? N4 Ni2 O1 C5 -36.4(9) . . . . ? O8 Ni2 O1 C5 -130.0(8) . . . . ? O3 Ni2 O1 C5 147.0(8) . . . . ? N3 Ni2 O1 C5 46.5(8) . . . . ? O6 Ni2 O1 C5 -172.0(14) . . . . ? Ni2 Ni2 O1 C5 -170.5(7) 4 . . . ? Ni1 Ni2 O1 C5 -171.8(11) . . . . ? N4 Ni2 O1 Ni1 135.4(6) . . . . ? O8 Ni2 O1 Ni1 41.8(5) . . . . ? O3 Ni2 O1 Ni1 -41.2(5) . . . . ? N3 Ni2 O1 Ni1 -141.7(5) . . . . ? O6 Ni2 O1 Ni1 -0.1(18) . . . . ? Ni2 Ni2 O1 Ni1 1.4(6) 4 . . . ? O2 Ni1 O1 C5 -150.2(9) . . . . ? O5 Ni1 O1 C5 161.4(10) . . . . ? N1 Ni1 O1 C5 31.6(9) . . . . ? N2 Ni1 O1 C5 -53.5(9) . . . . ? O7 Ni1 O1 C5 129.7(9) . . . . ? Ni1 Ni1 O1 C5 169.9(8) 4 . . . ? Ni2 Ni1 O1 C5 171.3(12) . . . . ? O2 Ni1 O1 Ni2 38.5(5) . . . . ? O5 Ni1 O1 Ni2 -9.9(13) . . . . ? N1 Ni1 O1 Ni2 -139.6(6) . . . . ? N2 Ni1 O1 Ni2 135.2(5) . . . . ? O7 Ni1 O1 Ni2 -41.6(5) . . . . ? Ni1 Ni1 O1 Ni2 -1.4(6) 4 . . . ? O3 Cl1 O2 Ni1 -64.3(6) . . . . ? O4 Cl1 O2 Ni1 174.8(6) 4 . . . ? O4 Cl1 O2 Ni1 56.6(8) . . . . ? O3 Cl1 O2 Ni1 64.3(6) . . . 4 ? O4 Cl1 O2 Ni1 -56.6(8) 4 . . 4 ? O4 Cl1 O2 Ni1 -174.8(6) . . . 4 ? O4 Cl1 O2 O3 -120.9(4) 4 . . . ? O4 Cl1 O2 O3 120.9(4) . . . . ? O1 Ni1 O2 Cl1 17.3(7) . . . . ? O5 Ni1 O2 Cl1 -177.6(7) . . . . ? N1 Ni1 O2 Cl1 173(5) . . . . ? N2 Ni1 O2 Cl1 -86.6(7) . . . . ? O7 Ni1 O2 Cl1 105.5(7) . . . . ? Ni1 Ni1 O2 Cl1 142.1(9) 4 . . . ? Ni2 Ni1 O2 Cl1 33.7(6) . . . . ? O1 Ni1 O2 Ni1 -124.8(4) . . . 4 ? O5 Ni1 O2 Ni1 40.3(3) . . . 4 ? N1 Ni1 O2 Ni1 31(5) . . . 4 ? N2 Ni1 O2 Ni1 131.3(4) . . . 4 ? O7 Ni1 O2 Ni1 -36.6(4) . . . 4 ? Ni2 Ni1 O2 Ni1 -108.4(3) . . . 4 ? O1 Ni1 O2 O3 -14.9(4) . . . . ? O5 Ni1 O2 O3 150.3(4) . . . . ? N1 Ni1 O2 O3 141(5) . . . . ? N2 Ni1 O2 O3 -118.8(4) . . . . ? O7 Ni1 O2 O3 73.3(4) . . . . ? Ni1 Ni1 O2 O3 109.9(5) 4 . . . ? Ni2 Ni1 O2 O3 1.5(3) . . . . ? O2 Cl1 O3 Ni2 -58.4(6) . . . 4 ? O4 Cl1 O3 Ni2 62.8(8) 4 . . 4 ? O4 Cl1 O3 Ni2 -179.6(5) . . . 4 ? O2 Cl1 O3 Ni2 58.4(6) . . . . ? O4 Cl1 O3 Ni2 179.6(5) 4 . . . ? O4 Cl1 O3 Ni2 -62.8(8) . . . . ? O4 Cl1 O3 O2 121.2(4) 4 . . . ? O4 Cl1 O3 O2 -121.2(4) . . . . ? N4 Ni2 O3 Cl1 -172(2) . . . . ? O8 Ni2 O3 Cl1 -104.2(7) . . . . ? O1 Ni2 O3 Cl1 -11.0(7) . . . . ? N3 Ni2 O3 Cl1 84.1(7) . . . . ? O6 Ni2 O3 Cl1 178.7(7) . . . . ? Ni2 Ni2 O3 Cl1 -133.3(9) 4 . . . ? Ni1 Ni2 O3 Cl1 -28.1(6) . . . . ? N4 Ni2 O3 Ni2 -39(3) . . . 4 ? O8 Ni2 O3 Ni2 29.1(4) . . . 4 ? O1 Ni2 O3 Ni2 122.3(4) . . . 4 ? N3 Ni2 O3 Ni2 -142.7(4) . . . 4 ? O6 Ni2 O3 Ni2 -48.1(3) . . . 4 ? Ni1 Ni2 O3 Ni2 105.2(3) . . . 4 ? N4 Ni2 O3 O2 -142(2) . . . . ? O8 Ni2 O3 O2 -74.6(4) . . . . ? O1 Ni2 O3 O2 18.6(4) . . . . ? N3 Ni2 O3 O2 113.6(4) . . . . ? O6 Ni2 O3 O2 -151.8(4) . . . . ? Ni2 Ni2 O3 O2 -103.7(5) 4 . . . ? Ni1 Ni2 O3 O2 1.5(2) . . . . ? Ni1 O2 O3 Cl1 131.6(3) . . . . ? Ni1 O2 O3 Cl1 -131.6(3) 4 . . . ? Cl1 O2 O3 Ni2 134.3(3) . . . 4 ? Ni1 O2 O3 Ni2 -94.1(3) . . . 4 ? Ni1 O2 O3 Ni2 2.7(4) 4 . . 4 ? Cl1 O2 O3 Ni2 -134.3(3) . . . . ? Ni1 O2 O3 Ni2 -2.7(4) . . . . ? Ni1 O2 O3 Ni2 94.1(3) 4 . . . ? O2 Ni1 O5 Ni1 -39.7(3) . . . 4 ? O1 Ni1 O5 Ni1 10.8(12) . . . 4 ? N1 Ni1 O5 Ni1 139.6(4) . . . 4 ? N2 Ni1 O5 Ni1 -135.4(4) . . . 4 ? O7 Ni1 O5 Ni1 43.7(3) . . . 4 ? Ni2 Ni1 O5 Ni1 4.8(5) . . . 4 ? N4 Ni2 O6 Ni2 -133.8(4) . . . 4 ? O8 Ni2 O6 Ni2 -41.7(3) . . . 4 ? O1 Ni2 O6 Ni2 1.7(16) . . . 4 ? O3 Ni2 O6 Ni2 44.5(3) . . . 4 ? N3 Ni2 O6 Ni2 143.1(3) . . . 4 ? Ni1 Ni2 O6 Ni2 1.7(6) . . . 4 ? N4 Ni2 O6 O3W 118.5(5) . . . . ? O8 Ni2 O6 O3W -149.4(5) . . . . ? O1 Ni2 O6 O3W -106.0(14) . . . . ? O3 Ni2 O6 O3W -63.2(5) . . . . ? N3 Ni2 O6 O3W 35.4(5) . . . . ? Ni2 Ni2 O6 O3W -107.7(5) 4 . . . ? Ni1 Ni2 O6 O3W -106.0(5) . . . . ? O2 Ni1 O7 Ni1 35.1(4) . . . 4 ? O1 Ni1 O7 Ni1 127.1(4) . . . 4 ? O5 Ni1 O7 Ni1 -42.5(3) . . . 4 ? N1 Ni1 O7 Ni1 -140.6(4) . . . 4 ? N2 Ni1 O7 Ni1 -38(2) . . . 4 ? Ni2 Ni1 O7 Ni1 109.3(3) . . . 4 ? O2 Ni1 O7 O8 -73.1(4) . . . . ? O1 Ni1 O7 O8 18.9(4) . . . . ? O5 Ni1 O7 O8 -150.7(4) . . . . ? N1 Ni1 O7 O8 111.2(4) . . . . ? N2 Ni1 O7 O8 -146.6(17) . . . . ? Ni1 Ni1 O7 O8 -108.2(5) 4 . . . ? Ni2 Ni1 O7 O8 1.2(2) . . . . ? O2 Ni1 O7 O1W -179.9(8) . . . . ? O1 Ni1 O7 O1W -87.9(7) . . . . ? O5 Ni1 O7 O1W 102.5(8) . . . . ? N1 Ni1 O7 O1W 4.4(8) . . . . ? N2 Ni1 O7 O1W 106.5(17) . . . . ? Ni1 Ni1 O7 O1W 145.0(9) 4 . . . ? Ni2 Ni1 O7 O1W -105.7(7) . . . . ? N4 Ni2 O8 Ni2 140.6(4) . . . 4 ? O1 Ni2 O8 Ni2 -124.0(3) . . . 4 ? O3 Ni2 O8 Ni2 -29.8(4) . . . 4 ? N3 Ni2 O8 Ni2 80(2) . . . 4 ? O6 Ni2 O8 Ni2 46.2(3) . . . 4 ? Ni1 Ni2 O8 Ni2 -106.6(3) . . . 4 ? N4 Ni2 O8 O7 -111.6(4) . . . . ? O1 Ni2 O8 O7 -16.2(4) . . . . ? O3 Ni2 O8 O7 78.0(4) . . . . ? N3 Ni2 O8 O7 -172(2) . . . . ? O6 Ni2 O8 O7 154.0(4) . . . . ? Ni2 Ni2 O8 O7 107.8(5) 4 . . . ? Ni1 Ni2 O8 O7 1.2(3) . . . . ? Ni1 O7 O8 Ni2 2.1(4) 4 . . 4 ? Ni1 O7 O8 Ni2 93.8(3) . . . 4 ? O1W O7 O8 Ni2 -132.0(3) . . . 4 ? Ni1 O7 O8 Ni2 -93.8(3) 4 . . . ? Ni1 O7 O8 Ni2 -2.1(4) . . . . ? O1W O7 O8 Ni2 132.0(3) . . . . ? O2 Ni1 N1 C8 -136(5) . . . . ? O1 Ni1 N1 C8 20.0(8) . . . . ? O5 Ni1 N1 C8 -144.9(8) . . . . ? N2 Ni1 N1 C8 123.5(9) . . . . ? O7 Ni1 N1 C8 -68.8(9) . . . . ? Ni1 Ni1 N1 C8 -106.9(8) 4 . . . ? Ni2 Ni1 N1 C8 2.6(9) . . . . ? O2 Ni1 N1 C11 102(5) . . . . ? O1 Ni1 N1 C11 -101.9(8) . . . . ? O5 Ni1 N1 C11 93.1(8) . . . . ? N2 Ni1 N1 C11 1.6(8) . . . . ? O7 Ni1 N1 C11 169.2(8) . . . . ? Ni1 Ni1 N1 C11 131.1(7) 4 . . . ? Ni2 Ni1 N1 C11 -119.4(7) . . . . ? O2 Ni1 N1 C9 -18(5) . . . . ? O1 Ni1 N1 C9 138.6(8) . . . . ? O5 Ni1 N1 C9 -26.4(8) . . . . ? N2 Ni1 N1 C9 -117.9(8) . . . . ? O7 Ni1 N1 C9 49.7(8) . . . . ? Ni1 Ni1 N1 C9 11.6(9) 4 . . . ? Ni2 Ni1 N1 C9 121.2(7) . . . . ? O2 Ni1 N2 C14 89.9(9) . . . . ? O1 Ni1 N2 C14 -3.4(10) . . . . ? O5 Ni1 N2 C14 165.6(9) . . . . ? N1 Ni1 N2 C14 -94.7(9) . . . . ? O7 Ni1 N2 C14 161.7(16) . . . . ? Ni1 Ni1 N2 C14 128.9(8) 4 . . . ? Ni2 Ni1 N2 C14 17.2(10) . . . . ? O2 Ni1 N2 C13 -35.2(9) . . . . ? O1 Ni1 N2 C13 -128.5(8) . . . . ? O5 Ni1 N2 C13 40.5(9) . . . . ? N1 Ni1 N2 C13 140.2(9) . . . . ? O7 Ni1 N2 C13 37(2) . . . . ? Ni1 Ni1 N2 C13 3.8(10) 4 . . . ? Ni2 Ni1 N2 C13 -107.9(8) . . . . ? O2 Ni1 N2 C12 -149.6(8) . . . . ? O1 Ni1 N2 C12 117.1(8) . . . . ? O5 Ni1 N2 C12 -73.9(8) . . . . ? N1 Ni1 N2 C12 25.8(8) . . . . ? O7 Ni1 N2 C12 -78(2) . . . . ? Ni1 Ni1 N2 C12 -110.6(7) 4 . . . ? Ni2 Ni1 N2 C12 137.7(7) . . . . ? N4 Ni2 N3 C15 101.3(8) . . . . ? O8 Ni2 N3 C15 162.8(19) . . . . ? O1 Ni2 N3 C15 6.6(8) . . . . ? O3 Ni2 N3 C15 -88.8(8) . . . . ? O6 Ni2 N3 C15 -164.5(8) . . . . ? Ni2 Ni2 N3 C15 -125.5(7) 4 . . . ? Ni1 Ni2 N3 C15 -10.4(9) . . . . ? N4 Ni2 N3 C16 -21.3(8) . . . . ? O8 Ni2 N3 C16 40(3) . . . . ? O1 Ni2 N3 C16 -115.9(8) . . . . ? O3 Ni2 N3 C16 148.6(8) . . . . ? O6 Ni2 N3 C16 72.9(8) . . . . ? Ni2 Ni2 N3 C16 111.9(7) 4 . . . ? Ni1 Ni2 N3 C16 -133.0(7) . . . . ? O8 Ni2 N4 C21 21.4(11) . . . . ? O1 Ni2 N4 C21 -72.7(10) . . . . ? O3 Ni2 N4 C21 88(3) . . . . ? N3 Ni2 N4 C21 -166.2(11) . . . . ? O6 Ni2 N4 C21 97.4(11) . . . . ? Ni2 Ni2 N4 C21 54.7(11) 4 . . . ? Ni1 Ni2 N4 C21 -53.4(11) . . . . ? O8 Ni2 N4 C17 -165.0(8) . . . . ? O1 Ni2 N4 C17 100.9(8) . . . . ? O3 Ni2 N4 C17 -98(2) . . . . ? N3 Ni2 N4 C17 7.5(8) . . . . ? O6 Ni2 N4 C17 -89.0(8) . . . . ? Ni2 Ni2 N4 C17 -131.7(7) 4 . . . ? Ni1 Ni2 N4 C17 120.2(8) . . . . ? C7 C2 C3 C4 -1.6(18) . . . . ? C1 C2 C3 C4 -175.2(11) . . . . ? C2 C3 C4 C5 -0.1(18) . . . . ? C2 C3 C4 C8 178.8(11) . . . . ? Ni2 O1 C5 C4 126.3(10) . . . . ? Ni1 O1 C5 C4 -46.4(14) . . . . ? Ni2 O1 C5 C6 -54.9(12) . . . . ? Ni1 O1 C5 C6 132.4(10) . . . . ? C3 C4 C5 O1 179.8(10) . . . . ? C8 C4 C5 O1 1.0(17) . . . . ? C3 C4 C5 C6 1.0(17) . . . . ? C8 C4 C5 C6 -177.9(11) . . . . ? O1 C5 C6 C7 -179.0(11) . . . . ? C4 C5 C6 C7 -0.1(17) . . . . ? O1 C5 C6 C15 0.1(17) . . . . ? C4 C5 C6 C15 178.9(11) . . . . ? C5 C6 C7 C2 -1.6(19) . . . . ? C15 C6 C7 C2 179.3(11) . . . . ? C3 C2 C7 C6 2.4(19) . . . . ? C1 C2 C7 C6 175.9(12) . . . . ? C11 N1 C8 C4 57.2(14) . . . . ? C9 N1 C8 C4 178.8(10) . . . . ? Ni1 N1 C8 C4 -62.9(12) . . . . ? C3 C4 C8 N1 -117.4(13) . . . . ? C5 C4 C8 N1 61.4(15) . . . . ? C8 N1 C9 C10 -63.8(15) . . . . ? C11 N1 C9 C10 58.4(15) . . . . ? Ni1 N1 C9 C10 176.4(12) . . . . ? C8 N1 C11 C12 -150.7(11) . . . . ? C9 N1 C11 C12 88.7(13) . . . . ? Ni1 N1 C11 C12 -29.3(12) . . . . ? C14 N2 C12 C11 73.6(13) . . . . ? C13 N2 C12 C11 -168.7(10) . . . . ? Ni1 N2 C12 C11 -50.0(12) . . . . ? N1 C11 C12 N2 55.2(14) . . . . ? C16 N3 C15 C6 63.5(14) . . . . ? Ni2 N3 C15 C6 -55.7(12) . . . . ? C7 C6 C15 N3 -115.5(12) . . . . ? C5 C6 C15 N3 65.4(14) . . . . ? C15 N3 C16 C17 -89.9(13) . . . . ? Ni2 N3 C16 C17 31.5(12) . . . . ? C21 N4 C17 C18 0.8(18) . . . . ? Ni2 N4 C17 C18 -173.3(9) . . . . ? C21 N4 C17 C16 -176.6(11) . . . . ? Ni2 N4 C17 C16 9.3(14) . . . . ? N3 C16 C17 N4 -28.1(16) . . . . ? N3 C16 C17 C18 154.5(11) . . . . ? N4 C17 C18 C19 -0.8(19) . . . . ? C16 C17 C18 C19 176.4(13) . . . . ? C17 C18 C19 C20 0(2) . . . . ? C18 C19 C20 C21 1(2) . . . . ? C17 N4 C21 C20 0(2) . . . . ? Ni2 N4 C21 C20 173.4(10) . . . . ? C19 C20 C21 N4 -1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.461 _refine_diff_density_min -0.846 _refine_diff_density_rms 0.142