Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_1 _database_code_CSD 167337 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Miao Du' 'Xian-He Bu' 'Ya-Mei Guo' 'Lei Zhang' 'Dai-Zheng Liao' 'Joan Ribas' _publ_contact_author_name 'Prof Xian-He Bu' _publ_contact_author_address ; Chemistry Nankai University Weijin Road 94 Tianjin 300071 CHINA ; _publ_contact_author_email 'BUXH@NANKAI.EDU.CN' _publ_requested_journal 'Chemical Communications' _publ_section_title ; First tetrameric NiII cluster with planar triangular topology exhibiting ferromagnetic pathways ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H68 Cl2 N6 Ni4 O24' _chemical_formula_weight 1274.70 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 C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 24.253(7) _cell_length_b 12.158(4) _cell_length_c 8.378(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.557(4) _cell_angle_gamma 90.00 _cell_volume 2443.0(12) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3318 _cell_measurement_theta_min 1.88 _cell_measurement_theta_max 25.02 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.733 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 1.718 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7250 _exptl_absorpt_correction_T_max 0.8469 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 1000 CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5084 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3350 _reflns_number_gt 3197 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _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^)+(0.0576P)^2^+3.6917P] 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 0.00 _refine_ls_number_reflns 3350 _refine_ls_number_parameters 338 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0906 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 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 Ni3 Ni 0.89289(2) 0.34422(5) 0.15138(7) 0.02634(15) Uani 1 1 d . . . Ni1 Ni 1.0000 0.41457(7) 0.0000 0.0244(2) Uani 1 2 d S . . Ni2 Ni 1.0000 0.65641(7) 0.0000 0.0279(2) Uani 1 2 d S . . N2 N 0.85644(17) 0.3843(4) 0.3540(5) 0.0350(10) Uani 1 1 d . . . N1 N 0.81858(16) 0.2648(4) 0.0672(5) 0.0343(10) Uani 1 1 d . . . N3 N 1.0534(2) 0.7787(4) 0.0996(6) 0.0411(11) Uani 1 1 d . . . O3 O 0.96641(13) 0.4403(3) 0.2205(4) 0.0277(8) Uani 1 1 d . . . O4 O 0.96941(15) 0.6253(3) 0.2164(4) 0.0365(9) Uani 1 1 d . . . O1 O 0.93565(13) 0.3032(3) -0.0393(4) 0.0307(8) Uani 1 1 d . . . O2 O 0.95916(16) 0.1795(4) -0.2114(6) 0.0629(14) Uani 1 1 d . . . O6 O 1.05742(11) 0.5322(4) 0.0866(4) 0.0270(6) Uani 1 1 d . . . O5 O 0.86609(13) 0.4828(3) 0.0182(4) 0.0342(8) Uani 1 1 d . . . O7 O 0.93590(16) 0.2098(4) 0.2583(6) 0.0469(11) Uani 1 1 d D . . C1 C 0.8397(2) 0.2830(6) 0.4368(7) 0.0466(15) Uani 1 1 d . . . H1A H 0.8225 0.3070 0.5282 0.056 Uiso 1 1 calc R . . H1B H 0.8737 0.2446 0.4803 0.056 Uiso 1 1 calc R . . C2 C 0.8011(2) 0.1995(5) 0.3455(8) 0.0474(15) Uani 1 1 d . . . H2A H 0.7633 0.2259 0.3425 0.057 Uiso 1 1 calc R . . H2B H 0.8043 0.1319 0.4076 0.057 Uiso 1 1 calc R . . C3 C 0.8092(2) 0.1708(5) 0.1723(7) 0.0429(14) Uani 1 1 d . . . H3A H 0.8407 0.1212 0.1770 0.051 Uiso 1 1 calc R . . H3B H 0.7764 0.1312 0.1219 0.051 Uiso 1 1 calc R . . C4 C 0.77023(17) 0.3442(6) 0.0485(6) 0.0396(11) Uani 1 1 d . . . H4A H 0.7368 0.3028 0.0092 0.047 Uiso 1 1 calc R . . H4B H 0.7758 0.3961 -0.0356 0.047 Uiso 1 1 calc R . . C5 C 0.7586(2) 0.4107(6) 0.1948(7) 0.0487(14) Uani 1 1 d . . . H5A H 0.7340 0.4709 0.1555 0.058 Uiso 1 1 calc R . . H5B H 0.7381 0.3637 0.2589 0.058 Uiso 1 1 calc R . . C6 C 0.8075(2) 0.4585(5) 0.3061(7) 0.0397(13) Uani 1 1 d . . . H6A H 0.8204 0.5229 0.2543 0.048 Uiso 1 1 calc R . . H6B H 0.7942 0.4832 0.4037 0.048 Uiso 1 1 calc R . . C7 C 0.8994(2) 0.4409(5) 0.4710(6) 0.0398(13) Uani 1 1 d . . . H7A H 0.9298 0.3899 0.5024 0.048 Uiso 1 1 calc R . . H7B H 0.8830 0.4578 0.5670 0.048 Uiso 1 1 calc R . . C8 C 0.9233(2) 0.5454(5) 0.4132(6) 0.0387(12) Uani 1 1 d . . . H8A H 0.9477 0.5775 0.5034 0.046 Uiso 1 1 calc R . . H8B H 0.8928 0.5966 0.3833 0.046 Uiso 1 1 calc R . . C9 C 0.95558(17) 0.5365(6) 0.2728(5) 0.0303(10) Uani 1 1 d . . . C10 C 0.8223(2) 0.2234(5) -0.1003(7) 0.0416(13) Uani 1 1 d . . . H10A H 0.8218 0.2863 -0.1716 0.050 Uiso 1 1 calc R . . H10B H 0.7892 0.1802 -0.1369 0.050 Uiso 1 1 calc R . . C11 C 0.8728(2) 0.1543(5) -0.1182(7) 0.0411(12) Uani 1 1 d . . . H11A H 0.8644 0.1115 -0.2165 0.049 Uiso 1 1 calc R . . H11B H 0.8787 0.1028 -0.0288 0.049 Uiso 1 1 calc R . . C12 C 0.9266(2) 0.2159(4) -0.1236(6) 0.0324(12) Uani 1 1 d . . . C13 C 0.89251(17) 0.5473(4) -0.0593(5) 0.0260(10) Uani 1 1 d . . . C14 C 0.8628(2) 0.6500(6) -0.1247(7) 0.0440(13) Uani 1 1 d . . . H14A H 0.8489 0.6876 -0.0367 0.053 Uiso 1 1 calc R . . H14B H 0.8308 0.6288 -0.2023 0.053 Uiso 1 1 calc R . . C15 C 0.8979(2) 0.7308(5) -0.2060(8) 0.0471(15) Uani 1 1 d . . . H15A H 0.9114 0.6935 -0.2950 0.057 Uiso 1 1 calc R . . H15B H 0.8740 0.7906 -0.2511 0.057 Uiso 1 1 calc R . . C16 C 0.9271(2) 0.8433(6) 0.0314(8) 0.0556(16) Uani 1 1 d . . . H16A H 0.9094 0.7930 0.0980 0.067 Uiso 1 1 calc R . . H16B H 0.8986 0.8940 -0.0176 0.067 Uiso 1 1 calc R . . C17 C 0.9697(3) 0.9077(6) 0.1392(10) 0.0639(19) Uani 1 1 d . . . H17A H 0.9524 0.9343 0.2291 0.077 Uiso 1 1 calc R . . H17B H 0.9791 0.9717 0.0796 0.077 Uiso 1 1 calc R . . C18 C 1.0251(2) 0.8499(6) 0.2100(8) 0.0555(16) Uani 1 1 d . . . H18A H 1.0513 0.9064 0.2535 0.067 Uiso 1 1 calc R . . H18B H 1.0178 0.8047 0.2999 0.067 Uiso 1 1 calc R . . Cl1 Cl 0.81393(10) 0.8690(2) 0.3827(3) 0.0947(9) Uani 1 1 d . . . O8 O 0.8104(4) 0.7641(8) 0.4115(18) 0.191(5) Uani 1 1 d . . . O9 O 0.8363(3) 0.9066(9) 0.2514(9) 0.130(3) Uani 1 1 d . . . O10 O 0.8397(4) 0.9234(9) 0.5222(10) 0.178(5) Uani 1 1 d . . . O11 O 0.7565(3) 0.9174(9) 0.3497(9) 0.131(3) Uani 1 1 d . . . O12 O 0.9319(2) 0.0633(4) 0.4942(5) 0.0607(12) Uani 1 1 d D . . H7C H 0.933(2) 0.165(4) 0.335(5) 0.041(16) Uiso 1 1 d D . . H7D H 0.9676(14) 0.187(6) 0.241(8) 0.06(2) Uiso 1 1 d D . . H12A H 0.9064(18) 0.016(4) 0.500(7) 0.042(17) Uiso 1 1 d 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 Ni3 0.0233(2) 0.0302(3) 0.0269(3) 0.0035(3) 0.00827(19) 0.0000(3) Ni1 0.0220(4) 0.0268(5) 0.0252(4) 0.000 0.0066(3) 0.000 Ni2 0.0316(4) 0.0228(4) 0.0317(5) 0.000 0.0128(3) 0.000 N2 0.035(2) 0.043(3) 0.031(2) 0.0074(19) 0.0160(16) 0.0024(17) N1 0.0277(19) 0.038(3) 0.038(2) 0.001(2) 0.0092(17) -0.0061(17) N3 0.052(3) 0.032(3) 0.043(3) -0.011(2) 0.019(2) -0.005(2) O3 0.0249(16) 0.033(2) 0.0257(18) -0.0042(16) 0.0048(12) -0.0020(14) O4 0.0422(18) 0.033(2) 0.0378(19) -0.0059(16) 0.0163(15) -0.0037(15) O1 0.0284(15) 0.033(2) 0.0318(19) -0.0057(16) 0.0083(13) -0.0038(13) O2 0.044(2) 0.068(3) 0.082(3) -0.046(3) 0.028(2) -0.021(2) O6 0.0258(14) 0.0263(17) 0.0299(16) -0.0033(17) 0.0072(11) -0.0016(16) O5 0.0260(16) 0.035(2) 0.042(2) 0.0050(17) 0.0087(15) 0.0004(14) O7 0.038(2) 0.047(3) 0.060(3) 0.029(2) 0.0204(19) 0.0115(18) C1 0.041(3) 0.052(4) 0.052(4) 0.026(3) 0.023(3) 0.009(3) C2 0.036(3) 0.044(3) 0.067(4) 0.016(3) 0.022(3) -0.006(2) C3 0.038(3) 0.038(3) 0.056(4) 0.004(3) 0.016(2) -0.005(2) C4 0.0214(19) 0.046(3) 0.051(3) 0.005(3) 0.0047(18) -0.004(2) C5 0.034(3) 0.057(4) 0.058(4) 0.008(3) 0.015(2) 0.006(3) C6 0.038(3) 0.039(3) 0.046(3) 0.000(2) 0.017(2) 0.012(2) C7 0.038(3) 0.060(4) 0.024(3) -0.001(3) 0.014(2) -0.002(2) C8 0.039(2) 0.050(3) 0.029(2) -0.013(3) 0.0115(19) -0.004(3) C9 0.030(2) 0.040(3) 0.022(2) -0.008(3) 0.0067(16) -0.003(3) C10 0.031(3) 0.047(4) 0.046(3) -0.008(3) 0.004(2) -0.014(2) C11 0.039(3) 0.036(3) 0.051(3) -0.011(3) 0.013(2) -0.010(2) C12 0.030(2) 0.033(3) 0.035(3) -0.002(2) 0.010(2) 0.000(2) C13 0.026(2) 0.028(3) 0.023(2) 0.003(2) 0.0025(16) 0.000(2) C14 0.034(2) 0.045(3) 0.053(3) 0.015(3) 0.006(2) 0.011(3) C15 0.048(3) 0.040(3) 0.057(4) 0.019(3) 0.018(3) 0.013(2) C16 0.064(3) 0.034(3) 0.077(4) 0.000(4) 0.037(3) 0.019(3) C17 0.070(4) 0.040(4) 0.088(5) -0.017(4) 0.032(4) 0.005(4) C18 0.069(4) 0.037(3) 0.068(4) -0.026(4) 0.032(3) -0.006(3) Cl1 0.0985(15) 0.114(2) 0.0669(12) 0.0158(12) -0.0037(10) -0.0564(14) O8 0.139(8) 0.084(7) 0.328(16) -0.013(9) -0.038(9) -0.008(6) O9 0.101(5) 0.189(9) 0.111(5) -0.028(6) 0.055(4) -0.027(6) O10 0.223(10) 0.179(9) 0.104(6) 0.071(6) -0.073(6) -0.136(8) O11 0.087(4) 0.199(9) 0.111(5) -0.037(6) 0.027(4) -0.030(5) O12 0.081(3) 0.051(3) 0.049(2) 0.009(2) 0.008(2) -0.014(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 Ni3 O5 2.071(4) . ? Ni3 N1 2.074(4) . ? Ni3 O7 2.069(4) . ? Ni3 O1 2.090(3) . ? Ni3 N2 2.085(4) . ? Ni3 O3 2.138(3) . ? Ni1 O6 2.052(4) . ? Ni1 O6 2.052(4) 2_755 ? Ni1 O1 2.056(3) . ? Ni1 O1 2.056(3) 2_755 ? Ni1 O3 2.150(3) . ? Ni1 O3 2.150(3) 2_755 ? Ni1 Ni2 2.9403(14) . ? Ni2 N3 2.064(5) . ? Ni2 N3 2.064(5) 2_755 ? Ni2 O4 2.093(4) 2_755 ? Ni2 O4 2.093(3) . ? Ni2 O6 2.109(4) 2_755 ? Ni2 O6 2.109(4) . ? N2 C7 1.488(7) . ? N2 C6 1.498(7) . ? N2 C1 1.499(7) . ? N1 C3 1.481(7) . ? N1 C10 1.506(7) . ? N1 C4 1.509(7) . ? N3 C16 1.484(7) 2_755 ? N3 C15 1.488(8) 2_755 ? N3 C18 1.505(7) . ? O3 C9 1.290(7) . ? O4 C9 1.245(7) . ? O1 C12 1.275(6) . ? O2 C12 1.238(6) . ? O6 C13 1.282(5) 2_755 ? O5 C13 1.253(6) . ? C1 C2 1.509(10) . ? C2 C3 1.533(9) . ? C4 C5 1.529(8) . ? C5 C6 1.511(8) . ? C7 C8 1.506(8) . ? C8 C9 1.511(6) . ? C10 C11 1.510(8) . ? C11 C12 1.513(7) . ? C13 O6 1.282(5) 2_755 ? C13 C14 1.504(8) . ? C14 C15 1.526(8) . ? C15 N3 1.488(8) 2_755 ? C16 N3 1.484(7) 2_755 ? C16 C17 1.490(9) . ? C17 C18 1.553(9) . ? Cl1 O8 1.303(11) . ? Cl1 O9 1.376(7) . ? Cl1 O10 1.406(9) . ? Cl1 O11 1.499(9) . ? 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 O5 Ni3 N1 90.48(16) . . ? O5 Ni3 O7 166.66(14) . . ? N1 Ni3 O7 97.82(19) . . ? O5 Ni3 O1 86.21(14) . . ? N1 Ni3 O1 97.68(15) . . ? O7 Ni3 O1 82.35(16) . . ? O5 Ni3 N2 96.41(16) . . ? N1 Ni3 N2 86.19(17) . . ? O7 Ni3 N2 94.57(17) . . ? O1 Ni3 N2 175.33(15) . . ? O5 Ni3 O3 83.33(14) . . ? N1 Ni3 O3 173.78(17) . . ? O7 Ni3 O3 88.15(16) . . ? O1 Ni3 O3 81.31(12) . . ? N2 Ni3 O3 95.13(15) . . ? O6 Ni1 O6 91.6(2) . 2_755 ? O6 Ni1 O1 167.15(12) . . ? O6 Ni1 O1 86.76(14) 2_755 . ? O6 Ni1 O1 86.76(14) . 2_755 ? O6 Ni1 O1 167.15(12) 2_755 2_755 ? O1 Ni1 O1 97.6(2) . 2_755 ? O6 Ni1 O3 85.34(12) . . ? O6 Ni1 O3 83.03(12) 2_755 . ? O1 Ni1 O3 81.81(13) . . ? O1 Ni1 O3 109.51(13) 2_755 . ? O6 Ni1 O3 83.03(12) . 2_755 ? O6 Ni1 O3 85.34(12) 2_755 2_755 ? O1 Ni1 O3 109.51(13) . 2_755 ? O1 Ni1 O3 81.81(13) 2_755 2_755 ? O3 Ni1 O3 163.29(19) . 2_755 ? O6 Ni1 Ni2 45.82(10) . . ? O6 Ni1 Ni2 45.82(10) 2_755 . ? O1 Ni1 Ni2 131.22(10) . . ? O1 Ni1 Ni2 131.22(10) 2_755 . ? O3 Ni1 Ni2 81.64(10) . . ? O3 Ni1 Ni2 81.64(10) 2_755 . ? N3 Ni2 N3 87.9(3) . 2_755 ? N3 Ni2 O4 101.46(16) . 2_755 ? N3 Ni2 O4 93.53(16) 2_755 2_755 ? N3 Ni2 O4 93.53(16) . . ? N3 Ni2 O4 101.46(16) 2_755 . ? O4 Ni2 O4 159.2(2) 2_755 . ? N3 Ni2 O6 175.81(15) . 2_755 ? N3 Ni2 O6 91.96(16) 2_755 2_755 ? O4 Ni2 O6 82.73(13) 2_755 2_755 ? O4 Ni2 O6 82.39(13) . 2_755 ? N3 Ni2 O6 91.96(16) . . ? N3 Ni2 O6 175.81(15) 2_755 . ? O4 Ni2 O6 82.39(13) 2_755 . ? O4 Ni2 O6 82.73(13) . . ? O6 Ni2 O6 88.50(19) 2_755 . ? N3 Ni2 Ni1 136.06(15) . . ? N3 Ni2 Ni1 136.06(15) 2_755 . ? O4 Ni2 Ni1 79.59(10) 2_755 . ? O4 Ni2 Ni1 79.59(10) . . ? O6 Ni2 Ni1 44.25(10) 2_755 . ? O6 Ni2 Ni1 44.25(10) . . ? C7 N2 C6 110.3(4) . . ? C7 N2 C1 106.6(4) . . ? C6 N2 C1 111.1(4) . . ? C7 N2 Ni3 107.7(3) . . ? C6 N2 Ni3 109.7(3) . . ? C1 N2 Ni3 111.2(4) . . ? C3 N1 C10 109.4(4) . . ? C3 N1 C4 111.7(4) . . ? C10 N1 C4 105.7(4) . . ? C3 N1 Ni3 111.1(3) . . ? C10 N1 Ni3 107.7(3) . . ? C4 N1 Ni3 111.1(3) . . ? C16 N3 C15 109.7(5) 2_755 2_755 ? C16 N3 C18 112.0(5) 2_755 . ? C15 N3 C18 104.5(5) 2_755 . ? C16 N3 Ni2 109.4(4) 2_755 . ? C15 N3 Ni2 110.8(4) 2_755 . ? C18 N3 Ni2 110.3(3) . . ? C9 O3 Ni3 112.6(3) . . ? C9 O3 Ni1 123.1(3) . . ? Ni3 O3 Ni1 95.47(13) . . ? C9 O4 Ni2 129.5(3) . . ? C12 O1 Ni1 134.4(3) . . ? C12 O1 Ni3 123.9(3) . . ? Ni1 O1 Ni3 99.87(14) . . ? C13 O6 Ni1 130.4(3) 2_755 . ? C13 O6 Ni2 115.5(3) 2_755 . ? Ni1 O6 Ni2 89.93(11) . . ? C13 O5 Ni3 130.1(3) . . ? N2 C1 C2 120.5(5) . . ? C1 C2 C3 118.4(4) . . ? N1 C3 C2 116.1(5) . . ? N1 C4 C5 119.2(4) . . ? C6 C5 C4 118.5(4) . . ? N2 C6 C5 116.8(5) . . ? N2 C7 C8 116.3(4) . . ? C7 C8 C9 117.3(5) . . ? O4 C9 O3 125.3(4) . . ? O4 C9 C8 115.7(5) . . ? O3 C9 C8 119.0(5) . . ? N1 C10 C11 116.1(5) . . ? C10 C11 C12 116.4(5) . . ? O2 C12 O1 123.7(5) . . ? O2 C12 C11 118.0(5) . . ? O1 C12 C11 118.2(4) . . ? O5 C13 O6 125.0(5) . 2_755 ? O5 C13 C14 117.0(4) . . ? O6 C13 C14 118.0(4) 2_755 . ? C13 C14 C15 115.3(4) . . ? N3 C15 C14 115.5(5) 2_755 . ? N3 C16 C17 117.2(5) 2_755 . ? C16 C17 C18 118.5(5) . . ? N3 C18 C17 118.3(5) . . ? O8 Cl1 O9 121.1(8) . . ? O8 Cl1 O10 109.9(8) . . ? O9 Cl1 O10 109.2(5) . . ? O8 Cl1 O11 109.5(6) . . ? O9 Cl1 O11 100.8(5) . . ? O10 Cl1 O11 104.8(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.879 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.070