Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr. Debashis Ray' _publ_contact_author_address ; Department of Chemistry Indian Institute of Technology Kharagpur-721302 India ; _publ_contact_author_email dray@chem.iitkgp.ernet.in _publ_contact_author_phone ' 03222-283324' _publ_contact_author_fax ' 913222-255303' loop_ _publ_author_name _publ_author_address 'Debashree Mandal' . 'Guillem Aromi' . 'Valerio Bertolasi' . 'Debashis Ray' ; Department of Chemistry Indian Institute of Technology Kharagpur-721302 India ; _publ_section_title ; A Ketone Oximate Based Cyclic Cationic [NiII4] Inverse Metallacrown from Simultaneous Chelation and Bridging of Two Ligands ; # Attachment 'Dr-Ni4.cif' data_drni4 _database_code_depnum_ccdc_archive 'CCDC 294831' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H50 N8 Ni4 O12, 3(Cl O4), C6 H16 N' _chemical_formula_sum 'C30 H66 Cl3 N9 Ni4 O24' _chemical_formula_weight 1278.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' 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 14.9193(3) _cell_length_b 24.7954(6) _cell_length_c 14.0215(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.150(2) _cell_angle_gamma 90.00 _cell_volume 5146.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295 _cell_measurement_reflns_used 13218 _cell_measurement_theta_min 3.38 _cell_measurement_theta_max 28.00 _exptl_crystal_description prismatic _exptl_crystal_colour brown _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2656 _exptl_absorpt_coefficient_mu 1.683 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.736 _exptl_absorpt_correction_T_max 0.901 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295 _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 'Nonius Kappa CCD' _diffrn_measurement_method '\f scans and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23241 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 28.00 _reflns_number_total 6184 _reflns_number_gt 4243 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1997)' _computing_cell_refinement 'Denzo SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996)' _computing_publication_material ; SHELXL-97 (Sheldrick, 1997), PARST (Nardelli, 1995) ; _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^)+(0.0670P)^2^+5.4277P] 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 6184 _refine_ls_number_parameters 328 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0782 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1287 _refine_ls_wR_factor_gt 0.1150 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Ni1 Ni 0.49130(2) 0.200330(16) 0.57712(2) 0.03262(12) Uani 1 1 d . . . Ni2 Ni 0.33480(2) 0.200904(17) 0.73609(2) 0.03315(13) Uani 1 1 d . . . O1 O 0.31485(14) 0.15654(10) 0.61388(14) 0.0421(5) Uani 1 1 d . . . O2 O 0.52373(15) 0.14599(10) 0.47336(14) 0.0428(5) Uani 1 1 d . . . O3 O 0.43922(13) 0.24639(8) 0.68241(13) 0.0332(4) Uani 1 1 d . . . O4 O 0.39911(14) 0.24615(9) 0.92939(14) 0.0392(5) Uani 1 1 d . . . O5 O 0.22580(15) 0.25387(10) 0.69655(15) 0.0433(5) Uani 1 1 d . . . O6 O 0.44176(14) 0.15450(9) 0.80423(14) 0.0321(4) Uani 1 1 d . . . N1 N 0.38443(16) 0.15020(11) 0.56594(16) 0.0344(6) Uani 1 1 d . . . N2 N 0.42551(19) 0.25804(12) 0.48451(18) 0.0438(7) Uani 1 1 d . . . H2A H 0.4663 0.2782 0.4583 0.053 Uiso 1 1 calc R . . H2B H 0.3895 0.2417 0.4368 0.053 Uiso 1 1 calc R . . N3 N 0.33845(16) 0.24921(11) 0.85297(16) 0.0338(5) Uani 1 1 d . . . N4 N 0.25572(18) 0.14206(12) 0.79028(19) 0.0447(7) Uani 1 1 d . . . H4A H 0.2138 0.1575 0.8223 0.054 Uiso 1 1 calc R . . H4B H 0.2273 0.1222 0.7420 0.054 Uiso 1 1 calc R . . C1 C 0.3837(2) 0.11090(14) 0.5042(2) 0.0411(7) Uani 1 1 d . . . C2 C 0.4670(2) 0.10952(14) 0.4582(2) 0.0408(7) Uani 1 1 d . . . C3 C 0.3075(3) 0.0721(2) 0.4848(3) 0.0748(14) Uani 1 1 d . . . H3A H 0.2642 0.0786 0.5287 0.112 Uiso 1 1 calc R . . H3B H 0.3301 0.0359 0.4931 0.112 Uiso 1 1 calc R . . H3C H 0.2791 0.0767 0.4200 0.112 Uiso 1 1 calc R . . C4 C 0.4847(3) 0.06385(17) 0.3937(3) 0.0611(10) Uani 1 1 d . . . H4C H 0.4423 0.0651 0.3364 0.092 Uiso 1 1 calc R . . H4D H 0.4783 0.0303 0.4263 0.092 Uiso 1 1 calc R . . H4E H 0.5450 0.0668 0.3770 0.092 Uiso 1 1 calc R . . C5 C 0.4198(2) 0.29917(14) 0.6420(2) 0.0423(8) Uani 1 1 d . . . H5A H 0.4755 0.3191 0.6401 0.051 Uiso 1 1 calc R . . H5B H 0.3821 0.3191 0.6812 0.051 Uiso 1 1 calc R . . C6 C 0.3714(3) 0.29227(16) 0.5413(2) 0.0488(9) Uani 1 1 d . . . H6A H 0.3128 0.2758 0.5441 0.059 Uiso 1 1 calc R . . H6B H 0.3619 0.3273 0.5107 0.059 Uiso 1 1 calc R . . C7 C 0.2719(2) 0.28272(14) 0.8550(2) 0.0355(7) Uani 1 1 d . . . C8 C 0.2102(2) 0.28339(14) 0.7649(2) 0.0389(7) Uani 1 1 d . . . C9 C 0.2585(3) 0.31686(16) 0.9402(2) 0.0494(9) Uani 1 1 d . . . H9A H 0.2023 0.3075 0.9626 0.074 Uiso 1 1 calc R . . H9B H 0.2575 0.3542 0.9221 0.074 Uiso 1 1 calc R . . H9C H 0.3072 0.3107 0.9906 0.074 Uiso 1 1 calc R . . C10 C 0.1313(3) 0.31965(18) 0.7554(3) 0.0583(10) Uani 1 1 d . . . H10A H 0.1511 0.3563 0.7512 0.087 Uiso 1 1 calc R . . H10B H 0.0995 0.3157 0.8105 0.087 Uiso 1 1 calc R . . H10C H 0.0917 0.3106 0.6984 0.087 Uiso 1 1 calc R . . C11 C 0.4046(2) 0.10172(14) 0.8168(2) 0.0396(7) Uani 1 1 d . . . H11A H 0.4462 0.0808 0.8610 0.048 Uiso 1 1 calc R . . H11B H 0.3958 0.0830 0.7557 0.048 Uiso 1 1 calc R . . C12 C 0.3162(2) 0.10742(16) 0.8560(2) 0.0465(8) Uani 1 1 d . . . H12A H 0.2889 0.0722 0.8613 0.056 Uiso 1 1 calc R . . H12B H 0.3257 0.1235 0.9195 0.056 Uiso 1 1 calc R . . H3 H 0.5000 0.2500 0.7500 0.08(2) Uiso 1 2 d S . . H6 H 0.473(4) 0.153(2) 0.765(4) 0.014(14) Uiso 0.50 1 d P . . Cl1 Cl 0.24165(11) -0.03046(6) 0.68640(11) 0.0936(5) Uani 1 1 d . . . O7 O 0.2420(7) -0.0437(2) 0.5898(4) 0.209(4) Uani 1 1 d . . . O8 O 0.3270(4) -0.0211(3) 0.7281(6) 0.191(3) Uani 1 1 d . . . O9 O 0.1936(4) 0.0177(2) 0.6860(5) 0.167(2) Uani 1 1 d . . . O10 O 0.2064(5) -0.0749(3) 0.7288(5) 0.161(2) Uani 1 1 d . . . Cl2 Cl 0.0000 0.17181(8) 0.7500 0.0764(5) Uani 1 2 d S . . O11 O 0.0561(4) 0.2028(2) 0.8205(4) 0.1338(19) Uani 1 1 d . . . O12 O 0.0585(3) 0.1424(3) 0.7012(5) 0.176(3) Uani 1 1 d . . . N1A N 0.5257(6) 0.5020(4) 0.5187(6) 0.081(3) Uani 0.50 1 d PD . . C1A C 0.5391(13) 0.5642(7) 0.5192(13) 0.146(6) Uiso 0.50 1 d PD . . C2A C 0.4545(13) 0.5924(8) 0.4951(14) 0.151(6) Uiso 0.50 1 d PD . . C3A C 0.5127(18) 0.4665(10) 0.4264(15) 0.186(9) Uiso 0.50 1 d PD . . C4A C 0.5913(19) 0.4731(13) 0.380(2) 0.219(11) Uiso 0.50 1 d PD . . C5A C 0.4483(13) 0.4885(9) 0.5812(13) 0.142(6) Uiso 0.50 1 d PD . . C6A C 0.458(2) 0.4396(11) 0.629(2) 0.230(11) Uiso 0.50 1 d PD . . 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 0.0253(2) 0.0456(3) 0.02616(19) -0.00141(14) -0.00022(13) -0.00202(16) Ni2 0.0226(2) 0.0488(3) 0.0273(2) -0.00436(14) 0.00019(13) 0.00175(17) O1 0.0245(11) 0.0667(16) 0.0352(11) -0.0106(10) 0.0045(8) -0.0043(10) O2 0.0367(12) 0.0589(16) 0.0332(11) -0.0038(9) 0.0058(9) -0.0013(11) O3 0.0280(10) 0.0417(12) 0.0279(9) 0.0001(8) -0.0037(7) 0.0009(9) O4 0.0307(11) 0.0594(15) 0.0258(10) -0.0047(9) -0.0028(8) 0.0081(10) O5 0.0311(12) 0.0634(16) 0.0341(11) -0.0044(10) -0.0016(8) 0.0070(11) O6 0.0249(10) 0.0423(13) 0.0292(10) -0.0006(8) 0.0043(8) -0.0024(9) N1 0.0275(13) 0.0492(16) 0.0256(11) -0.0033(10) -0.0003(9) -0.0022(11) N2 0.0395(15) 0.0605(19) 0.0288(13) 0.0034(11) -0.0061(10) -0.0032(14) N3 0.0248(12) 0.0469(16) 0.0288(12) 0.0004(10) 0.0003(9) 0.0033(11) N4 0.0286(14) 0.0607(19) 0.0451(15) -0.0069(12) 0.0060(11) -0.0062(13) C1 0.0381(17) 0.050(2) 0.0347(16) -0.0069(13) 0.0004(12) -0.0055(15) C2 0.0449(19) 0.047(2) 0.0295(15) -0.0039(12) 0.0013(12) 0.0034(16) C3 0.068(3) 0.085(3) 0.074(3) -0.034(2) 0.020(2) -0.032(3) C4 0.068(3) 0.058(3) 0.060(2) -0.0173(18) 0.0159(19) 0.002(2) C5 0.0434(19) 0.0435(19) 0.0378(17) 0.0006(13) -0.0039(13) 0.0037(15) C6 0.044(2) 0.061(2) 0.0385(17) 0.0077(14) -0.0070(14) 0.0087(17) C7 0.0317(16) 0.0459(18) 0.0296(14) -0.0008(12) 0.0066(11) 0.0019(14) C8 0.0282(16) 0.049(2) 0.0387(16) 0.0026(13) 0.0029(12) 0.0019(14) C9 0.050(2) 0.056(2) 0.0419(18) -0.0055(15) 0.0052(15) 0.0128(18) C10 0.043(2) 0.070(3) 0.058(2) -0.0056(18) -0.0092(16) 0.019(2) C11 0.0378(17) 0.0420(19) 0.0393(16) -0.0019(13) 0.0061(12) -0.0013(14) C12 0.0404(19) 0.055(2) 0.0450(18) -0.0002(15) 0.0094(14) -0.0100(16) Cl1 0.1001(11) 0.0805(9) 0.0897(9) -0.0134(7) -0.0297(8) 0.0204(8) O7 0.409(12) 0.119(4) 0.090(4) -0.017(3) -0.002(5) -0.052(6) O8 0.115(5) 0.202(7) 0.235(7) -0.024(6) -0.065(4) 0.036(4) O9 0.125(4) 0.115(4) 0.253(7) -0.033(4) -0.003(4) 0.050(4) O10 0.203(6) 0.130(5) 0.159(5) 0.018(4) 0.058(4) 0.011(4) Cl2 0.0418(8) 0.0832(12) 0.1044(12) 0.000 0.0099(8) 0.000 O11 0.101(3) 0.172(5) 0.132(4) -0.053(3) 0.027(3) -0.046(3) O12 0.075(3) 0.215(6) 0.226(6) -0.121(5) -0.028(3) 0.054(3) N1A 0.079(8) 0.087(6) 0.074(6) -0.015(5) -0.001(4) 0.019(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O4 2.002(2) 2_656 ? Ni1 N1 2.012(3) . ? Ni1 O2 2.084(2) . ? Ni1 O3 2.091(2) . ? Ni1 N2 2.093(3) . ? Ni1 O6 2.155(2) 2_656 ? Ni2 N3 2.025(2) . ? Ni2 O1 2.027(2) . ? Ni2 N4 2.079(3) . ? Ni2 O6 2.099(2) . ? Ni2 O5 2.110(2) . ? Ni2 O3 2.135(2) . ? O1 N1 1.315(3) . ? O2 C2 1.239(4) . ? O3 C5 1.441(4) . ? O3 H3 1.230(5) . ? O4 N3 1.316(3) . ? O4 Ni1 2.002(2) 2_656 ? O5 C8 1.250(4) . ? O6 C11 1.441(4) . ? O6 Ni1 2.155(2) 2_656 ? O6 H6 0.78(5) . ? N1 C1 1.302(4) . ? N2 C6 1.472(5) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C7 1.297(4) . ? N4 C12 1.481(5) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? C1 C2 1.471(4) . ? C1 C3 1.488(5) . ? C2 C4 1.493(5) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4C 0.9600 . ? C4 H4D 0.9600 . ? C4 H4E 0.9600 . ? C5 C6 1.514(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.469(4) . ? C7 C9 1.498(4) . ? C8 C10 1.474(5) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.498(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? Cl1 O8 1.353(6) . ? Cl1 O10 1.386(6) . ? Cl1 O9 1.392(5) . ? Cl1 O7 1.395(5) . ? Cl2 O12 1.381(5) . ? Cl2 O12 1.381(5) 2_556 ? Cl2 O11 1.436(5) . ? Cl2 O11 1.436(5) 2_556 ? N1A N1A 0.878(15) 5_666 ? N1A C3A 1.28(2) 5_666 ? N1A C5A 1.52(2) 5_666 ? N1A C1A 1.554(15) . ? N1A C3A 1.557(16) . ? N1A C5A 1.570(15) . ? N1A C1A 1.94(2) 5_666 ? C1A C3A 1.38(3) 5_666 ? C1A C2A 1.445(19) . ? C1A N1A 1.94(2) 5_666 ? C1A C5A 1.95(3) 5_666 ? C2A C3A 1.86(3) 5_666 ? C3A C5A 1.27(3) 5_666 ? C3A N1A 1.28(2) 5_666 ? C3A C1A 1.38(3) 5_666 ? C3A C4A 1.42(2) . ? C3A C2A 1.86(3) 5_666 ? C4A C5A 1.28(3) 5_666 ? C5A C3A 1.27(3) 5_666 ? C5A C4A 1.28(3) 5_666 ? C5A C6A 1.38(2) . ? C5A N1A 1.52(2) 5_666 ? C5A C1A 1.95(3) 5_666 ? 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 O4 Ni1 N1 172.08(9) 2_656 . ? O4 Ni1 O2 94.20(9) 2_656 . ? N1 Ni1 O2 78.27(10) . . ? O4 Ni1 O3 95.71(9) 2_656 . ? N1 Ni1 O3 91.83(9) . . ? O2 Ni1 O3 170.09(9) . . ? O4 Ni1 N2 84.63(10) 2_656 . ? N1 Ni1 N2 93.91(11) . . ? O2 Ni1 N2 98.09(10) . . ? O3 Ni1 N2 82.98(10) . . ? O4 Ni1 O6 91.82(8) 2_656 2_656 ? N1 Ni1 O6 91.20(9) . 2_656 ? O2 Ni1 O6 94.16(8) . 2_656 ? O3 Ni1 O6 85.42(8) . 2_656 ? N2 Ni1 O6 167.46(10) . 2_656 ? N3 Ni2 O1 172.53(9) . . ? N3 Ni2 N4 94.51(11) . . ? O1 Ni2 N4 84.13(10) . . ? N3 Ni2 O6 90.77(9) . . ? O1 Ni2 O6 96.36(9) . . ? N4 Ni2 O6 83.27(10) . . ? N3 Ni2 O5 77.68(9) . . ? O1 Ni2 O5 95.07(9) . . ? N4 Ni2 O5 94.53(11) . . ? O6 Ni2 O5 168.07(8) . . ? N3 Ni2 O3 91.46(9) . . ? O1 Ni2 O3 91.46(8) . . ? N4 Ni2 O3 166.40(10) . . ? O6 Ni2 O3 84.45(8) . . ? O5 Ni2 O3 98.68(9) . . ? N1 O1 Ni2 117.07(17) . . ? C2 O2 Ni1 112.3(2) . . ? C5 O3 Ni1 107.01(17) . . ? C5 O3 Ni2 119.93(19) . . ? Ni1 O3 Ni2 108.17(9) . . ? C5 O3 H3 110(3) . . ? Ni1 O3 H3 106.0(18) . . ? Ni2 O3 H3 105.2(17) . . ? N3 O4 Ni1 118.58(17) . 2_656 ? C8 O5 Ni2 111.99(19) . . ? C11 O6 Ni2 105.77(17) . . ? C11 O6 Ni1 122.18(17) . 2_656 ? Ni2 O6 Ni1 108.39(9) . 2_656 ? C11 O6 H6 108(4) . . ? Ni2 O6 H6 102(4) . . ? Ni1 O6 H6 109(4) 2_656 . ? C1 N1 O1 119.2(3) . . ? C1 N1 Ni1 117.1(2) . . ? O1 N1 Ni1 123.69(19) . . ? C6 N2 Ni1 107.78(19) . . ? C6 N2 H2A 110.1 . . ? Ni1 N2 H2A 110.2 . . ? C6 N2 H2B 110.2 . . ? Ni1 N2 H2B 110.2 . . ? H2A N2 H2B 108.5 . . ? C7 N3 O4 118.0(2) . . ? C7 N3 Ni2 116.94(19) . . ? O4 N3 Ni2 124.85(19) . . ? C12 N4 Ni2 107.8(2) . . ? C12 N4 H4A 110.2 . . ? Ni2 N4 H4A 110.2 . . ? C12 N4 H4B 110.2 . . ? Ni2 N4 H4B 110.2 . . ? H4A N4 H4B 108.5 . . ? N1 C1 C2 111.8(3) . . ? N1 C1 C3 123.3(3) . . ? C2 C1 C3 124.9(3) . . ? O2 C2 C1 120.3(3) . . ? O2 C2 C4 119.3(3) . . ? C1 C2 C4 120.5(3) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4C 109.5 . . ? C2 C4 H4D 109.5 . . ? H4C C4 H4D 109.5 . . ? C2 C4 H4E 109.5 . . ? H4C C4 H4E 109.5 . . ? H4D C4 H4E 109.5 . . ? O3 C5 C6 108.3(3) . . ? O3 C5 H5A 110.0 . . ? C6 C5 H5A 110.0 . . ? O3 C5 H5B 110.0 . . ? C6 C5 H5B 110.0 . . ? H5A C5 H5B 108.4 . . ? N2 C6 C5 109.8(3) . . ? N2 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 . . ? N2 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? N3 C7 C8 112.8(3) . . ? N3 C7 C9 123.9(3) . . ? C8 C7 C9 123.2(3) . . ? O5 C8 C7 119.7(3) . . ? O5 C8 C10 120.8(3) . . ? C7 C8 C10 119.5(3) . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 C11 C12 109.2(3) . . ? O6 C11 H11A 109.8 . . ? C12 C11 H11A 109.8 . . ? O6 C11 H11B 109.8 . . ? C12 C11 H11B 109.8 . . ? H11A C11 H11B 108.3 . . ? N4 C12 C11 108.8(3) . . ? N4 C12 H12A 109.9 . . ? C11 C12 H12A 109.9 . . ? N4 C12 H12B 109.9 . . ? C11 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? O8 Cl1 O10 109.8(5) . . ? O8 Cl1 O9 108.1(4) . . ? O10 Cl1 O9 117.4(4) . . ? O8 Cl1 O7 110.0(6) . . ? O10 Cl1 O7 106.1(4) . . ? O9 Cl1 O7 105.2(5) . . ? O12 Cl2 O12 116.4(7) . 2_556 ? O12 Cl2 O11 105.9(3) . . ? O12 Cl2 O11 106.9(4) 2_556 . ? O12 Cl2 O11 106.9(4) . 2_556 ? O12 Cl2 O11 105.9(3) 2_556 2_556 ? O11 Cl2 O11 115.3(5) . 2_556 ? N1A N1A C3A 90.4(16) 5_666 5_666 ? N1A N1A C5A 76.8(13) 5_666 5_666 ? C3A N1A C5A 130.2(15) 5_666 5_666 ? N1A N1A C1A 102.6(16) 5_666 . ? C3A N1A C1A 57.2(13) 5_666 . ? C5A N1A C1A 78.7(12) 5_666 . ? N1A N1A C3A 55.3(14) 5_666 . ? C3A N1A C3A 145.7(8) 5_666 . ? C5A N1A C3A 48.8(11) 5_666 . ? C1A N1A C3A 124.6(13) . . ? N1A N1A C5A 70.2(15) 5_666 . ? C3A N1A C5A 51.7(13) 5_666 . ? C5A N1A C5A 147.0(7) 5_666 . ? C1A N1A C5A 108.2(12) . . ? C3A N1A C5A 108.6(13) . . ? N1A N1A C1A 51.3(12) 5_666 5_666 ? C3A N1A C1A 115.9(13) 5_666 5_666 ? C5A N1A C1A 93.1(10) 5_666 5_666 ? C1A N1A C1A 153.9(6) . 5_666 ? C3A N1A C1A 44.7(10) . 5_666 ? C5A N1A C1A 66.3(10) . 5_666 ? C3A C1A C2A 82.2(16) 5_666 . ? C3A C1A N1A 51.4(11) 5_666 . ? C2A C1A N1A 111.7(14) . . ? C3A C1A N1A 52.6(9) 5_666 5_666 ? C2A C1A N1A 87.4(12) . 5_666 ? N1A C1A N1A 26.1(6) . 5_666 ? C3A C1A C5A 98.1(11) 5_666 5_666 ? C2A C1A C5A 108.4(14) . 5_666 ? N1A C1A C5A 49.8(8) . 5_666 ? N1A C1A C5A 47.6(6) 5_666 5_666 ? C1A C2A C3A 47.4(11) . 5_666 ? C5A C3A N1A 76.0(13) 5_666 5_666 ? C5A C3A C1A 145.6(17) 5_666 5_666 ? N1A C3A C1A 71.4(13) 5_666 5_666 ? C5A C3A C4A 56.3(18) 5_666 . ? N1A C3A C4A 131(2) 5_666 . ? C1A C3A C4A 150(3) 5_666 . ? C5A C3A N1A 64.0(12) 5_666 . ? N1A C3A N1A 34.3(8) 5_666 . ? C1A C3A N1A 82.7(14) 5_666 . ? C4A C3A N1A 107(2) . . ? C5A C3A C2A 131(2) 5_666 5_666 ? N1A C3A C2A 103.2(16) 5_666 5_666 ? C1A C3A C2A 50.5(12) 5_666 5_666 ? C4A C3A C2A 101(2) . 5_666 ? N1A C3A C2A 87.5(13) . 5_666 ? C5A C4A C3A 55.9(16) 5_666 . ? C3A C5A C4A 67.8(16) 5_666 5_666 ? C3A C5A C6A 142(3) 5_666 . ? C4A C5A C6A 118(2) 5_666 . ? C3A C5A N1A 67.3(11) 5_666 5_666 ? C4A C5A N1A 117(2) 5_666 5_666 ? C6A C5A N1A 124(2) . 5_666 ? C3A C5A N1A 52.3(11) 5_666 . ? C4A C5A N1A 119.3(19) 5_666 . ? C6A C5A N1A 115(2) . . ? N1A C5A N1A 33.0(7) 5_666 . ? C3A C5A C1A 116.2(13) 5_666 5_666 ? C4A C5A C1A 154(2) 5_666 5_666 ? C6A C5A C1A 75.4(18) . 5_666 ? N1A C5A C1A 51.5(7) 5_666 5_666 ? N1A C5A C1A 66.1(9) . 5_666 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.627 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.086