Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_for #complex 1 _database_code_CSD 166398 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Ribas, Joan' 'Diaz, Carmen' 'Maestro, Miguel' 'Mahia, Jose' 'Tercero, Javier' _publ_contact_author_name 'Prof Joan Ribas' _publ_contact_author_address ; Inorganic Chemistry University of Barcelona Martí i Franqués 1-11 Barcelona 08028 SPAIN ; _publ_contact_author_email 'JOAN.RIBAS@QI.UB.ES' _publ_section_title ; Synthesis and characterization of [Cu(Me2oxpn)Ni(NO2)(tmen)] (ClO4): a single ferrimagnetic dinuclear CuII-NiII complex acting as weak molecule-based magnet ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H40 Cu N7 Ni O4, Cl O4' _chemical_formula_sum 'C18 H40 Cl Cu N7 Ni O8' _chemical_formula_weight 640.27 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.61560(10) _cell_length_b 17.9957(3) _cell_length_c 26.61340(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5563.02(11) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2680 _exptl_absorpt_coefficient_mu 1.590 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5347 _exptl_absorpt_correction_T_max 0.6061 _exptl_absorpt_process_details 'Sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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_% 0.73 _diffrn_reflns_number 36060 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 28.27 _reflns_number_total 6878 _reflns_number_gt 5471 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0349P)^2^+4.7130P] 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 6878 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0936 _refine_ls_wR_factor_gt 0.0858 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 Cu1 Cu 0.17102(3) 0.864605(17) 0.325524(11) 0.04016(9) Uani 1 1 d . . . Ni1 Ni 0.10232(3) 0.672600(16) 0.473748(11) 0.03344(8) Uani 1 1 d . . . Cl1 Cl 0.05214(7) 0.46389(5) 0.30216(3) 0.05984(19) Uani 1 1 d . . . O1 O 0.17012(17) 0.67376(9) 0.40183(7) 0.0445(4) Uani 1 1 d . . . O2 O 0.09868(15) 0.78422(9) 0.46161(6) 0.0389(4) Uani 1 1 d . . . O3 O 0.16384(19) 0.56365(10) 0.48329(8) 0.0535(5) Uani 1 1 d . . . O4 O 0.27355(18) 0.65202(12) 0.50094(8) 0.0583(5) Uani 1 1 d . . . O5 O 0.069(2) 0.3868(8) 0.3062(11) 0.184(12) Uani 0.349(16) 1 d P A 1 O6 O -0.066(2) 0.4770(17) 0.3120(8) 0.084(5) Uani 0.349(16) 1 d P A 1 O7 O 0.102(2) 0.5112(12) 0.2671(9) 0.183(12) Uani 0.349(16) 1 d P A 1 O8 O 0.1109(17) 0.4977(17) 0.3403(8) 0.170(11) Uani 0.349(16) 1 d P A 1 O5' O 0.0322(6) 0.3946(4) 0.2815(4) 0.119(3) Uani 0.651(16) 1 d P A 2 O6' O -0.0550(15) 0.4977(11) 0.3062(6) 0.130(6) Uani 0.651(16) 1 d P A 2 O7' O 0.1170(8) 0.4888(6) 0.2612(3) 0.115(3) Uani 0.651(16) 1 d P A 2 O8' O 0.1132(9) 0.4588(6) 0.3459(3) 0.112(4) Uani 0.651(16) 1 d P A 2 N1 N 0.2084(2) 0.85606(13) 0.25126(9) 0.0503(5) Uani 1 1 d . . . H1A H 0.1424 0.8642 0.2344 0.060 Uiso 1 1 calc R . . H1B H 0.2559 0.8939 0.2437 0.060 Uiso 1 1 calc R . . N2 N 0.1995(2) 0.75908(12) 0.33820(8) 0.0440(5) Uani 1 1 d . . . N3 N 0.1309(2) 0.97289(13) 0.31419(9) 0.0535(6) Uani 1 1 d . . . H3A H 0.1940 0.9948 0.3013 0.064 Uiso 1 1 calc R . . H3B H 0.0768 0.9741 0.2900 0.064 Uiso 1 1 calc R . . N4 N 0.1197(2) 0.86582(11) 0.39553(8) 0.0406(5) Uani 1 1 d . . . N5 N 0.2637(2) 0.58249(15) 0.49713(11) 0.0616(7) Uani 1 1 d . . . N6 N 0.02840(19) 0.67899(11) 0.54684(8) 0.0399(5) Uani 1 1 d . . . N7 N -0.06745(19) 0.65060(12) 0.44969(8) 0.0424(5) Uani 1 1 d . . . C1 C 0.2604(3) 0.78798(16) 0.23003(10) 0.0504(7) Uani 1 1 d . . . H1C H 0.3419 0.7879 0.2379 0.060 Uiso 1 1 calc R . . H1D H 0.2529 0.7896 0.1937 0.060 Uiso 1 1 calc R . . C2 C 0.2075(2) 0.71531(15) 0.24903(10) 0.0449(6) Uani 1 1 d . . . C3 C 0.2405(3) 0.70139(16) 0.30350(10) 0.0524(7) Uani 1 1 d . . . H3C H 0.2091 0.6538 0.3139 0.063 Uiso 1 1 calc R . . H3D H 0.3237 0.6983 0.3059 0.063 Uiso 1 1 calc R . . C4 C 0.2600(3) 0.65173(18) 0.21775(11) 0.0619(8) Uani 1 1 d . . . H4A H 0.2357 0.6048 0.2313 0.093 Uiso 1 1 calc R . . H4B H 0.3425 0.6549 0.2189 0.093 Uiso 1 1 calc R . . H4C H 0.2345 0.6558 0.1835 0.093 Uiso 1 1 calc R . . C5 C 0.0776(3) 0.7152(2) 0.24276(15) 0.0739(10) Uani 1 1 d . . . H5A H 0.0443 0.7524 0.2642 0.111 Uiso 1 1 calc R . . H5B H 0.0477 0.6673 0.2518 0.111 Uiso 1 1 calc R . . H5C H 0.0585 0.7258 0.2084 0.111 Uiso 1 1 calc R . . C6 C 0.0897(3) 1.02097(15) 0.35521(11) 0.0514(7) Uani 1 1 d . . . H6A H 0.0508 1.0635 0.3406 0.062 Uiso 1 1 calc R . . H6B H 0.1559 1.0395 0.3735 0.062 Uiso 1 1 calc R . . C7 C 0.0080(2) 0.98380(13) 0.39246(10) 0.0411(5) Uani 1 1 d . . . C8 C 0.0723(3) 0.92764(14) 0.42475(10) 0.0478(6) Uani 1 1 d . . . H8A H 0.1347 0.9527 0.4421 0.057 Uiso 1 1 calc R . . H8B H 0.0202 0.9081 0.4500 0.057 Uiso 1 1 calc R . . C9 C -0.0380(3) 1.04443(16) 0.42766(12) 0.0593(8) Uani 1 1 d . . . H9A H -0.0877 1.0224 0.4523 0.089 Uiso 1 1 calc R . . H9B H -0.0803 1.0804 0.4085 0.089 Uiso 1 1 calc R . . H9C H 0.0253 1.0684 0.4442 0.089 Uiso 1 1 calc R . . C10 C -0.0927(3) 0.94676(19) 0.36563(12) 0.0608(8) Uani 1 1 d . . . H10A H -0.0642 0.9088 0.3436 0.091 Uiso 1 1 calc R . . H10B H -0.1339 0.9832 0.3464 0.091 Uiso 1 1 calc R . . H10C H -0.1434 0.9250 0.3900 0.091 Uiso 1 1 calc R . . C11 C 0.1693(2) 0.73826(13) 0.38351(9) 0.0371(5) Uani 1 1 d . . . C12 C 0.1260(2) 0.80082(13) 0.41709(9) 0.0355(5) Uani 1 1 d . . . C13 C -0.0795(3) 0.6366(2) 0.54157(12) 0.0649(9) Uani 1 1 d . . . H13A H -0.1286 0.6464 0.5703 0.078 Uiso 1 1 calc R . . H13B H -0.0621 0.5838 0.5412 0.078 Uiso 1 1 calc R . . C14 C -0.1416(3) 0.6565(2) 0.49493(12) 0.0617(8) Uani 1 1 d . . . H14A H -0.1701 0.7069 0.4978 0.074 Uiso 1 1 calc R . . H14B H -0.2074 0.6238 0.4910 0.074 Uiso 1 1 calc R . . C15 C 0.0085(4) 0.75580(17) 0.56260(12) 0.0690(10) Uani 1 1 d . . . H15A H -0.0349 0.7562 0.5933 0.104 Uiso 1 1 calc R . . H15B H -0.0337 0.7816 0.5370 0.104 Uiso 1 1 calc R . . H15C H 0.0811 0.7801 0.5679 0.104 Uiso 1 1 calc R . . C16 C 0.0966(3) 0.64277(19) 0.58709(11) 0.0645(9) Uani 1 1 d . . . H16A H 0.0561 0.6467 0.6184 0.097 Uiso 1 1 calc R . . H16B H 0.1700 0.6668 0.5899 0.097 Uiso 1 1 calc R . . H16C H 0.1077 0.5913 0.5790 0.097 Uiso 1 1 calc R . . C17 C -0.0711(3) 0.57464(19) 0.42891(15) 0.0748(10) Uani 1 1 d . . . H17A H -0.1478 0.5637 0.4176 0.112 Uiso 1 1 calc R . . H17B H -0.0492 0.5397 0.4544 0.112 Uiso 1 1 calc R . . H17C H -0.0188 0.5710 0.4011 0.112 Uiso 1 1 calc R . . C18 C -0.1116(3) 0.7028(2) 0.41161(13) 0.0687(9) Uani 1 1 d . . . H18A H -0.1907 0.6915 0.4045 0.103 Uiso 1 1 calc R . . H18B H -0.0670 0.6983 0.3814 0.103 Uiso 1 1 calc R . . H18C H -0.1059 0.7527 0.4241 0.103 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.04647(18) 0.03548(16) 0.03853(16) 0.00957(12) 0.00550(13) 0.00488(13) Ni1 0.03851(16) 0.02718(14) 0.03462(15) 0.00463(12) 0.00223(12) 0.00184(12) Cl1 0.0673(5) 0.0624(5) 0.0498(4) -0.0054(3) -0.0037(3) -0.0096(4) O1 0.0622(12) 0.0310(8) 0.0402(9) 0.0067(7) 0.0105(8) 0.0077(8) O2 0.0552(11) 0.0294(8) 0.0322(8) 0.0039(6) 0.0019(7) 0.0001(7) O3 0.0650(14) 0.0343(9) 0.0611(12) 0.0078(8) 0.0056(10) 0.0063(9) O4 0.0445(11) 0.0601(13) 0.0704(14) 0.0100(11) -0.0020(10) -0.0018(9) O5 0.212(19) 0.062(7) 0.28(2) 0.068(11) 0.193(17) 0.049(10) O6 0.073(8) 0.107(13) 0.070(7) 0.002(7) -0.019(5) -0.004(8) O7 0.26(2) 0.114(12) 0.178(17) 0.068(11) 0.030(15) -0.111(15) O8 0.071(8) 0.28(3) 0.160(16) -0.163(16) -0.002(10) -0.021(13) O5' 0.072(3) 0.089(5) 0.196(7) -0.076(5) -0.028(4) -0.003(3) O6' 0.108(9) 0.129(11) 0.152(10) -0.039(7) -0.014(7) 0.050(7) O7' 0.123(5) 0.149(7) 0.073(4) 0.059(4) 0.020(3) 0.051(5) O8' 0.095(4) 0.191(10) 0.050(3) 0.033(5) -0.024(3) -0.029(6) N1 0.0579(14) 0.0470(12) 0.0459(12) 0.0098(10) 0.0071(11) 0.0040(11) N2 0.0584(13) 0.0362(11) 0.0375(11) 0.0083(9) 0.0113(10) 0.0121(10) N3 0.0627(15) 0.0440(13) 0.0538(14) 0.0170(11) 0.0140(11) 0.0093(11) N4 0.0569(13) 0.0288(10) 0.0361(10) 0.0056(8) 0.0032(9) 0.0045(9) N5 0.0533(16) 0.0602(17) 0.0713(17) 0.0151(13) 0.0046(13) 0.0190(13) N6 0.0465(12) 0.0365(11) 0.0367(10) 0.0028(8) 0.0039(9) 0.0000(9) N7 0.0441(12) 0.0405(11) 0.0427(11) -0.0042(9) -0.0017(9) -0.0013(9) C1 0.0539(16) 0.0540(16) 0.0432(14) 0.0029(12) 0.0143(12) -0.0002(13) C2 0.0433(14) 0.0463(14) 0.0452(13) 0.0015(12) 0.0099(11) 0.0014(11) C3 0.0648(19) 0.0471(15) 0.0452(14) 0.0037(12) 0.0141(13) 0.0189(14) C4 0.076(2) 0.0580(18) 0.0520(17) -0.0079(14) 0.0185(16) -0.0023(16) C5 0.0486(18) 0.076(2) 0.097(3) -0.002(2) 0.0003(18) -0.0083(16) C6 0.0600(18) 0.0335(13) 0.0607(17) 0.0092(12) 0.0089(14) 0.0021(12) C7 0.0479(14) 0.0306(11) 0.0447(13) 0.0015(10) 0.0030(11) 0.0024(10) C8 0.0722(19) 0.0320(12) 0.0391(13) 0.0001(10) -0.0004(13) 0.0051(12) C9 0.079(2) 0.0397(15) 0.0595(17) -0.0023(13) 0.0083(16) 0.0144(14) C10 0.0487(17) 0.070(2) 0.0634(19) -0.0047(16) 0.0025(14) -0.0025(15) C11 0.0388(12) 0.0325(12) 0.0401(12) 0.0044(10) 0.0015(10) 0.0053(9) C12 0.0389(12) 0.0309(11) 0.0368(12) 0.0021(9) 0.0013(10) -0.0009(9) C13 0.0574(19) 0.082(2) 0.0550(17) 0.0021(17) 0.0136(15) -0.0121(17) C14 0.0416(16) 0.081(2) 0.0621(19) -0.0021(17) 0.0038(14) -0.0005(15) C15 0.109(3) 0.0465(16) 0.0516(17) -0.0049(14) 0.0173(18) 0.0099(18) C16 0.083(2) 0.068(2) 0.0418(15) 0.0134(14) 0.0019(15) 0.0113(18) C17 0.071(2) 0.0550(19) 0.099(3) -0.0311(19) -0.006(2) -0.0089(16) C18 0.0584(19) 0.081(2) 0.067(2) 0.0132(18) -0.0250(16) -0.0029(17) _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 Cu1 N4 1.956(2) . ? Cu1 N2 1.957(2) . ? Cu1 N3 2.026(2) . ? Cu1 N1 2.029(2) . ? Ni1 O2 2.0349(16) . ? Ni1 O1 2.0697(17) . ? Ni1 O3 2.1021(18) . ? Ni1 N7 2.111(2) . ? Ni1 N6 2.129(2) . ? Ni1 O4 2.149(2) . ? Cl1 O8' 1.366(7) . ? Cl1 O8 1.366(16) . ? Cl1 O5' 1.382(6) . ? Cl1 O7 1.387(15) . ? Cl1 O6' 1.389(17) . ? Cl1 O7' 1.398(8) . ? Cl1 O5 1.407(13) . ? Cl1 O6 1.41(3) . ? O1 C11 1.259(3) . ? O2 C12 1.262(3) . ? O3 N5 1.264(3) . ? O4 N5 1.260(3) . ? N1 C1 1.478(3) . ? N2 C11 1.311(3) . ? N2 C3 1.469(3) . ? N3 C6 1.473(4) . ? N4 C12 1.305(3) . ? N4 C8 1.465(3) . ? N6 C15 1.463(4) . ? N6 C13 1.474(4) . ? N6 C16 1.483(4) . ? N7 C18 1.474(4) . ? N7 C17 1.475(4) . ? N7 C14 1.484(4) . ? C1 C2 1.531(4) . ? C2 C5 1.519(4) . ? C2 C3 1.520(4) . ? C2 C4 1.541(4) . ? C6 C7 1.527(4) . ? C7 C8 1.522(3) . ? C7 C10 1.524(4) . ? C7 C9 1.534(4) . ? C11 C12 1.523(3) . ? C13 C14 1.479(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 N4 Cu1 N2 84.16(8) . . ? N4 Cu1 N3 93.49(9) . . ? N2 Cu1 N3 176.22(10) . . ? N4 Cu1 N1 173.47(10) . . ? N2 Cu1 N1 93.33(9) . . ? N3 Cu1 N1 88.69(9) . . ? O2 Ni1 O1 81.44(6) . . ? O2 Ni1 O3 161.24(8) . . ? O1 Ni1 O3 89.53(7) . . ? O2 Ni1 N7 96.75(8) . . ? O1 Ni1 N7 94.41(8) . . ? O3 Ni1 N7 100.33(9) . . ? O2 Ni1 N6 94.78(7) . . ? O1 Ni1 N6 176.05(7) . . ? O3 Ni1 N6 94.42(8) . . ? N7 Ni1 N6 84.87(8) . . ? O2 Ni1 O4 104.06(8) . . ? O1 Ni1 O4 87.76(8) . . ? O3 Ni1 O4 58.93(8) . . ? N7 Ni1 O4 159.17(8) . . ? N6 Ni1 O4 94.30(8) . . ? O8' Cl1 O8 30.3(14) . . ? O8' Cl1 O5' 111.5(5) . . ? O8 Cl1 O5' 141.3(13) . . ? O8' Cl1 O7 113.5(11) . . ? O8 Cl1 O7 91.1(17) . . ? O5' Cl1 O7 110.8(13) . . ? O8' Cl1 O6' 115.4(9) . . ? O8 Cl1 O6' 101.3(12) . . ? O5' Cl1 O6' 106.0(8) . . ? O7 Cl1 O6' 98.9(13) . . ? O8' Cl1 O7' 113.9(6) . . ? O8 Cl1 O7' 99.6(13) . . ? O5' Cl1 O7' 94.0(7) . . ? O7 Cl1 O7' 19.4(14) . . ? O6' Cl1 O7' 113.8(8) . . ? O8' Cl1 O5 78.2(13) . . ? O8 Cl1 O5 108.1(13) . . ? O5' Cl1 O5 33.3(13) . . ? O7 Cl1 O5 126.7(14) . . ? O6' Cl1 O5 123.6(10) . . ? O7' Cl1 O5 107.4(7) . . ? O8' Cl1 O6 110.9(10) . . ? O8 Cl1 O6 105.8(13) . . ? O5' Cl1 O6 93.6(12) . . ? O7 Cl1 O6 115.0(15) . . ? O6' Cl1 O6 17.3(17) . . ? O7' Cl1 O6 127.8(10) . . ? O5 Cl1 O6 106.8(14) . . ? C11 O1 Ni1 111.38(15) . . ? C12 O2 Ni1 112.17(15) . . ? N5 O3 Ni1 95.58(16) . . ? N5 O4 Ni1 93.46(17) . . ? C1 N1 Cu1 121.49(17) . . ? C11 N2 C3 117.6(2) . . ? C11 N2 Cu1 113.00(16) . . ? C3 N2 Cu1 129.23(16) . . ? C6 N3 Cu1 121.96(17) . . ? C12 N4 C8 117.9(2) . . ? C12 N4 Cu1 113.05(16) . . ? C8 N4 Cu1 128.95(16) . . ? O4 N5 O3 111.9(2) . . ? C15 N6 C13 112.5(3) . . ? C15 N6 C16 107.0(2) . . ? C13 N6 C16 107.2(2) . . ? C15 N6 Ni1 112.12(17) . . ? C13 N6 Ni1 103.18(17) . . ? C16 N6 Ni1 114.89(18) . . ? C18 N7 C17 108.8(3) . . ? C18 N7 C14 108.1(2) . . ? C17 N7 C14 110.7(3) . . ? C18 N7 Ni1 114.45(18) . . ? C17 N7 Ni1 108.34(19) . . ? C14 N7 Ni1 106.43(17) . . ? N1 C1 C2 114.7(2) . . ? C5 C2 C3 110.8(3) . . ? C5 C2 C1 111.3(3) . . ? C3 C2 C1 110.8(2) . . ? C5 C2 C4 109.4(3) . . ? C3 C2 C4 107.1(2) . . ? C1 C2 C4 107.3(2) . . ? N2 C3 C2 113.7(2) . . ? N3 C6 C7 115.2(2) . . ? C8 C7 C10 110.5(2) . . ? C8 C7 C6 110.7(2) . . ? C10 C7 C6 111.4(2) . . ? C8 C7 C9 107.4(2) . . ? C10 C7 C9 109.2(2) . . ? C6 C7 C9 107.5(2) . . ? N4 C8 C7 112.9(2) . . ? O1 C11 N2 128.2(2) . . ? O1 C11 C12 117.2(2) . . ? N2 C11 C12 114.6(2) . . ? O2 C12 N4 127.6(2) . . ? O2 C12 C11 117.3(2) . . ? N4 C12 C11 115.0(2) . . ? N6 C13 C14 111.6(3) . . ? C13 C14 N7 112.4(3) . . ? 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 O1 C11 -4.90(17) . . . . ? O3 Ni1 O1 C11 -168.40(18) . . . . ? N7 Ni1 O1 C11 91.28(18) . . . . ? N6 Ni1 O1 C11 12.0(13) . . . . ? O4 Ni1 O1 C11 -109.48(18) . . . . ? O1 Ni1 O2 C12 6.56(17) . . . . ? O3 Ni1 O2 C12 68.6(3) . . . . ? N7 Ni1 O2 C12 -86.91(17) . . . . ? N6 Ni1 O2 C12 -172.29(17) . . . . ? O4 Ni1 O2 C12 92.06(17) . . . . ? O2 Ni1 O3 N5 24.4(3) . . . . ? O1 Ni1 O3 N5 85.29(17) . . . . ? N7 Ni1 O3 N5 179.68(17) . . . . ? N6 Ni1 O3 N5 -94.74(17) . . . . ? O4 Ni1 O3 N5 -2.38(16) . . . . ? O2 Ni1 O4 N5 -169.01(16) . . . . ? O1 Ni1 O4 N5 -88.41(17) . . . . ? O3 Ni1 O4 N5 2.38(16) . . . . ? N7 Ni1 O4 N5 8.1(3) . . . . ? N6 Ni1 O4 N5 94.96(17) . . . . ? N4 Cu1 N1 C1 -77.4(8) . . . . ? N2 Cu1 N1 C1 -10.2(2) . . . . ? N3 Cu1 N1 C1 173.0(2) . . . . ? N4 Cu1 N2 C11 2.39(19) . . . . ? N3 Cu1 N2 C11 -49.3(16) . . . . ? N1 Cu1 N2 C11 -171.6(2) . . . . ? N4 Cu1 N2 C3 177.3(3) . . . . ? N3 Cu1 N2 C3 125.7(15) . . . . ? N1 Cu1 N2 C3 3.4(3) . . . . ? N4 Cu1 N3 C6 4.9(2) . . . . ? N2 Cu1 N3 C6 56.4(16) . . . . ? N1 Cu1 N3 C6 178.8(2) . . . . ? N2 Cu1 N4 C12 -0.61(19) . . . . ? N3 Cu1 N4 C12 176.4(2) . . . . ? N1 Cu1 N4 C12 67.1(8) . . . . ? N2 Cu1 N4 C8 -177.8(3) . . . . ? N3 Cu1 N4 C8 -0.8(3) . . . . ? N1 Cu1 N4 C8 -110.2(8) . . . . ? Ni1 O4 N5 O3 -3.7(2) . . . . ? Ni1 O3 N5 O4 3.8(3) . . . . ? O2 Ni1 N6 C15 -3.0(2) . . . . ? O1 Ni1 N6 C15 -19.8(13) . . . . ? O3 Ni1 N6 C15 160.6(2) . . . . ? N7 Ni1 N6 C15 -99.4(2) . . . . ? O4 Ni1 N6 C15 101.5(2) . . . . ? O2 Ni1 N6 C13 118.26(19) . . . . ? O1 Ni1 N6 C13 101.5(12) . . . . ? O3 Ni1 N6 C13 -78.10(19) . . . . ? N7 Ni1 N6 C13 21.90(19) . . . . ? O4 Ni1 N6 C13 -137.22(19) . . . . ? O2 Ni1 N6 C16 -125.5(2) . . . . ? O1 Ni1 N6 C16 -142.3(11) . . . . ? O3 Ni1 N6 C16 38.2(2) . . . . ? N7 Ni1 N6 C16 138.2(2) . . . . ? O4 Ni1 N6 C16 -21.0(2) . . . . ? O2 Ni1 N7 C18 28.5(2) . . . . ? O1 Ni1 N7 C18 -53.4(2) . . . . ? O3 Ni1 N7 C18 -143.7(2) . . . . ? N6 Ni1 N7 C18 122.7(2) . . . . ? O4 Ni1 N7 C18 -148.7(3) . . . . ? O2 Ni1 N7 C17 150.1(2) . . . . ? O1 Ni1 N7 C17 68.3(2) . . . . ? O3 Ni1 N7 C17 -22.1(2) . . . . ? N6 Ni1 N7 C17 -115.6(2) . . . . ? O4 Ni1 N7 C17 -27.0(4) . . . . ? O2 Ni1 N7 C14 -90.81(19) . . . . ? O1 Ni1 N7 C14 -172.69(19) . . . . ? O3 Ni1 N7 C14 96.98(19) . . . . ? N6 Ni1 N7 C14 3.41(19) . . . . ? O4 Ni1 N7 C14 92.0(3) . . . . ? Cu1 N1 C1 C2 43.6(3) . . . . ? N1 C1 C2 C5 52.5(3) . . . . ? N1 C1 C2 C3 -71.2(3) . . . . ? N1 C1 C2 C4 172.2(3) . . . . ? C11 N2 C3 C2 145.8(3) . . . . ? Cu1 N2 C3 C2 -28.9(4) . . . . ? C5 C2 C3 N2 -62.6(3) . . . . ? C1 C2 C3 N2 61.5(3) . . . . ? C4 C2 C3 N2 178.2(3) . . . . ? Cu1 N3 C6 C7 -38.5(3) . . . . ? N3 C6 C7 C8 70.6(3) . . . . ? N3 C6 C7 C10 -52.7(3) . . . . ? N3 C6 C7 C9 -172.4(3) . . . . ? C12 N4 C8 C7 -147.8(2) . . . . ? Cu1 N4 C8 C7 29.3(4) . . . . ? C10 C7 C8 N4 60.2(3) . . . . ? C6 C7 C8 N4 -63.7(3) . . . . ? C9 C7 C8 N4 179.2(2) . . . . ? Ni1 O1 C11 N2 -175.9(2) . . . . ? Ni1 O1 C11 C12 2.7(3) . . . . ? C3 N2 C11 O1 -0.4(4) . . . . ? Cu1 N2 C11 O1 175.2(2) . . . . ? C3 N2 C11 C12 -179.1(2) . . . . ? Cu1 N2 C11 C12 -3.5(3) . . . . ? Ni1 O2 C12 N4 171.5(2) . . . . ? Ni1 O2 C12 C11 -7.1(3) . . . . ? C8 N4 C12 O2 -2.1(4) . . . . ? Cu1 N4 C12 O2 -179.6(2) . . . . ? C8 N4 C12 C11 176.5(2) . . . . ? Cu1 N4 C12 C11 -1.1(3) . . . . ? O1 C11 C12 O2 3.0(3) . . . . ? N2 C11 C12 O2 -178.1(2) . . . . ? O1 C11 C12 N4 -175.7(2) . . . . ? N2 C11 C12 N4 3.1(3) . . . . ? C15 N6 C13 C14 76.1(3) . . . . ? C16 N6 C13 C14 -166.6(3) . . . . ? Ni1 N6 C13 C14 -44.9(3) . . . . ? N6 C13 C14 N7 52.8(4) . . . . ? C18 N7 C14 C13 -152.9(3) . . . . ? C17 N7 C14 C13 88.0(3) . . . . ? Ni1 N7 C14 C13 -29.5(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 N1 H1A O5' 0.90 2.14 3.009(6) 161.0 3 N1 H1A O5 0.90 2.72 3.61(3) 173.4 3 N1 H1A O6 0.90 2.54 3.21(2) 132.2 3 N1 H1A O6' 0.90 2.82 3.465(18) 129.4 3 N1 H1B O7' 0.90 2.30 3.144(9) 155.3 8_665 N1 H1B O7 0.90 2.75 3.58(3) 154.0 8_665 N1 H1B O5' 0.90 2.66 3.195(8) 119.1 8_665 N1 H1B O5 0.90 2.63 3.018(14) 107.1 8_665 N3 H3A O7 0.90 2.56 3.42(3) 160.3 8_665 N3 H3A O7' 0.90 2.44 3.262(9) 151.5 8_665 N3 H3A O8' 0.90 2.61 3.100(11) 114.7 8_665 N3 H3A O8 0.90 2.49 3.11(2) 126.3 8_665 N3 H3B O6' 0.90 2.61 3.352(16) 140.7 3 N3 H3B O6 0.90 2.72 3.44(2) 138.4 3 N3 H3B O7' 0.90 2.65 3.522(10) 164.9 3 N3 H3B O7 0.90 2.66 3.53(3) 163.8 3 N3 H3B Cl1 0.90 2.88 3.759(3) 166.2 3 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.662 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.057