#------------------------------------------------------------------------------ #$Date: 2008-01-26 19:25:03 +0200 (Sat, 26 Jan 2008) $ #$Revision: 20 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100157.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100157 _journal_name_full 'Polyhedron' _journal_volume 23 _journal_page_first 1505 _journal_page_last 1518 _journal_year 2004 _publ_section_title ; 'Solid state coordination chemistry of mononuclear mixed-ligand complexes of Ni(II), Cu(II) and Zn(II) with \a-hydroxycarboxylic acids and imidazole' ; loop_ _publ_author_name 'Carballo, Rosa' 'Vazquez-Lopez, Ezequiel M.' 'Covelo, Berta' 'Garcia-Martinez, Emilia' 'Castineiras, Alfonso' 'Niclos, Juan' _chemical_formula_sum 'C37 H34 N6 Ni O6' _chemical_formula_weight 717.41 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' '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.2191(11) _cell_length_b 29.972(4) _cell_length_c 12.5644(15) _cell_angle_alpha 90.00 _cell_angle_beta 94.428(3) _cell_angle_gamma 90.00 _cell_volume 3461.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 684 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 26.88 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.616 _exptl_absorpt_correction_type MULTISCAN _exptl_absorpt_correction_T_min 0.8782 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_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 '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 18394 _diffrn_reflns_av_R_equivalents 0.0885 _diffrn_reflns_av_sigmaI/netI 0.1784 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 28.07 _reflns_number_total 7653 _reflns_number_gt 3567 _reflns_threshold_expression >2sigma(I) _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^)+(0.0672P)^2^+0.8395P] 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 7653 _refine_ls_number_parameters 468 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2271 _refine_ls_R_factor_gt 0.1056 _refine_ls_wR_factor_ref 0.2022 _refine_ls_wR_factor_gt 0.1633 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 Ni Ni 0.33844(8) 0.14851(2) 0.50942(6) 0.0372(2) Uani 1 1 d . . . O11 O 0.5421(4) 0.15643(12) 0.4605(3) 0.0402(10) Uani 1 1 d . . . O12 O 0.6853(4) 0.19225(13) 0.3574(3) 0.0494(12) Uani 1 1 d . . . O13 O 0.2997(4) 0.19112(13) 0.3740(3) 0.0381(10) Uani 1 1 d . . . C101 C 0.5641(6) 0.18459(19) 0.3894(5) 0.0373(15) Uani 1 1 d . . . C102 C 0.4291(6) 0.21106(18) 0.3381(5) 0.0371(14) Uani 1 1 d . . . C103 C 0.4327(6) 0.25950(18) 0.3773(5) 0.0396(15) Uani 1 1 d . . . C104 C 0.5579(7) 0.2838(2) 0.3863(6) 0.064(2) Uani 1 1 d . . . H104 H 0.6446 0.2700 0.3719 0.077 Uiso 1 1 calc R . . C105 C 0.5606(9) 0.3283(2) 0.4161(7) 0.087(3) Uani 1 1 d . . . H105 H 0.6475 0.3442 0.4202 0.105 Uiso 1 1 calc R . . C106 C 0.4357(10) 0.3483(2) 0.4390(8) 0.093(3) Uani 1 1 d . . . H106 H 0.4364 0.3779 0.4610 0.112 Uiso 1 1 calc R . . C107 C 0.3099(9) 0.3251(3) 0.4301(10) 0.127(4) Uani 1 1 d . . . H107 H 0.2236 0.3389 0.4454 0.152 Uiso 1 1 calc R . . C108 C 0.3081(7) 0.2812(2) 0.3984(8) 0.088(3) Uani 1 1 d . . . H108 H 0.2200 0.2659 0.3912 0.106 Uiso 1 1 calc R . . C109 C 0.4293(6) 0.20746(19) 0.2174(5) 0.0376(14) Uani 1 1 d . . . C110 C 0.3895(6) 0.2428(2) 0.1509(6) 0.0491(17) Uani 1 1 d . . . H110 H 0.3627 0.2700 0.1793 0.059 Uiso 1 1 calc R . . C111 C 0.3901(7) 0.2375(2) 0.0416(6) 0.060(2) Uani 1 1 d . . . H111 H 0.3640 0.2614 -0.0028 0.072 Uiso 1 1 calc R . . C112 C 0.4278(7) 0.1980(3) -0.0029(6) 0.064(2) Uani 1 1 d . . . H112 H 0.4281 0.1951 -0.0765 0.077 Uiso 1 1 calc R . . C113 C 0.4652(7) 0.1630(2) 0.0634(6) 0.061(2) Uani 1 1 d . . . H113 H 0.4917 0.1359 0.0347 0.073 Uiso 1 1 calc R . . C114 C 0.4637(7) 0.1677(2) 0.1722(5) 0.0530(18) Uani 1 1 d . . . H114 H 0.4866 0.1433 0.2160 0.064 Uiso 1 1 calc R . . O21 O 0.3046(4) 0.09236(12) 0.4032(3) 0.0477(11) Uani 1 1 d . . . O22 O 0.1791(4) 0.12654(13) 0.2669(3) 0.0478(11) Uani 1 1 d . . . O23 O 0.2272(5) 0.01446(13) 0.3532(3) 0.0563(12) Uani 1 1 d . . . H23 H 0.2564 0.0265 0.4094 0.084 Uiso 1 1 calc R . . C201 C 0.2194(6) 0.0925(2) 0.3189(5) 0.0399(15) Uani 1 1 d . . . C202 C 0.1576(6) 0.04702(19) 0.2827(5) 0.0414(15) Uani 1 1 d . . . C203 C -0.0066(7) 0.0465(2) 0.2940(5) 0.0459(16) Uani 1 1 d . . . C204 C -0.0707(9) 0.0154(3) 0.3544(6) 0.079(2) Uani 1 1 d . . . H204 H -0.0145 -0.0065 0.3902 0.095 Uiso 1 1 calc R . . C205 C -0.2219(11) 0.0166(4) 0.3623(8) 0.122(4) Uani 1 1 d . . . H205 H -0.2647 -0.0047 0.4036 0.147 Uiso 1 1 calc R . . C206 C -0.3057(11) 0.0476(5) 0.3120(9) 0.128(5) Uani 1 1 d . . . H206 H -0.4049 0.0486 0.3206 0.154 Uiso 1 1 calc R . . C207 C -0.2439(9) 0.0775(3) 0.2481(9) 0.097(3) Uani 1 1 d . . . H207 H -0.3022 0.0983 0.2100 0.117 Uiso 1 1 calc R . . C208 C -0.0966(8) 0.0775(2) 0.2391(6) 0.067(2) Uani 1 1 d . . . H208 H -0.0561 0.0985 0.1957 0.080 Uiso 1 1 calc R . . C209 C 0.1908(7) 0.0345(2) 0.1695(5) 0.0499(17) Uani 1 1 d . . . C210 C 0.1550(9) -0.0053(3) 0.1289(6) 0.075(2) Uani 1 1 d . . . H210 H 0.1050 -0.0249 0.1701 0.090 Uiso 1 1 calc R . . C211 C 0.1883(10) -0.0190(3) 0.0285(7) 0.080(2) Uani 1 1 d . . . H211 H 0.1637 -0.0476 0.0050 0.096 Uiso 1 1 calc R . . C212 C 0.2536(13) 0.0079(4) -0.0330(8) 0.129(4) Uani 1 1 d . . . H212 H 0.2773 -0.0009 -0.1004 0.155 Uiso 1 1 calc R . . C213 C 0.285(2) 0.0481(5) 0.0032(11) 0.271(12) Uani 1 1 d . . . H213 H 0.3291 0.0682 -0.0404 0.325 Uiso 1 1 calc R . . C214 C 0.2542(16) 0.0613(4) 0.1045(10) 0.216(9) Uani 1 1 d . . . H214 H 0.2792 0.0900 0.1273 0.260 Uiso 1 1 calc R . . N1 N 0.3685(5) 0.20248(16) 0.6095(4) 0.0429(13) Uani 1 1 d . . . N2 N 0.3251(7) 0.26150(19) 0.7049(5) 0.0606(17) Uani 1 1 d . . . C2 C 0.4956(7) 0.2226(3) 0.6435(6) 0.067(2) Uani 1 1 d . . . H2 H 0.5877 0.2128 0.6288 0.080 Uiso 1 1 calc R . . C3 C 0.4686(8) 0.2588(3) 0.7014(6) 0.074(2) Uani 1 1 d . . . H3 H 0.5373 0.2784 0.7331 0.089 Uiso 1 1 calc R . . C1 C 0.2689(7) 0.2268(2) 0.6500(6) 0.0555(18) Uani 1 1 d . . . H1 H 0.1698 0.2206 0.6414 0.067 Uiso 1 1 calc R . . N3 N 0.4241(5) 0.10459(16) 0.6235(4) 0.0421(13) Uani 1 1 d . . . N4 N 0.5741(6) 0.0534(2) 0.6884(5) 0.0534(15) Uani 1 1 d . . . C5 C 0.4241(8) 0.1038(2) 0.7315(6) 0.066(2) Uani 1 1 d . . . H5 H 0.3675 0.1222 0.7713 0.079 Uiso 1 1 calc R . . C6 C 0.5169(8) 0.0730(3) 0.7726(6) 0.075(2) Uani 1 1 d . . . H6 H 0.5379 0.0663 0.8444 0.090 Uiso 1 1 calc R . . C4 C 0.5158(6) 0.0732(2) 0.6005(5) 0.0484(17) Uani 1 1 d . . . H4 H 0.5372 0.0657 0.5316 0.058 Uiso 1 1 calc R . . N5 N 0.1198(5) 0.14080(16) 0.5347(4) 0.0436(13) Uani 1 1 d . . . N6 N -0.1164(7) 0.1415(2) 0.5085(6) 0.066(2) Uani 1 1 d . . . C8 C 0.0592(8) 0.1199(3) 0.6150(7) 0.107(4) Uani 1 1 d . . . H8 H 0.1109 0.1069 0.6735 0.129 Uiso 1 1 calc R . . C9 C -0.0863(8) 0.1203(3) 0.5985(9) 0.127(4) Uani 1 1 d . . . H9 H -0.1526 0.1080 0.6424 0.153 Uiso 1 1 calc R . . C7 C 0.0071(8) 0.1537(2) 0.4726(6) 0.0582(19) Uani 1 1 d . . . H7 H 0.0140 0.1698 0.4099 0.070 Uiso 1 1 calc R . . H60 H -0.190(7) 0.145(2) 0.470(6) 0.07(2) Uiso 1 1 d . . . H13 H 0.270(7) 0.171(2) 0.326(6) 0.08(3) Uiso 1 1 d . . . H20 H 0.272(8) 0.280(3) 0.755(6) 0.10(3) Uiso 1 1 d . . . H40 H 0.639(6) 0.031(2) 0.686(5) 0.05(2) 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 Ni 0.0375(4) 0.0374(4) 0.0360(5) 0.0001(4) -0.0030(3) 0.0060(4) O11 0.036(2) 0.041(2) 0.043(3) 0.008(2) 0.0015(19) 0.0087(18) O12 0.023(2) 0.057(3) 0.067(3) 0.018(2) -0.001(2) 0.0044(19) O13 0.033(2) 0.037(2) 0.044(3) -0.002(2) -0.001(2) -0.0003(18) C101 0.039(4) 0.033(3) 0.038(4) -0.008(3) -0.009(3) 0.001(3) C102 0.034(3) 0.032(3) 0.045(4) 0.005(3) -0.001(3) 0.004(3) C103 0.039(4) 0.032(3) 0.046(4) 0.000(3) -0.007(3) 0.003(3) C104 0.045(4) 0.045(4) 0.101(6) -0.018(4) -0.004(4) 0.004(3) C105 0.060(5) 0.052(5) 0.149(9) -0.026(5) -0.007(5) -0.005(4) C106 0.087(6) 0.041(4) 0.156(9) -0.028(5) 0.036(6) -0.008(5) C107 0.069(6) 0.061(6) 0.258(14) -0.034(7) 0.066(8) 0.001(5) C108 0.039(4) 0.045(4) 0.182(10) -0.021(5) 0.015(5) 0.006(3) C109 0.026(3) 0.038(3) 0.049(4) 0.008(3) -0.002(3) -0.002(3) C110 0.041(4) 0.049(4) 0.054(5) 0.008(3) -0.016(3) -0.001(3) C111 0.059(5) 0.061(5) 0.056(5) 0.024(4) -0.022(4) -0.009(4) C112 0.046(4) 0.107(7) 0.040(5) 0.007(5) -0.002(4) -0.019(4) C113 0.057(5) 0.064(5) 0.061(5) -0.001(4) 0.005(4) 0.003(4) C114 0.060(5) 0.059(4) 0.040(4) 0.011(3) 0.003(4) 0.012(3) O21 0.053(3) 0.042(3) 0.046(3) -0.006(2) -0.012(2) 0.004(2) O22 0.064(3) 0.036(2) 0.042(3) 0.002(2) -0.005(2) -0.003(2) O23 0.072(3) 0.040(2) 0.054(3) 0.003(2) -0.013(3) 0.015(2) C201 0.033(3) 0.048(4) 0.039(4) -0.002(3) 0.006(3) 0.000(3) C202 0.050(4) 0.038(4) 0.036(4) 0.003(3) -0.002(3) 0.002(3) C203 0.048(4) 0.048(4) 0.042(4) -0.009(3) 0.001(3) -0.008(3) C204 0.074(6) 0.112(7) 0.050(5) 0.024(5) -0.001(4) -0.019(5) C205 0.067(7) 0.220(14) 0.082(8) 0.023(8) 0.016(6) -0.062(8) C206 0.053(7) 0.238(16) 0.098(10) -0.063(10) 0.031(6) -0.018(8) C207 0.049(6) 0.107(8) 0.132(10) -0.042(7) -0.013(6) 0.020(5) C208 0.055(5) 0.053(5) 0.090(6) -0.006(4) -0.009(4) 0.003(4) C209 0.055(4) 0.044(4) 0.051(4) -0.018(4) 0.010(4) -0.006(3) C210 0.109(7) 0.069(5) 0.049(5) -0.015(4) 0.012(5) -0.023(5) C211 0.108(7) 0.067(6) 0.064(6) -0.031(5) 0.008(5) -0.007(5) C212 0.190(12) 0.123(9) 0.082(7) -0.052(7) 0.064(8) -0.054(8) C213 0.47(3) 0.188(13) 0.191(13) -0.139(11) 0.260(17) -0.215(16) C214 0.35(2) 0.151(10) 0.175(12) -0.119(9) 0.215(13) -0.169(12) N1 0.029(3) 0.049(3) 0.051(3) -0.004(3) 0.007(3) 0.007(2) N2 0.057(4) 0.061(4) 0.063(4) -0.027(3) 0.007(3) 0.003(3) C2 0.024(4) 0.099(6) 0.075(6) -0.041(5) -0.001(4) 0.001(4) C3 0.041(5) 0.101(6) 0.080(6) -0.045(5) 0.002(4) -0.024(4) C1 0.035(4) 0.064(5) 0.068(5) -0.016(4) 0.004(4) -0.002(3) N3 0.039(3) 0.051(3) 0.036(3) 0.006(3) 0.003(3) 0.006(2) N4 0.050(4) 0.056(4) 0.053(4) 0.007(3) 0.000(3) 0.016(3) C5 0.071(5) 0.084(6) 0.042(5) 0.005(4) 0.003(4) 0.026(4) C6 0.084(6) 0.101(6) 0.040(5) 0.014(5) 0.005(4) 0.032(5) C4 0.042(4) 0.061(4) 0.042(4) 0.006(4) -0.001(3) 0.007(3) N5 0.039(3) 0.043(3) 0.047(3) 0.002(3) -0.006(3) 0.003(2) N6 0.038(4) 0.072(5) 0.083(5) -0.012(4) -0.023(4) 0.007(3) C8 0.036(5) 0.172(9) 0.110(8) 0.089(7) -0.021(5) -0.016(5) C9 0.036(5) 0.167(10) 0.178(11) 0.092(9) -0.003(6) -0.023(5) C7 0.055(5) 0.066(5) 0.052(5) -0.001(4) -0.004(4) 0.014(4) _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 Ni O11 2.034(4) . ? Ni N1 2.055(5) . ? Ni N3 2.058(5) . ? Ni N5 2.078(5) . ? Ni O13 2.136(4) . ? Ni O21 2.156(4) . ? O11 C101 1.257(7) . ? O12 C101 1.238(7) . ? O13 C102 1.438(7) . ? C101 C102 1.571(7) . ? C102 C109 1.521(8) . ? C102 C103 1.533(7) . ? C103 C108 1.363(8) . ? C103 C104 1.362(8) . ? C104 C105 1.385(9) . ? C105 C106 1.349(10) . ? C106 C107 1.350(10) . ? C107 C108 1.375(10) . ? C109 C114 1.367(8) . ? C109 C110 1.382(8) . ? C110 C111 1.382(9) . ? C111 C112 1.364(9) . ? C112 C113 1.367(9) . ? C113 C114 1.375(9) . ? O21 C201 1.269(6) . ? O22 C201 1.252(6) . ? O23 C202 1.436(6) . ? C201 C202 1.533(8) . ? C202 C209 1.524(8) . ? C202 C203 1.531(8) . ? C203 C204 1.365(9) . ? C203 C208 1.393(9) . ? C204 C205 1.406(11) . ? C205 C206 1.335(14) . ? C206 C207 1.359(14) . ? C207 C208 1.372(10) . ? C209 C214 1.315(11) . ? C209 C210 1.327(8) . ? C210 C211 1.383(10) . ? C211 C212 1.297(11) . ? C212 C213 1.310(12) . ? C213 C214 1.383(13) . ? N1 C1 1.306(7) . ? N1 C2 1.358(7) . ? N2 C3 1.330(8) . ? N2 C1 1.330(8) . ? C2 C3 1.340(9) . ? N3 C4 1.312(7) . ? N3 C5 1.358(8) . ? N4 C4 1.329(7) . ? N4 C6 1.352(8) . ? C5 C6 1.336(9) . ? N5 C7 1.309(7) . ? N5 C8 1.345(8) . ? N6 C7 1.309(9) . ? N6 C9 1.309(10) . ? C8 C9 1.342(10) . ? 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 O11 Ni N1 90.52(17) . . ? O11 Ni N3 88.37(17) . . ? N1 Ni N3 92.91(19) . . ? O11 Ni N5 171.23(18) . . ? N1 Ni N5 94.61(19) . . ? N3 Ni N5 98.45(19) . . ? O11 Ni O13 77.94(15) . . ? N1 Ni O13 91.35(18) . . ? N3 Ni O13 165.70(17) . . ? N5 Ni O13 94.80(18) . . ? O11 Ni O21 89.84(15) . . ? N1 Ni O21 179.23(17) . . ? N3 Ni O21 87.79(17) . . ? N5 Ni O21 84.95(17) . . ? O13 Ni O21 88.06(16) . . ? C101 O11 Ni 119.7(4) . . ? C102 O13 Ni 114.0(3) . . ? O12 C101 O11 123.6(5) . . ? O12 C101 C102 118.6(5) . . ? O11 C101 C102 117.7(5) . . ? O13 C102 C109 110.4(4) . . ? O13 C102 C103 106.9(5) . . ? C109 C102 C103 112.7(5) . . ? O13 C102 C101 108.1(5) . . ? C109 C102 C101 108.1(5) . . ? C103 C102 C101 110.5(4) . . ? C108 C103 C104 116.8(6) . . ? C108 C103 C102 121.1(5) . . ? C104 C103 C102 122.0(5) . . ? C103 C104 C105 122.4(6) . . ? C106 C105 C104 119.2(7) . . ? C105 C106 C107 119.7(7) . . ? C106 C107 C108 120.5(7) . . ? C103 C108 C107 121.4(7) . . ? C114 C109 C110 118.5(6) . . ? C114 C109 C102 119.6(5) . . ? C110 C109 C102 121.8(6) . . ? C109 C110 C111 119.3(6) . . ? C112 C111 C110 121.9(7) . . ? C111 C112 C113 118.4(7) . . ? C112 C113 C114 120.4(7) . . ? C109 C114 C113 121.4(6) . . ? C201 O21 Ni 124.4(4) . . ? O22 C201 O21 125.3(6) . . ? O22 C201 C202 118.7(5) . . ? O21 C201 C202 115.9(5) . . ? O23 C202 C209 107.2(5) . . ? O23 C202 C203 109.5(5) . . ? C209 C202 C203 110.8(5) . . ? O23 C202 C201 106.5(5) . . ? C209 C202 C201 113.6(5) . . ? C203 C202 C201 109.2(5) . . ? C204 C203 C208 117.6(7) . . ? C204 C203 C202 122.1(6) . . ? C208 C203 C202 120.2(6) . . ? C203 C204 C205 119.7(8) . . ? C206 C205 C204 121.7(10) . . ? C205 C206 C207 119.0(10) . . ? C206 C207 C208 120.7(10) . . ? C207 C208 C203 121.0(8) . . ? C214 C209 C210 114.7(7) . . ? C214 C209 C202 124.0(6) . . ? C210 C209 C202 121.3(6) . . ? C209 C210 C211 123.5(8) . . ? C212 C211 C210 120.2(8) . . ? C211 C212 C213 117.7(9) . . ? C212 C213 C214 121.8(10) . . ? C209 C214 C213 122.0(9) . . ? C1 N1 C2 104.2(5) . . ? C1 N1 Ni 127.8(4) . . ? C2 N1 Ni 127.9(4) . . ? C3 N2 C1 106.5(6) . . ? C3 C2 N1 109.8(6) . . ? N2 C3 C2 107.1(6) . . ? N1 C1 N2 112.4(6) . . ? C4 N3 C5 104.9(5) . . ? C4 N3 Ni 121.6(4) . . ? C5 N3 Ni 132.7(5) . . ? C4 N4 C6 107.5(6) . . ? C6 C5 N3 110.4(6) . . ? C5 C6 N4 105.9(6) . . ? N3 C4 N4 111.3(6) . . ? C7 N5 C8 103.2(6) . . ? C7 N5 Ni 127.7(5) . . ? C8 N5 Ni 129.1(4) . . ? C7 N6 C9 107.5(6) . . ? C9 C8 N5 110.4(7) . . ? N6 C9 C8 106.3(8) . . ? N6 C7 N5 112.6(7) . . ? 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 C214 H214 O22 0.93 2.32 2.947(10) 124.5 . C208 H208 O22 0.93 2.43 2.933(8) 113.9 . C204 H204 O23 0.93 2.40 2.748(9) 102.3 . C108 H108 O13 0.93 2.37 2.716(8) 101.5 . C104 H104 O12 0.93 2.37 3.018(7) 126.5 . N4 H40 O23 0.89(6) 1.93(6) 2.814(7) 168(6) 3_656 N2 H20 O12 0.99(8) 1.78(8) 2.763(7) 172(7) 4_566 O13 H13 O21 0.87(7) 2.56(7) 2.982(5) 110(5) . O13 H13 O22 0.87(7) 1.72(7) 2.562(5) 161(7) . N6 H60 O11 0.81(7) 2.48(7) 3.191(7) 146(6) 1_455 N6 H60 O12 0.81(7) 2.25(7) 2.953(8) 145(6) 1_455 O23 H23 O21 0.82 2.03 2.507(5) 117.0 . _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 28.07 _diffrn_measured_fraction_theta_full 0.909 _refine_diff_density_max 0.605 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.068