Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'McGaff, Robert W.' 'Halfen, Jason A.' 'Loe, Jocelyn C.' 'Molek, Christopher D.' _publ_contact_author_name 'Dr Robert W McGaff' _publ_contact_author_address ; La Crosse Department of Chemistry University of WIsconsin 1725 State Street La Crosse WI 54601 UNITED STATES OF AMERICA ; _publ_contact_author_email 'MCGAFF.ROBE@UWLAX.EDU' _publ_section_title ; Solventothermal synthesis and X-ray crystal structures of two nickel complexes with novel alkoxy-substituted phthalocyanine ligands ; data_0052 _database_code_CSD 174008 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '0052 Compound 1' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H26 N8 Ni O3' _chemical_formula_weight 665.35 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.160(2) _cell_length_b 12.853(3) _cell_length_c 16.936(3) _cell_angle_alpha 93.33(2) _cell_angle_beta 99.98(2) _cell_angle_gamma 105.28(4) _cell_volume 1471.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 3.56 _cell_measurement_theta_max 20.09 _exptl_crystal_description block _exptl_crystal_colour 'red-orange' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.712 _exptl_absorpt_correction_type 'psi-scan corrections' _exptl_absorpt_correction_T_min 0.8056 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 'Enraf-Nonius CAD4' _diffrn_measurement_method 'Omega 2-theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '5400 seconds' _diffrn_standards_decay_% 0 _diffrn_reflns_number 5620 _diffrn_reflns_av_R_equivalents 0.0892 _diffrn_reflns_av_sigmaI/netI 0.1745 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 24.96 _reflns_number_total 5170 _reflns_number_gt 2796 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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^)+(0.0734P)^2^+0.3391P] 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 5170 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1830 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1656 _refine_ls_wR_factor_gt 0.1295 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 0.05627(11) 0.48468(6) 0.28103(4) 0.0313(2) Uani 1 1 d . . . N1 N -0.0622(7) 0.4181(4) 0.1785(3) 0.0371(12) Uani 1 1 d . . . N4 N -0.0047(6) 0.3513(3) 0.3223(3) 0.0313(10) Uani 1 1 d . . . N3 N 0.2038(6) 0.5500(3) 0.3797(3) 0.0292(10) Uani 1 1 d . . . N2 N 0.0662(7) 0.6199(4) 0.2444(3) 0.0345(11) Uani 1 1 d . . . N8 N -0.1623(7) 0.2271(4) 0.2017(3) 0.0388(12) Uani 1 1 d . . . N7 N 0.1097(6) 0.4095(3) 0.4647(3) 0.0307(10) Uani 1 1 d . . . N6 N 0.2844(7) 0.7421(4) 0.3556(3) 0.0339(11) Uani 1 1 d . . . N5 N -0.1609(7) 0.5624(4) 0.1162(3) 0.0416(12) Uani 1 1 d . . . C8 C -0.1442(9) 0.4608(5) 0.1183(3) 0.0398(14) Uani 1 1 d . . . C7 C -0.2193(9) 0.3804(5) 0.0464(3) 0.0423(15) Uani 1 1 d . . . C6 C -0.3190(10) 0.3861(6) -0.0295(4) 0.0529(17) Uani 1 1 d . . . H3A H -0.3584 0.4475 -0.0422 0.063 Uiso 1 1 calc R . . C5 C -0.3592(10) 0.2965(6) -0.0869(4) 0.0572(19) Uani 1 1 d . . . H4A H -0.4230 0.2985 -0.1393 0.069 Uiso 1 1 calc R . . C4 C -0.3051(10) 0.2064(6) -0.0664(4) 0.0570(19) Uani 1 1 d . . . H5B H -0.3354 0.1472 -0.1052 0.068 Uiso 1 1 calc R . . C3 C -0.2072(10) 0.1994(5) 0.0098(4) 0.0522(17) Uani 1 1 d . . . H6B H -0.1700 0.1375 0.0228 0.063 Uiso 1 1 calc R . . C2 C -0.1670(9) 0.2879(5) 0.0655(3) 0.0435(15) Uani 1 1 d . . . C1 C -0.0622(9) 0.3066(5) 0.1532(3) 0.0397(14) Uani 1 1 d . . . C32 C -0.1202(8) 0.2526(4) 0.2785(3) 0.0329(13) Uani 1 1 d . . . C31 C -0.1867(8) 0.1757(4) 0.3363(3) 0.0333(13) Uani 1 1 d . . . C30 C -0.3061(9) 0.0700(5) 0.3259(4) 0.0439(15) Uani 1 1 d . . . H11A H -0.3655 0.0346 0.2746 0.053 Uiso 1 1 calc R . . C29 C -0.3341(9) 0.0186(5) 0.3943(4) 0.0465(16) Uani 1 1 d . . . H12A H -0.4132 -0.0526 0.3891 0.056 Uiso 1 1 calc R . . C28 C -0.2461(9) 0.0717(5) 0.4701(4) 0.0472(16) Uani 1 1 d . . . H13A H -0.2688 0.0358 0.5152 0.057 Uiso 1 1 calc R . . C27 C -0.1245(8) 0.1776(4) 0.4811(3) 0.0366(13) Uani 1 1 d . . . H14A H -0.0629 0.2127 0.5322 0.044 Uiso 1 1 calc R . . C26 C -0.0996(8) 0.2280(4) 0.4121(3) 0.0334(13) Uani 1 1 d . . . C25 C 0.0115(7) 0.3391(4) 0.4027(3) 0.0295(12) Uani 1 1 d . . . C24 C 0.2117(8) 0.5102(4) 0.4492(3) 0.0280(12) Uani 1 1 d . . . C23 C 0.3520(8) 0.5870(4) 0.5134(3) 0.0313(13) Uani 1 1 d . . . C22 C 0.3956(8) 0.5832(5) 0.5958(3) 0.0357(13) Uani 1 1 d . . . H19A H 0.3364 0.5229 0.6196 0.043 Uiso 1 1 calc R . . C21 C 0.5299(9) 0.6721(5) 0.6410(4) 0.0497(17) Uani 1 1 d . . . H20A H 0.5651 0.6714 0.6964 0.060 Uiso 1 1 calc R . . C20 C 0.6144(9) 0.7630(5) 0.6058(4) 0.0467(16) Uani 1 1 d . . . H21A H 0.7020 0.8227 0.6384 0.056 Uiso 1 1 calc R . . C19 C 0.5720(8) 0.7672(5) 0.5238(4) 0.0407(14) Uani 1 1 d . . . H22A H 0.6301 0.8283 0.5006 0.049 Uiso 1 1 calc R . . C18 C 0.4392(8) 0.6767(5) 0.4768(3) 0.0368(14) Uani 1 1 d . . . C17 C 0.3564(8) 0.6551(4) 0.3874(3) 0.0322(13) Uani 1 1 d . . . C16 C 0.1570(8) 0.7209(4) 0.2909(3) 0.0320(13) Uani 1 1 d . . . C15 C 0.0797(8) 0.8032(4) 0.2488(3) 0.0347(13) Uani 1 1 d . . . C14 C 0.1162(9) 0.9126(5) 0.2688(4) 0.0433(15) Uani 1 1 d . . . H27A H 0.2051 0.9478 0.3153 0.052 Uiso 1 1 calc R . . C13 C 0.0163(11) 0.9691(5) 0.2174(4) 0.0556(18) Uani 1 1 d . . . H28A H 0.0358 1.0430 0.2300 0.067 Uiso 1 1 calc R . . C12 C -0.1127(11) 0.9156(6) 0.1472(4) 0.0582(19) Uani 1 1 d . . . H29A H -0.1790 0.9546 0.1136 0.070 Uiso 1 1 calc R . . C11 C -0.1452(9) 0.8057(5) 0.1258(4) 0.0443(15) Uani 1 1 d . . . H30A H -0.2286 0.7706 0.0780 0.053 Uiso 1 1 calc R . . C10 C -0.0481(8) 0.7504(4) 0.1788(3) 0.0357(13) Uani 1 1 d . . . C9 C -0.0545(8) 0.6350(4) 0.1767(3) 0.0341(13) Uani 1 1 d . . . O1 O 0.4893(6) 0.6308(3) 0.3402(3) 0.0458(10) Uani 1 1 d . . . O2 O 0.1327(6) 0.2960(3) 0.1655(2) 0.0475(11) Uani 1 1 d . . . C33 C 0.6634(10) 0.7130(6) 0.3391(5) 0.076(2) Uani 1 1 d . . . H33A H 0.7380 0.6872 0.3044 0.114 Uiso 1 1 calc R . . H33B H 0.7410 0.7323 0.3928 0.114 Uiso 1 1 calc R . . H33C H 0.6296 0.7756 0.3195 0.114 Uiso 1 1 calc R . . C34 C 0.2660(10) 0.3687(6) 0.1255(4) 0.0613(19) Uani 1 1 d . . . H34A H 0.3938 0.3561 0.1372 0.092 Uiso 1 1 calc R . . H34B H 0.2765 0.4423 0.1443 0.092 Uiso 1 1 calc R . . H34C H 0.2166 0.3562 0.0683 0.092 Uiso 1 1 calc R . . O1S O -0.5006(11) 0.0553(5) 0.1250(4) 0.109(2) Uani 1 1 d . . . H1SD H -0.4151 0.1026 0.1558 0.164 Uiso 1 1 calc R . . C1S C -0.6432(14) 0.0994(8) 0.0873(7) 0.110(3) Uani 1 1 d . . . H1SA H -0.7529 0.0423 0.0578 0.165 Uiso 1 1 calc R . . H1SB H -0.5891 0.1479 0.0508 0.165 Uiso 1 1 calc R . . H1SC H -0.6871 0.1386 0.1269 0.165 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 Ni1 0.0346(4) 0.0233(4) 0.0336(4) 0.0059(3) 0.0063(3) 0.0037(3) N1 0.047(3) 0.026(3) 0.034(3) 0.001(2) 0.006(2) 0.005(2) N4 0.033(3) 0.021(2) 0.035(3) 0.003(2) 0.005(2) 0.000(2) N3 0.034(3) 0.018(2) 0.035(3) 0.007(2) 0.010(2) 0.004(2) N2 0.035(3) 0.026(3) 0.041(3) 0.012(2) 0.005(2) 0.007(2) N8 0.049(3) 0.030(3) 0.036(3) 0.004(2) 0.010(2) 0.007(2) N7 0.029(2) 0.024(3) 0.037(3) 0.006(2) 0.004(2) 0.005(2) N6 0.033(3) 0.027(3) 0.039(3) 0.005(2) 0.006(2) 0.003(2) N5 0.046(3) 0.029(3) 0.044(3) 0.008(2) 0.004(2) 0.003(2) C8 0.042(3) 0.037(4) 0.037(3) 0.010(3) 0.006(3) 0.005(3) C7 0.050(4) 0.033(4) 0.040(4) 0.006(3) 0.009(3) 0.005(3) C6 0.054(4) 0.052(4) 0.048(4) 0.014(3) 0.007(3) 0.008(3) C5 0.062(5) 0.059(5) 0.037(4) 0.001(4) 0.007(3) -0.004(4) C4 0.066(5) 0.052(5) 0.037(4) -0.006(3) 0.009(3) -0.009(4) C3 0.061(4) 0.047(4) 0.040(4) -0.007(3) 0.015(3) 0.000(3) C2 0.049(4) 0.038(4) 0.037(3) 0.002(3) 0.011(3) 0.001(3) C1 0.050(4) 0.030(3) 0.039(3) 0.005(3) 0.011(3) 0.009(3) C32 0.034(3) 0.023(3) 0.042(3) 0.007(3) 0.009(3) 0.006(3) C31 0.036(3) 0.020(3) 0.044(3) 0.006(2) 0.012(3) 0.005(2) C30 0.047(4) 0.031(3) 0.050(4) 0.004(3) 0.007(3) 0.005(3) C29 0.055(4) 0.021(3) 0.057(4) 0.014(3) 0.012(3) -0.004(3) C28 0.056(4) 0.035(4) 0.051(4) 0.013(3) 0.015(3) 0.009(3) C27 0.039(3) 0.028(3) 0.041(3) 0.007(3) 0.011(3) 0.005(3) C26 0.030(3) 0.024(3) 0.046(3) 0.011(3) 0.010(3) 0.004(2) C25 0.028(3) 0.028(3) 0.036(3) 0.011(3) 0.007(2) 0.011(2) C24 0.029(3) 0.026(3) 0.031(3) 0.003(2) 0.006(2) 0.010(2) C23 0.027(3) 0.032(3) 0.036(3) 0.006(3) 0.006(2) 0.010(3) C22 0.034(3) 0.030(3) 0.040(3) 0.000(3) 0.002(3) 0.007(3) C21 0.051(4) 0.052(4) 0.048(4) 0.007(3) 0.001(3) 0.022(4) C20 0.036(3) 0.038(4) 0.054(4) -0.010(3) -0.011(3) 0.005(3) C19 0.036(3) 0.031(3) 0.049(4) 0.003(3) -0.001(3) 0.005(3) C18 0.024(3) 0.035(3) 0.050(4) 0.008(3) 0.002(3) 0.009(3) C17 0.031(3) 0.021(3) 0.042(3) 0.001(2) 0.004(3) 0.004(2) C16 0.032(3) 0.022(3) 0.045(3) 0.010(3) 0.017(3) 0.005(2) C15 0.035(3) 0.027(3) 0.046(4) 0.012(3) 0.016(3) 0.009(3) C14 0.053(4) 0.031(3) 0.046(4) 0.006(3) 0.003(3) 0.015(3) C13 0.072(5) 0.027(3) 0.068(5) 0.012(3) 0.009(4) 0.016(3) C12 0.067(5) 0.052(5) 0.068(5) 0.023(4) 0.014(4) 0.034(4) C11 0.045(4) 0.041(4) 0.048(4) 0.014(3) 0.005(3) 0.016(3) C10 0.034(3) 0.029(3) 0.045(3) 0.012(3) 0.011(3) 0.006(3) C9 0.035(3) 0.029(3) 0.040(3) 0.013(3) 0.013(3) 0.007(3) O1 0.041(2) 0.037(2) 0.065(3) 0.012(2) 0.021(2) 0.013(2) O2 0.049(3) 0.046(3) 0.052(3) 0.014(2) 0.015(2) 0.016(2) C33 0.048(4) 0.079(6) 0.094(6) 0.007(5) 0.030(4) -0.005(4) C34 0.059(4) 0.054(4) 0.071(5) 0.016(4) 0.030(4) 0.004(4) O1S 0.116(6) 0.064(4) 0.108(5) 0.013(4) -0.028(4) -0.013(4) C1S 0.077(7) 0.086(7) 0.158(10) 0.032(7) 0.009(7) 0.015(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 N3 1.836(4) . ? Ni1 N1 1.845(4) . ? Ni1 N4 1.862(4) . ? Ni1 N2 1.867(4) . ? N1 C8 1.307(7) . ? N1 C1 1.472(7) . ? N4 C25 1.368(6) . ? N4 C32 1.403(7) . ? N3 C24 1.309(6) . ? N3 C17 1.479(7) . ? N2 C9 1.368(7) . ? N2 C16 1.409(7) . ? N8 C32 1.286(7) . ? N8 C1 1.466(7) . ? N7 C25 1.310(6) . ? N7 C24 1.373(6) . ? N6 C16 1.263(7) . ? N6 C17 1.444(7) . ? N5 C9 1.320(7) . ? N5 C8 1.344(7) . ? N5 H1SD 5.8218 . ? C8 C7 1.475(8) . ? C7 C6 1.374(8) . ? C7 C2 1.377(8) . ? C6 C5 1.397(9) . ? C5 C4 1.360(9) . ? C4 C3 1.376(9) . ? C3 C2 1.369(8) . ? C2 C1 1.518(8) . ? C1 O2 1.418(7) . ? C32 C31 1.478(7) . ? C31 C26 1.374(8) . ? C31 C30 1.384(7) . ? C30 C29 1.385(8) . ? C29 C28 1.380(8) . ? C28 C27 1.391(8) . ? C27 C26 1.384(7) . ? C26 C25 1.473(7) . ? C24 C23 1.462(7) . ? C23 C22 1.384(7) . ? C23 C18 1.393(7) . ? C22 C21 1.372(8) . ? C21 C20 1.385(9) . ? C20 C19 1.377(8) . ? C19 C18 1.392(8) . ? C18 C17 1.507(8) . ? C17 O1 1.426(7) . ? C16 C15 1.481(7) . ? C15 C14 1.371(8) . ? C15 C10 1.381(8) . ? C14 C13 1.388(8) . ? C13 C12 1.389(9) . ? C12 C11 1.385(9) . ? C11 C10 1.382(8) . ? C10 C9 1.471(7) . ? O1 C33 1.410(7) . ? O2 C34 1.438(7) . ? O1S C1S 1.376(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 N3 Ni1 N1 172.8(2) . . ? N3 Ni1 N4 90.46(19) . . ? N1 Ni1 N4 90.4(2) . . ? N3 Ni1 N2 90.77(19) . . ? N1 Ni1 N2 89.9(2) . . ? N4 Ni1 N2 167.88(19) . . ? C8 N1 C1 110.9(5) . . ? C8 N1 Ni1 127.4(4) . . ? C1 N1 Ni1 121.5(4) . . ? C25 N4 C32 108.2(4) . . ? C25 N4 Ni1 124.3(4) . . ? C32 N4 Ni1 125.5(4) . . ? C24 N3 C17 109.9(4) . . ? C24 N3 Ni1 128.2(4) . . ? C17 N3 Ni1 121.3(3) . . ? C9 N2 C16 109.0(4) . . ? C9 N2 Ni1 123.8(4) . . ? C16 N2 Ni1 125.3(4) . . ? C32 N8 C1 116.5(5) . . ? C25 N7 C24 117.5(4) . . ? C16 N6 C17 118.4(5) . . ? C9 N5 C8 117.1(5) . . ? C9 N5 H1SD 121.6 . . ? C8 N5 H1SD 24.1 . . ? N1 C8 N5 128.6(6) . . ? N1 C8 C7 110.3(5) . . ? N5 C8 C7 121.2(5) . . ? C6 C7 C2 120.7(6) . . ? C6 C7 C8 131.8(6) . . ? C2 C7 C8 107.5(5) . . ? C7 C6 C5 117.8(7) . . ? C4 C5 C6 120.1(6) . . ? C5 C4 C3 122.5(6) . . ? C2 C3 C4 117.0(7) . . ? C3 C2 C7 121.8(6) . . ? C3 C2 C1 130.1(6) . . ? C7 C2 C1 108.0(5) . . ? O2 C1 N8 103.8(4) . . ? O2 C1 N1 111.1(5) . . ? N8 C1 N1 112.6(5) . . ? O2 C1 C2 114.3(5) . . ? N8 C1 C2 112.1(5) . . ? N1 C1 C2 103.2(5) . . ? N8 C32 N4 128.5(5) . . ? N8 C32 C31 123.0(5) . . ? N4 C32 C31 108.5(5) . . ? C26 C31 C30 121.0(5) . . ? C26 C31 C32 106.5(5) . . ? C30 C31 C32 132.5(5) . . ? C31 C30 C29 117.8(6) . . ? C28 C29 C30 120.8(5) . . ? C29 C28 C27 121.7(6) . . ? C26 C27 C28 116.7(5) . . ? C31 C26 C27 122.0(5) . . ? C31 C26 C25 107.7(5) . . ? C27 C26 C25 130.3(5) . . ? N7 C25 N4 128.7(5) . . ? N7 C25 C26 122.2(5) . . ? N4 C25 C26 109.0(5) . . ? N3 C24 N7 127.5(5) . . ? N3 C24 C23 111.5(5) . . ? N7 C24 C23 121.0(5) . . ? C22 C23 C18 122.2(5) . . ? C22 C23 C24 131.3(5) . . ? C18 C23 C24 106.4(5) . . ? C21 C22 C23 117.2(6) . . ? C22 C21 C20 121.4(6) . . ? C19 C20 C21 121.7(6) . . ? C20 C19 C18 117.7(6) . . ? C19 C18 C23 119.9(5) . . ? C19 C18 C17 131.6(5) . . ? C23 C18 C17 108.5(5) . . ? O1 C17 N6 109.1(4) . . ? O1 C17 N3 102.6(4) . . ? N6 C17 N3 114.5(4) . . ? O1 C17 C18 114.2(4) . . ? N6 C17 C18 112.9(4) . . ? N3 C17 C18 103.2(4) . . ? N6 C16 N2 128.5(5) . . ? N6 C16 C15 124.1(5) . . ? N2 C16 C15 107.3(5) . . ? C14 C15 C10 121.5(5) . . ? C14 C15 C16 131.2(6) . . ? C10 C15 C16 107.3(5) . . ? C15 C14 C13 118.0(6) . . ? C14 C13 C12 120.3(6) . . ? C11 C12 C13 121.8(6) . . ? C10 C11 C12 117.0(6) . . ? C15 C10 C11 121.4(5) . . ? C15 C10 C9 107.4(5) . . ? C11 C10 C9 131.2(5) . . ? N5 C9 N2 128.5(5) . . ? N5 C9 C10 122.5(5) . . ? N2 C9 C10 109.0(5) . . ? C33 O1 C17 117.6(5) . . ? C1 O2 C34 115.1(5) . . ? 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 N3 Ni1 N1 C8 -110.3(16) . . . . ? N4 Ni1 N1 C8 152.6(5) . . . . ? N2 Ni1 N1 C8 -15.3(5) . . . . ? N3 Ni1 N1 C1 65.4(18) . . . . ? N4 Ni1 N1 C1 -31.8(4) . . . . ? N2 Ni1 N1 C1 160.4(4) . . . . ? N3 Ni1 N4 C25 19.1(4) . . . . ? N1 Ni1 N4 C25 -168.1(4) . . . . ? N2 Ni1 N4 C25 -76.8(11) . . . . ? N3 Ni1 N4 C32 -178.9(4) . . . . ? N1 Ni1 N4 C32 -6.1(4) . . . . ? N2 Ni1 N4 C32 85.2(10) . . . . ? N1 Ni1 N3 C24 -108.8(16) . . . . ? N4 Ni1 N3 C24 -11.7(5) . . . . ? N2 Ni1 N3 C24 156.3(5) . . . . ? N1 Ni1 N3 C17 62.3(18) . . . . ? N4 Ni1 N3 C17 159.5(4) . . . . ? N2 Ni1 N3 C17 -32.5(4) . . . . ? N3 Ni1 N2 C9 -165.0(4) . . . . ? N1 Ni1 N2 C9 22.2(4) . . . . ? N4 Ni1 N2 C9 -69.2(11) . . . . ? N3 Ni1 N2 C16 -2.4(4) . . . . ? N1 Ni1 N2 C16 -175.2(4) . . . . ? N4 Ni1 N2 C16 93.4(10) . . . . ? C1 N1 C8 N5 -175.5(6) . . . . ? Ni1 N1 C8 N5 0.6(10) . . . . ? C1 N1 C8 C7 3.2(7) . . . . ? Ni1 N1 C8 C7 179.2(4) . . . . ? C9 N5 C8 N1 12.6(9) . . . . ? H1SD N5 C8 N1 -94.8 . . . . ? C9 N5 C8 C7 -165.9(5) . . . . ? H1SD N5 C8 C7 86.7 . . . . ? N1 C8 C7 C6 178.3(6) . . . . ? N5 C8 C7 C6 -2.9(11) . . . . ? N1 C8 C7 C2 -3.4(7) . . . . ? N5 C8 C7 C2 175.3(6) . . . . ? C2 C7 C6 C5 -2.1(10) . . . . ? C8 C7 C6 C5 175.9(6) . . . . ? C7 C6 C5 C4 1.9(10) . . . . ? C6 C5 C4 C3 -1.2(11) . . . . ? C5 C4 C3 C2 0.6(10) . . . . ? C4 C3 C2 C7 -0.9(9) . . . . ? C4 C3 C2 C1 -179.7(6) . . . . ? C6 C7 C2 C3 1.7(10) . . . . ? C8 C7 C2 C3 -176.8(6) . . . . ? C6 C7 C2 C1 -179.3(6) . . . . ? C8 C7 C2 C1 2.2(7) . . . . ? C32 N8 C1 O2 75.0(6) . . . . ? C32 N8 C1 N1 -45.3(7) . . . . ? C32 N8 C1 C2 -161.2(5) . . . . ? C8 N1 C1 O2 121.2(5) . . . . ? Ni1 N1 C1 O2 -55.1(6) . . . . ? C8 N1 C1 N8 -122.9(5) . . . . ? Ni1 N1 C1 N8 60.8(6) . . . . ? C8 N1 C1 C2 -1.7(6) . . . . ? Ni1 N1 C1 C2 -178.0(4) . . . . ? C3 C2 C1 O2 57.6(8) . . . . ? C7 C2 C1 O2 -121.3(5) . . . . ? C3 C2 C1 N8 -60.1(8) . . . . ? C7 C2 C1 N8 121.0(5) . . . . ? C3 C2 C1 N1 178.4(6) . . . . ? C7 C2 C1 N1 -0.5(6) . . . . ? C1 N8 C32 N4 6.7(8) . . . . ? C1 N8 C32 C31 -171.3(5) . . . . ? C25 N4 C32 N8 -175.7(5) . . . . ? Ni1 N4 C32 N8 19.9(8) . . . . ? C25 N4 C32 C31 2.5(6) . . . . ? Ni1 N4 C32 C31 -161.9(4) . . . . ? N8 C32 C31 C26 174.7(5) . . . . ? N4 C32 C31 C26 -3.6(6) . . . . ? N8 C32 C31 C30 -3.6(10) . . . . ? N4 C32 C31 C30 178.1(6) . . . . ? C26 C31 C30 C29 -0.3(9) . . . . ? C32 C31 C30 C29 177.8(6) . . . . ? C31 C30 C29 C28 0.3(9) . . . . ? C30 C29 C28 C27 -0.9(10) . . . . ? C29 C28 C27 C26 1.5(9) . . . . ? C30 C31 C26 C27 0.9(9) . . . . ? C32 C31 C26 C27 -177.6(5) . . . . ? C30 C31 C26 C25 -178.3(5) . . . . ? C32 C31 C26 C25 3.2(6) . . . . ? C28 C27 C26 C31 -1.4(8) . . . . ? C28 C27 C26 C25 177.5(5) . . . . ? C24 N7 C25 N4 0.1(8) . . . . ? C24 N7 C25 C26 178.6(4) . . . . ? C32 N4 C25 N7 178.2(5) . . . . ? Ni1 N4 C25 N7 -17.2(8) . . . . ? C32 N4 C25 C26 -0.5(6) . . . . ? Ni1 N4 C25 C26 164.2(3) . . . . ? C31 C26 C25 N7 179.4(5) . . . . ? C27 C26 C25 N7 0.4(9) . . . . ? C31 C26 C25 N4 -1.8(6) . . . . ? C27 C26 C25 N4 179.1(5) . . . . ? C17 N3 C24 N7 -172.4(5) . . . . ? Ni1 N3 C24 N7 -0.4(8) . . . . ? C17 N3 C24 C23 6.3(6) . . . . ? Ni1 N3 C24 C23 178.3(3) . . . . ? C25 N7 C24 N3 9.3(8) . . . . ? C25 N7 C24 C23 -169.3(5) . . . . ? N3 C24 C23 C22 174.0(5) . . . . ? N7 C24 C23 C22 -7.2(8) . . . . ? N3 C24 C23 C18 -3.0(6) . . . . ? N7 C24 C23 C18 175.8(5) . . . . ? C18 C23 C22 C21 -0.1(8) . . . . ? C24 C23 C22 C21 -176.7(5) . . . . ? C23 C22 C21 C20 1.6(9) . . . . ? C22 C21 C20 C19 -1.9(9) . . . . ? C21 C20 C19 C18 0.5(9) . . . . ? C20 C19 C18 C23 1.1(8) . . . . ? C20 C19 C18 C17 178.0(5) . . . . ? C22 C23 C18 C19 -1.3(8) . . . . ? C24 C23 C18 C19 176.1(5) . . . . ? C22 C23 C18 C17 -178.9(5) . . . . ? C24 C23 C18 C17 -1.5(6) . . . . ? C16 N6 C17 O1 75.0(6) . . . . ? C16 N6 C17 N3 -39.3(7) . . . . ? C16 N6 C17 C18 -157.0(5) . . . . ? C24 N3 C17 O1 112.1(5) . . . . ? Ni1 N3 C17 O1 -60.5(5) . . . . ? C24 N3 C17 N6 -129.9(5) . . . . ? Ni1 N3 C17 N6 57.4(6) . . . . ? C24 N3 C17 C18 -6.8(5) . . . . ? Ni1 N3 C17 C18 -179.5(3) . . . . ? C19 C18 C17 O1 77.1(7) . . . . ? C23 C18 C17 O1 -105.7(5) . . . . ? C19 C18 C17 N6 -48.2(8) . . . . ? C23 C18 C17 N6 129.0(5) . . . . ? C19 C18 C17 N3 -172.3(6) . . . . ? C23 C18 C17 N3 4.9(5) . . . . ? C17 N6 C16 N2 2.3(8) . . . . ? C17 N6 C16 C15 -176.0(5) . . . . ? C9 N2 C16 N6 -176.6(5) . . . . ? Ni1 N2 C16 N6 18.7(8) . . . . ? C9 N2 C16 C15 1.9(6) . . . . ? Ni1 N2 C16 C15 -162.9(4) . . . . ? N6 C16 C15 C14 -2.9(10) . . . . ? N2 C16 C15 C14 178.5(6) . . . . ? N6 C16 C15 C10 177.0(5) . . . . ? N2 C16 C15 C10 -1.6(6) . . . . ? C10 C15 C14 C13 1.7(9) . . . . ? C16 C15 C14 C13 -178.4(6) . . . . ? C15 C14 C13 C12 -1.5(10) . . . . ? C14 C13 C12 C11 -0.4(11) . . . . ? C13 C12 C11 C10 1.9(10) . . . . ? C14 C15 C10 C11 -0.1(9) . . . . ? C16 C15 C10 C11 180.0(5) . . . . ? C14 C15 C10 C9 -179.4(5) . . . . ? C16 C15 C10 C9 0.7(6) . . . . ? C12 C11 C10 C15 -1.7(9) . . . . ? C12 C11 C10 C9 177.4(6) . . . . ? C8 N5 C9 N2 -3.3(9) . . . . ? H1SD N5 C9 N2 23.9 . . . . ? C8 N5 C9 C10 175.5(5) . . . . ? H1SD N5 C9 C10 -157.3 . . . . ? C16 N2 C9 N5 177.5(5) . . . . ? Ni1 N2 C9 N5 -17.5(8) . . . . ? C16 N2 C9 C10 -1.5(6) . . . . ? Ni1 N2 C9 C10 163.6(4) . . . . ? C15 C10 C9 N5 -178.6(5) . . . . ? C11 C10 C9 N5 2.2(10) . . . . ? C15 C10 C9 N2 0.4(6) . . . . ? C11 C10 C9 N2 -178.7(6) . . . . ? N6 C17 O1 C33 62.6(7) . . . . ? N3 C17 O1 C33 -175.6(5) . . . . ? C18 C17 O1 C33 -64.7(7) . . . . ? N8 C1 O2 C34 -178.3(5) . . . . ? N1 C1 O2 C34 -57.0(6) . . . . ? C2 C1 O2 C34 59.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.579 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.088 #===END data_0107 _database_code_CSD 174009 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '0107 Compound 2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H26 N8 Ni O2' _chemical_formula_weight 661.36 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.950(2) _cell_length_b 13.080(4) _cell_length_c 15.395(5) _cell_angle_alpha 109.12(3) _cell_angle_beta 97.99(3) _cell_angle_gamma 94.14(3) _cell_volume 1486.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.82 _cell_measurement_theta_max 19.45 _exptl_crystal_description 'Irregular block' _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 0.703 _exptl_absorpt_correction_type 'Psi-scan corrections' _exptl_absorpt_correction_T_min 0.9004 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 'Enraf-Nonius CAD4' _diffrn_measurement_method 'Omega 2-theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '5400 seconds' _diffrn_standards_decay_% 8.0 _diffrn_reflns_number 5587 _diffrn_reflns_av_R_equivalents 0.1106 _diffrn_reflns_av_sigmaI/netI 0.0771 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 24.96 _reflns_number_total 5199 _reflns_number_gt 3531 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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^)+(0.0828P)^2^+1.9760P] 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 5199 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1161 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1643 _refine_ls_wR_factor_gt 0.1285 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 0.32542(7) 0.21937(5) 0.23730(4) 0.0296(2) Uani 1 1 d . . . N1 N 0.3598(4) 0.0767(3) 0.1855(2) 0.0291(8) Uani 1 1 d . . . N2 N 0.2643(5) 0.2280(3) 0.1195(2) 0.0329(9) Uani 1 1 d . . . N3 N 0.3211(5) 0.3668(3) 0.2914(3) 0.0327(9) Uani 1 1 d . . . N4 N 0.3306(5) 0.2024(3) 0.3530(2) 0.0312(9) Uani 1 1 d . . . N5 N 0.2310(5) 0.0376(3) 0.0264(3) 0.0351(9) Uani 1 1 d . . . N6 N 0.2555(5) 0.4215(3) 0.1543(3) 0.0376(9) Uani 1 1 d . . . N7 N 0.2490(5) 0.3767(3) 0.4381(3) 0.0359(9) Uani 1 1 d . . . N8 N 0.3862(5) 0.0150(3) 0.3196(3) 0.0331(9) Uani 1 1 d . . . O1 O 0.6248(4) 0.0810(3) 0.2810(2) 0.0369(8) Uani 1 1 d . . . O2 O 0.5318(4) 0.4344(3) 0.2199(2) 0.0430(8) Uani 1 1 d . . . C1 C 0.4595(6) 0.0214(4) 0.2402(3) 0.0318(10) Uani 1 1 d . . . C2 C 0.4637(6) -0.0903(4) 0.1692(3) 0.0322(10) Uani 1 1 d . . . C3 C 0.5338(6) -0.1794(4) 0.1792(4) 0.0387(11) Uani 1 1 d . . . H3A H 0.5926 -0.1771 0.2366 0.046 Uiso 1 1 calc R . . C4 C 0.5148(7) -0.2734(4) 0.1012(4) 0.0486(13) Uani 1 1 d . . . H4A H 0.5606 -0.3350 0.1064 0.058 Uiso 1 1 calc R . . C5 C 0.4286(7) -0.2762(4) 0.0161(4) 0.0493(14) Uani 1 1 d . . . H5B H 0.4178 -0.3399 -0.0351 0.059 Uiso 1 1 calc R . . C6 C 0.3583(7) -0.1874(4) 0.0050(3) 0.0425(12) Uani 1 1 d . . . H6B H 0.3001 -0.1898 -0.0526 0.051 Uiso 1 1 calc R . . C8 C 0.3179(6) 0.0128(4) 0.0971(3) 0.0320(10) Uani 1 1 d . . . C7 C 0.3779(6) -0.0932(4) 0.0839(3) 0.0340(10) Uani 1 1 d . . . C9 C 0.2067(6) 0.1398(4) 0.0411(3) 0.0322(10) Uani 1 1 d . . . C10 C 0.1152(6) 0.1763(4) -0.0314(3) 0.0344(11) Uani 1 1 d . . . C11 C 0.0302(6) 0.1182(4) -0.1216(3) 0.0404(12) Uani 1 1 d . . . H11A H 0.0230 0.0426 -0.1463 0.048 Uiso 1 1 calc R . . C12 C -0.0427(6) 0.1774(5) -0.1727(3) 0.0453(13) Uani 1 1 d . . . H12A H -0.1015 0.1408 -0.2329 0.054 Uiso 1 1 calc R . . C13 C -0.0310(7) 0.2889(5) -0.1373(4) 0.0522(14) Uani 1 1 d . . . H13A H -0.0805 0.3264 -0.1740 0.063 Uiso 1 1 calc R . . C14 C 0.0546(7) 0.3469(5) -0.0464(4) 0.0486(13) Uani 1 1 d . . . H14A H 0.0642 0.4226 -0.0222 0.058 Uiso 1 1 calc R . . C15 C 0.1234(6) 0.2878(4) 0.0053(3) 0.0385(11) Uani 1 1 d . . . C16 C 0.2196(6) 0.3215(4) 0.1013(3) 0.0342(10) Uani 1 1 d . . . C17 C 0.3664(6) 0.4433(4) 0.2433(3) 0.0344(10) Uani 1 1 d . . . C18 C 0.3494(6) 0.5537(4) 0.3131(3) 0.0346(11) Uani 1 1 d . . . C19 C 0.3720(6) 0.6555(4) 0.3070(4) 0.0416(12) Uani 1 1 d . . . H19A H 0.4007 0.6655 0.2536 0.050 Uiso 1 1 calc R . . C20 C 0.3507(7) 0.7435(4) 0.3829(4) 0.0468(13) Uani 1 1 d . . . H20A H 0.3668 0.8137 0.3809 0.056 Uiso 1 1 calc R . . C21 C 0.3063(7) 0.7282(4) 0.4607(4) 0.0480(13) Uani 1 1 d . . . H21A H 0.2911 0.7886 0.5103 0.058 Uiso 1 1 calc R . . C22 C 0.2833(7) 0.6258(4) 0.4679(4) 0.0447(13) Uani 1 1 d . . . H22A H 0.2546 0.6159 0.5214 0.054 Uiso 1 1 calc R . . C23 C 0.3053(6) 0.5382(4) 0.3912(3) 0.0359(11) Uani 1 1 d . . . C24 C 0.2902(6) 0.4199(4) 0.3744(3) 0.0322(10) Uani 1 1 d . . . C25 C 0.2681(6) 0.2735(4) 0.4244(3) 0.0310(10) Uani 1 1 d . . . C26 C 0.2260(6) 0.2191(4) 0.4893(3) 0.0329(10) Uani 1 1 d . . . C27 C 0.1556(7) 0.2538(4) 0.5691(3) 0.0431(12) Uani 1 1 d . . . H27A H 0.1228 0.3233 0.5901 0.052 Uiso 1 1 calc R . . C28 C 0.1352(7) 0.1836(5) 0.6167(4) 0.0498(14) Uani 1 1 d . . . H28A H 0.0879 0.2059 0.6708 0.060 Uiso 1 1 calc R . . C29 C 0.1831(8) 0.0802(5) 0.5863(4) 0.0543(15) Uani 1 1 d . . . H29A H 0.1697 0.0345 0.6208 0.065 Uiso 1 1 calc R . . C30 C 0.2511(7) 0.0436(4) 0.5050(4) 0.0462(13) Uani 1 1 d . . . H30A H 0.2829 -0.0262 0.4836 0.055 Uiso 1 1 calc R . . C31 C 0.2696(6) 0.1151(4) 0.4574(3) 0.0334(10) Uani 1 1 d . . . C32 C 0.3350(6) 0.1027(4) 0.3692(3) 0.0316(10) Uani 1 1 d . . . C33 C 0.6681(7) 0.4495(6) 0.2950(4) 0.0613(17) Uani 1 1 d . . . H33A H 0.6589 0.3890 0.3181 0.074 Uiso 1 1 calc R . . H33B H 0.6635 0.5163 0.3457 0.074 Uiso 1 1 calc R . . C34 C 0.8328(8) 0.4554(7) 0.2593(6) 0.085(2) Uani 1 1 d . . . H34A H 0.9270 0.4653 0.3088 0.127 Uiso 1 1 calc R . . H34B H 0.8410 0.5158 0.2370 0.127 Uiso 1 1 calc R . . H34C H 0.8361 0.3890 0.2091 0.127 Uiso 1 1 calc R . . C35 C 0.7197(6) 0.1113(5) 0.2193(4) 0.0495(14) Uani 1 1 d . . . H35A H 0.6639 0.1635 0.1967 0.059 Uiso 1 1 calc R . . H35B H 0.7271 0.0477 0.1661 0.059 Uiso 1 1 calc R . . C36 C 0.8936(7) 0.1606(6) 0.2723(5) 0.0671(18) Uani 1 1 d . . . H36A H 0.9607 0.1818 0.2324 0.101 Uiso 1 1 calc R . . H36B H 0.9477 0.1082 0.2942 0.101 Uiso 1 1 calc R . . H36C H 0.8848 0.2236 0.3246 0.101 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 Ni1 0.0333(3) 0.0273(3) 0.0232(3) 0.0047(2) -0.0003(2) 0.0014(2) N1 0.033(2) 0.027(2) 0.0230(19) 0.0046(16) 0.0008(15) 0.0031(16) N2 0.038(2) 0.034(2) 0.0228(19) 0.0068(16) 0.0008(16) 0.0058(17) N3 0.037(2) 0.027(2) 0.031(2) 0.0081(17) 0.0016(17) 0.0026(16) N4 0.037(2) 0.030(2) 0.0250(19) 0.0076(16) 0.0026(16) 0.0034(16) N5 0.039(2) 0.034(2) 0.027(2) 0.0061(17) -0.0015(16) 0.0019(17) N6 0.046(2) 0.035(2) 0.029(2) 0.0103(18) 0.0003(18) 0.0052(18) N7 0.042(2) 0.032(2) 0.031(2) 0.0077(17) 0.0067(17) 0.0054(17) N8 0.040(2) 0.030(2) 0.027(2) 0.0072(17) 0.0028(17) 0.0052(17) O1 0.0327(17) 0.0418(19) 0.0324(17) 0.0120(15) -0.0026(14) 0.0000(14) O2 0.0410(19) 0.043(2) 0.039(2) 0.0075(16) 0.0034(15) 0.0013(15) C1 0.034(2) 0.028(2) 0.032(2) 0.0092(19) 0.0006(19) 0.0049(19) C2 0.033(2) 0.031(2) 0.031(2) 0.009(2) 0.0041(19) 0.0025(19) C3 0.044(3) 0.036(3) 0.038(3) 0.013(2) 0.007(2) 0.008(2) C4 0.056(3) 0.040(3) 0.051(3) 0.012(3) 0.014(3) 0.017(3) C5 0.066(4) 0.032(3) 0.045(3) 0.004(2) 0.016(3) 0.011(3) C6 0.059(3) 0.038(3) 0.026(2) 0.004(2) 0.011(2) 0.006(2) C8 0.032(2) 0.031(2) 0.029(2) 0.005(2) 0.0049(19) 0.0008(19) C7 0.037(3) 0.031(3) 0.033(3) 0.008(2) 0.009(2) 0.003(2) C9 0.031(2) 0.035(3) 0.025(2) 0.004(2) 0.0035(18) 0.0009(19) C10 0.029(2) 0.040(3) 0.032(3) 0.012(2) -0.0011(19) 0.002(2) C11 0.037(3) 0.050(3) 0.030(3) 0.012(2) 0.000(2) -0.001(2) C12 0.041(3) 0.062(4) 0.028(3) 0.014(2) -0.003(2) -0.004(3) C13 0.050(3) 0.070(4) 0.040(3) 0.028(3) -0.006(2) 0.012(3) C14 0.059(3) 0.047(3) 0.042(3) 0.019(3) 0.000(3) 0.016(3) C15 0.041(3) 0.044(3) 0.029(2) 0.011(2) 0.002(2) 0.009(2) C16 0.037(3) 0.040(3) 0.027(2) 0.013(2) 0.0019(19) 0.008(2) C17 0.042(3) 0.028(2) 0.030(2) 0.008(2) 0.001(2) 0.003(2) C18 0.036(3) 0.030(3) 0.031(2) 0.006(2) -0.002(2) 0.002(2) C19 0.048(3) 0.034(3) 0.039(3) 0.011(2) -0.002(2) 0.002(2) C20 0.058(3) 0.030(3) 0.047(3) 0.010(2) 0.001(3) 0.004(2) C21 0.064(4) 0.026(3) 0.043(3) 0.000(2) 0.001(3) 0.010(2) C22 0.056(3) 0.037(3) 0.036(3) 0.005(2) 0.006(2) 0.015(2) C23 0.038(3) 0.026(2) 0.036(3) 0.003(2) -0.001(2) 0.005(2) C24 0.037(3) 0.027(2) 0.028(2) 0.0052(19) -0.0019(19) 0.0038(19) C25 0.032(2) 0.030(2) 0.026(2) 0.0046(19) 0.0010(19) 0.0008(19) C26 0.031(2) 0.036(3) 0.029(2) 0.010(2) -0.0022(19) -0.001(2) C27 0.051(3) 0.046(3) 0.031(3) 0.012(2) 0.007(2) 0.005(2) C28 0.057(3) 0.061(4) 0.031(3) 0.013(3) 0.013(2) 0.002(3) C29 0.067(4) 0.060(4) 0.041(3) 0.025(3) 0.011(3) 0.001(3) C30 0.061(3) 0.041(3) 0.038(3) 0.017(2) 0.007(2) 0.003(3) C31 0.037(3) 0.034(3) 0.026(2) 0.010(2) 0.0010(19) -0.002(2) C32 0.033(2) 0.031(3) 0.030(2) 0.014(2) -0.0035(19) -0.0003(19) C33 0.045(3) 0.070(4) 0.055(4) 0.010(3) -0.003(3) -0.001(3) C34 0.048(4) 0.090(6) 0.090(6) -0.003(4) 0.013(4) 0.002(4) C35 0.039(3) 0.058(4) 0.047(3) 0.015(3) 0.005(2) -0.003(3) C36 0.043(3) 0.073(5) 0.071(4) 0.013(4) 0.002(3) -0.013(3) _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 N1 1.831(4) . ? Ni1 N3 1.838(4) . ? Ni1 N2 1.854(4) . ? Ni1 N4 1.862(4) . ? N1 C8 1.323(6) . ? N1 C1 1.469(6) . ? N2 C9 1.362(6) . ? N2 C16 1.399(6) . ? N3 C24 1.306(6) . ? N3 C17 1.478(6) . ? N4 C25 1.367(6) . ? N4 C32 1.407(6) . ? N5 C9 1.315(6) . ? N5 C8 1.349(6) . ? N6 C16 1.281(6) . ? N6 C17 1.452(6) . ? N7 C25 1.319(6) . ? N7 C24 1.346(6) . ? N8 C32 1.282(6) . ? N8 C1 1.449(6) . ? O1 C35 1.425(6) . ? O1 C1 1.425(5) . ? O2 C17 1.414(6) . ? O2 C33 1.422(6) . ? C1 C2 1.517(6) . ? C2 C3 1.371(7) . ? C2 C7 1.381(6) . ? C3 C4 1.390(7) . ? C4 C5 1.379(8) . ? C5 C6 1.374(7) . ? C6 C7 1.398(6) . ? C8 C7 1.459(6) . ? C9 C10 1.475(6) . ? C10 C15 1.373(7) . ? C10 C11 1.392(6) . ? C11 C12 1.375(7) . ? C12 C13 1.370(8) . ? C13 C14 1.400(8) . ? C14 C15 1.370(7) . ? C15 C16 1.473(6) . ? C17 C18 1.519(6) . ? C18 C19 1.366(7) . ? C18 C23 1.370(7) . ? C19 C20 1.386(7) . ? C20 C21 1.365(8) . ? C21 C22 1.381(7) . ? C22 C23 1.392(7) . ? C23 C24 1.477(6) . ? C25 C26 1.464(6) . ? C26 C31 1.374(6) . ? C26 C27 1.375(7) . ? C27 C28 1.363(7) . ? C28 C29 1.380(8) . ? C29 C30 1.386(8) . ? C30 C31 1.377(7) . ? C31 C32 1.484(6) . ? C33 C34 1.495(8) . ? C35 C36 1.485(7) . ? 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 N1 Ni1 N3 172.58(17) . . ? N1 Ni1 N2 90.49(16) . . ? N3 Ni1 N2 90.76(17) . . ? N1 Ni1 N4 90.30(16) . . ? N3 Ni1 N4 90.23(17) . . ? N2 Ni1 N4 166.26(16) . . ? C8 N1 C1 110.4(4) . . ? C8 N1 Ni1 128.0(3) . . ? C1 N1 Ni1 121.3(3) . . ? C9 N2 C16 108.3(4) . . ? C9 N2 Ni1 123.8(3) . . ? C16 N2 Ni1 125.1(3) . . ? C24 N3 C17 110.7(4) . . ? C24 N3 Ni1 128.2(3) . . ? C17 N3 Ni1 121.1(3) . . ? C25 N4 C32 108.2(4) . . ? C25 N4 Ni1 122.6(3) . . ? C32 N4 Ni1 125.1(3) . . ? C9 N5 C8 118.2(4) . . ? C16 N6 C17 116.7(4) . . ? C25 N7 C24 118.4(4) . . ? C32 N8 C1 116.0(4) . . ? C35 O1 C1 116.1(4) . . ? C17 O2 C33 116.2(4) . . ? O1 C1 N8 103.8(3) . . ? O1 C1 N1 110.7(4) . . ? N8 C1 N1 113.5(4) . . ? O1 C1 C2 113.7(4) . . ? N8 C1 C2 112.3(4) . . ? N1 C1 C2 103.2(4) . . ? C3 C2 C7 121.0(4) . . ? C3 C2 C1 130.7(4) . . ? C7 C2 C1 108.3(4) . . ? C2 C3 C4 118.2(5) . . ? C5 C4 C3 120.7(5) . . ? C6 C5 C4 121.8(5) . . ? C5 C6 C7 117.2(5) . . ? N1 C8 N5 126.9(4) . . ? N1 C8 C7 110.6(4) . . ? N5 C8 C7 122.5(4) . . ? C2 C7 C6 121.2(4) . . ? C2 C7 C8 107.4(4) . . ? C6 C7 C8 131.4(5) . . ? N5 C9 N2 128.0(4) . . ? N5 C9 C10 122.8(4) . . ? N2 C9 C10 109.1(4) . . ? C15 C10 C11 121.3(5) . . ? C15 C10 C9 107.4(4) . . ? C11 C10 C9 131.3(5) . . ? C12 C11 C10 117.1(5) . . ? C13 C12 C11 121.8(5) . . ? C12 C13 C14 120.8(5) . . ? C15 C14 C13 117.4(5) . . ? C14 C15 C10 121.5(5) . . ? C14 C15 C16 131.7(5) . . ? C10 C15 C16 106.8(4) . . ? N6 C16 N2 128.8(4) . . ? N6 C16 C15 122.8(4) . . ? N2 C16 C15 108.4(4) . . ? O2 C17 N6 103.8(4) . . ? O2 C17 N3 111.8(4) . . ? N6 C17 N3 113.1(4) . . ? O2 C17 C18 113.6(4) . . ? N6 C17 C18 111.8(4) . . ? N3 C17 C18 103.0(4) . . ? C19 C18 C23 121.3(4) . . ? C19 C18 C17 130.2(4) . . ? C23 C18 C17 108.5(4) . . ? C18 C19 C20 118.0(5) . . ? C21 C20 C19 120.8(5) . . ? C20 C21 C22 121.9(5) . . ? C21 C22 C23 116.7(5) . . ? C18 C23 C22 121.3(5) . . ? C18 C23 C24 107.4(4) . . ? C22 C23 C24 131.3(5) . . ? N3 C24 N7 126.8(4) . . ? N3 C24 C23 110.5(4) . . ? N7 C24 C23 122.7(4) . . ? N7 C25 N4 128.0(4) . . ? N7 C25 C26 122.5(4) . . ? N4 C25 C26 109.6(4) . . ? C31 C26 C27 120.5(5) . . ? C31 C26 C25 107.5(4) . . ? C27 C26 C25 132.0(5) . . ? C28 C27 C26 118.3(5) . . ? C27 C28 C29 121.5(5) . . ? C28 C29 C30 120.8(5) . . ? C31 C30 C29 117.0(5) . . ? C26 C31 C30 121.9(5) . . ? C26 C31 C32 106.9(4) . . ? C30 C31 C32 131.1(5) . . ? N8 C32 N4 128.3(4) . . ? N8 C32 C31 124.0(4) . . ? N4 C32 C31 107.7(4) . . ? O2 C33 C34 107.9(5) . . ? O1 C35 C36 107.6(5) . . ? 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 N3 Ni1 N1 C8 -110.3(13) . . . . ? N2 Ni1 N1 C8 -10.7(4) . . . . ? N4 Ni1 N1 C8 155.6(4) . . . . ? N3 Ni1 N1 C1 62.9(14) . . . . ? N2 Ni1 N1 C1 162.5(3) . . . . ? N4 Ni1 N1 C1 -31.2(3) . . . . ? N1 Ni1 N2 C9 22.1(4) . . . . ? N3 Ni1 N2 C9 -165.3(4) . . . . ? N4 Ni1 N2 C9 -71.2(8) . . . . ? N1 Ni1 N2 C16 -178.8(4) . . . . ? N3 Ni1 N2 C16 -6.1(4) . . . . ? N4 Ni1 N2 C16 88.0(8) . . . . ? N1 Ni1 N3 C24 -108.1(13) . . . . ? N2 Ni1 N3 C24 152.3(4) . . . . ? N4 Ni1 N3 C24 -14.0(4) . . . . ? N1 Ni1 N3 C17 67.8(14) . . . . ? N2 Ni1 N3 C17 -31.8(3) . . . . ? N4 Ni1 N3 C17 161.9(3) . . . . ? N1 Ni1 N4 C25 -162.5(4) . . . . ? N3 Ni1 N4 C25 24.9(4) . . . . ? N2 Ni1 N4 C25 -69.2(8) . . . . ? N1 Ni1 N4 C32 -7.6(4) . . . . ? N3 Ni1 N4 C32 179.8(4) . . . . ? N2 Ni1 N4 C32 85.7(8) . . . . ? C35 O1 C1 N8 -172.7(4) . . . . ? C35 O1 C1 N1 -50.6(5) . . . . ? C35 O1 C1 C2 65.0(5) . . . . ? C32 N8 C1 O1 75.2(5) . . . . ? C32 N8 C1 N1 -45.1(5) . . . . ? C32 N8 C1 C2 -161.6(4) . . . . ? C8 N1 C1 O1 119.6(4) . . . . ? Ni1 N1 C1 O1 -54.7(5) . . . . ? C8 N1 C1 N8 -124.2(4) . . . . ? Ni1 N1 C1 N8 61.5(5) . . . . ? C8 N1 C1 C2 -2.4(5) . . . . ? Ni1 N1 C1 C2 -176.7(3) . . . . ? O1 C1 C2 C3 62.1(6) . . . . ? N8 C1 C2 C3 -55.3(6) . . . . ? N1 C1 C2 C3 -177.9(5) . . . . ? O1 C1 C2 C7 -118.5(4) . . . . ? N8 C1 C2 C7 124.1(4) . . . . ? N1 C1 C2 C7 1.5(5) . . . . ? C7 C2 C3 C4 -0.7(7) . . . . ? C1 C2 C3 C4 178.6(5) . . . . ? C2 C3 C4 C5 0.5(8) . . . . ? C3 C4 C5 C6 -0.2(9) . . . . ? C4 C5 C6 C7 0.1(8) . . . . ? C1 N1 C8 N5 -178.0(4) . . . . ? Ni1 N1 C8 N5 -4.2(7) . . . . ? C1 N1 C8 C7 2.5(5) . . . . ? Ni1 N1 C8 C7 176.3(3) . . . . ? C9 N5 C8 N1 11.6(7) . . . . ? C9 N5 C8 C7 -168.9(4) . . . . ? C3 C2 C7 C6 0.6(7) . . . . ? C1 C2 C7 C6 -178.8(4) . . . . ? C3 C2 C7 C8 179.3(4) . . . . ? C1 C2 C7 C8 -0.1(5) . . . . ? C5 C6 C7 C2 -0.3(7) . . . . ? C5 C6 C7 C8 -178.7(5) . . . . ? N1 C8 C7 C2 -1.5(5) . . . . ? N5 C8 C7 C2 178.9(4) . . . . ? N1 C8 C7 C6 177.0(5) . . . . ? N5 C8 C7 C6 -2.5(8) . . . . ? C8 N5 C9 N2 2.6(7) . . . . ? C8 N5 C9 C10 179.4(4) . . . . ? C16 N2 C9 N5 175.4(4) . . . . ? Ni1 N2 C9 N5 -22.5(7) . . . . ? C16 N2 C9 C10 -1.8(5) . . . . ? Ni1 N2 C9 C10 160.4(3) . . . . ? N5 C9 C10 C15 -176.0(4) . . . . ? N2 C9 C10 C15 1.3(5) . . . . ? N5 C9 C10 C11 4.6(8) . . . . ? N2 C9 C10 C11 -178.2(5) . . . . ? C15 C10 C11 C12 1.0(7) . . . . ? C9 C10 C11 C12 -179.7(5) . . . . ? C10 C11 C12 C13 0.8(8) . . . . ? C11 C12 C13 C14 -0.9(9) . . . . ? C12 C13 C14 C15 -0.8(8) . . . . ? C13 C14 C15 C10 2.6(8) . . . . ? C13 C14 C15 C16 -179.9(5) . . . . ? C11 C10 C15 C14 -2.7(8) . . . . ? C9 C10 C15 C14 177.8(5) . . . . ? C11 C10 C15 C16 179.2(4) . . . . ? C9 C10 C15 C16 -0.3(5) . . . . ? C17 N6 C16 N2 4.3(7) . . . . ? C17 N6 C16 C15 -173.7(4) . . . . ? C9 N2 C16 N6 -176.6(5) . . . . ? Ni1 N2 C16 N6 21.5(7) . . . . ? C9 N2 C16 C15 1.6(5) . . . . ? Ni1 N2 C16 C15 -160.3(3) . . . . ? C14 C15 C16 N6 -0.3(9) . . . . ? C10 C15 C16 N6 177.5(5) . . . . ? C14 C15 C16 N2 -178.6(5) . . . . ? C10 C15 C16 N2 -0.8(5) . . . . ? C33 O2 C17 N6 -178.5(4) . . . . ? C33 O2 C17 N3 -56.2(5) . . . . ? C33 O2 C17 C18 59.8(6) . . . . ? C16 N6 C17 O2 77.7(5) . . . . ? C16 N6 C17 N3 -43.7(6) . . . . ? C16 N6 C17 C18 -159.4(4) . . . . ? C24 N3 C17 O2 120.2(4) . . . . ? Ni1 N3 C17 O2 -56.4(5) . . . . ? C24 N3 C17 N6 -123.0(4) . . . . ? Ni1 N3 C17 N6 60.4(5) . . . . ? C24 N3 C17 C18 -2.2(5) . . . . ? Ni1 N3 C17 C18 -178.7(3) . . . . ? O2 C17 C18 C19 60.3(6) . . . . ? N6 C17 C18 C19 -56.9(7) . . . . ? N3 C17 C18 C19 -178.6(5) . . . . ? O2 C17 C18 C23 -119.4(4) . . . . ? N6 C17 C18 C23 123.4(4) . . . . ? N3 C17 C18 C23 1.7(5) . . . . ? C23 C18 C19 C20 0.7(7) . . . . ? C17 C18 C19 C20 -178.9(5) . . . . ? C18 C19 C20 C21 -0.9(8) . . . . ? C19 C20 C21 C22 1.0(9) . . . . ? C20 C21 C22 C23 -0.9(8) . . . . ? C19 C18 C23 C22 -0.7(7) . . . . ? C17 C18 C23 C22 179.0(4) . . . . ? C19 C18 C23 C24 179.6(4) . . . . ? C17 C18 C23 C24 -0.7(5) . . . . ? C21 C22 C23 C18 0.8(7) . . . . ? C21 C22 C23 C24 -179.6(5) . . . . ? C17 N3 C24 N7 -178.5(4) . . . . ? Ni1 N3 C24 N7 -2.2(7) . . . . ? C17 N3 C24 C23 1.8(5) . . . . ? Ni1 N3 C24 C23 178.1(3) . . . . ? C25 N7 C24 N3 12.3(7) . . . . ? C25 N7 C24 C23 -168.1(4) . . . . ? C18 C23 C24 N3 -0.7(5) . . . . ? C22 C23 C24 N3 179.6(5) . . . . ? C18 C23 C24 N7 179.6(4) . . . . ? C22 C23 C24 N7 -0.1(8) . . . . ? C24 N7 C25 N4 2.0(7) . . . . ? C24 N7 C25 C26 -179.7(4) . . . . ? C32 N4 C25 N7 177.3(4) . . . . ? Ni1 N4 C25 N7 -24.1(6) . . . . ? C32 N4 C25 C26 -1.2(5) . . . . ? Ni1 N4 C25 C26 157.3(3) . . . . ? N7 C25 C26 C31 -176.6(4) . . . . ? N4 C25 C26 C31 2.0(5) . . . . ? N7 C25 C26 C27 3.7(8) . . . . ? N4 C25 C26 C27 -177.7(5) . . . . ? C31 C26 C27 C28 1.8(7) . . . . ? C25 C26 C27 C28 -178.5(5) . . . . ? C26 C27 C28 C29 -0.1(8) . . . . ? C27 C28 C29 C30 -1.2(9) . . . . ? C28 C29 C30 C31 0.6(8) . . . . ? C27 C26 C31 C30 -2.5(7) . . . . ? C25 C26 C31 C30 177.8(4) . . . . ? C27 C26 C31 C32 177.9(4) . . . . ? C25 C26 C31 C32 -1.8(5) . . . . ? C29 C30 C31 C26 1.2(8) . . . . ? C29 C30 C31 C32 -179.3(5) . . . . ? C1 N8 C32 N4 4.6(7) . . . . ? C1 N8 C32 C31 -174.8(4) . . . . ? C25 N4 C32 N8 -179.4(4) . . . . ? Ni1 N4 C32 N8 22.7(7) . . . . ? C25 N4 C32 C31 0.1(5) . . . . ? Ni1 N4 C32 C31 -157.8(3) . . . . ? C26 C31 C32 N8 -179.4(4) . . . . ? C30 C31 C32 N8 1.0(8) . . . . ? C26 C31 C32 N4 1.2(5) . . . . ? C30 C31 C32 N4 -178.4(5) . . . . ? C17 O2 C33 C34 -170.8(5) . . . . ? C1 O1 C35 C36 -173.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.706 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.095