Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 _publ_contact_author_name 'Prof. M. Julve' _publ_contact_author_address ; Prof. M. Julve Departament de Quimica Inorganica/Instituto de Ciencia Molecular Facultat de Quimica, Dr. Moliner 50 46100 Burjassot, Valencia Spain ; _publ_contact_author_phone +34963864856 _publ_contact_author_fax +34963544322 _publ_contact_author_email miguel.julve@uv.es _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis, Crystal Structures and Magnetic Properties of Cyanide- and Phenolate-Bridged [MIIINiII]2 Tetranuclear Complexes (M = Fe and Cr) ; loop_ _publ_author_name _publ_author_address 'Liviu Toma' ; Departament de Quimica Inorganica/Instituto de Ciencia Molecular Facultat de Quimica, Dr. Moliner 50 46100 Burjassot, Valencia Spain ; 'Luminita Marilena Toma' ; Departament de Quimica Inorganica/Instituto de Ciencia Molecular Facultat de Quimica, Dr. Moliner 50 46100 Burjassot, Valencia Spain ; 'Rodrigue Lescouezec' ; Departament de Quimica Inorganica/Instituto de Ciencia Molecular Facultat de Quimica, Dr. Moliner 50 46100 Burjassot, Valencia Spain ; 'Donatella Armentano' ; Dipartimento di Chimica Universita degli Studi della Calabria I-87030 Arcavacata di Rende, Cosenza Italy ; 'Giovanni De Munno' ; Dipartimento di Chimica Universita degli Studi della Calabria I-87030 Arcavacata di Rende, Cosenza Italy ; 'Marius Andruh' ; Inorganic Chemistry Laboratory, Faculty of Chemistry, University of Bucarest Str. Dumbrava Rosie nr. 23, 020464 Bucharest, Romania ; 'Joan Cano' ; Institucio Catalana de Recerca i Estudis Avancats (ICREA)/Departament de Quimica Inorganica and Centre de Recerca en Quimica Teorica Universitat de Barcelona, Diagonal 647, 08028 Spain ; 'Francesc Lloret' ; Departament de Quimica Inorganica/Instituto de Ciencia Molecular Facultat de Quimica, Dr. Moliner 50 46100 Burjassot, Valencia Spain ; 'Miguel Julve' ; Departament de Quimica Inorganica/Instituto de Ciencia Molecular Facultat de Quimica, Dr. Moliner 50 46100 Burjassot, Valencia Spain ; data_2 _database_code_depnum_ccdc_archive 'CCDC 259752' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H26 Fe N9 Ni O2' _chemical_formula_weight 659.16 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' Fe Fe 0.3463 0.8444 '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 9.841(2) _cell_length_b 11.514(2) _cell_length_c 14.595(3) _cell_angle_alpha 100.95(3) _cell_angle_beta 103.44(3) _cell_angle_gamma 109.17(3) _cell_volume 1454.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 15 _cell_measurement_theta_max 30 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 678 _exptl_absorpt_coefficient_mu 1.192 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'R3m/V automatic four-circle diffractometer' _diffrn_measurement_method omega/2-theta-scans _diffrn_standards_decay_% 2.9 _diffrn_reflns_number 6124 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.05 _reflns_number_total 5739 _reflns_number_gt 4246 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0743P)^2^+0.0000P] 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 5739 _refine_ls_number_parameters 403 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.928 _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 Fe1 Fe -0.14858(5) 0.21134(4) 0.30039(3) 0.03232(13) Uani 1 1 d . . . N1 N 0.0562(3) 0.2960(3) 0.40300(18) 0.0370(6) Uani 1 1 d . . . N2 N -0.1180(3) 0.0519(3) 0.31797(19) 0.0399(6) Uani 1 1 d . . . C1 C 0.1410(4) 0.4205(3) 0.4469(2) 0.0444(8) Uani 1 1 d . . . H1A H 0.1008 0.4804 0.4335 0.053 Uiso 1 1 calc R . . C2 C 0.2863(4) 0.4638(4) 0.5113(3) 0.0599(10) Uani 1 1 d . . . H2A H 0.3417 0.5515 0.5406 0.072 Uiso 1 1 calc R . . C3 C 0.3484(4) 0.3794(5) 0.5321(3) 0.0631(11) Uani 1 1 d . . . H3A H 0.4470 0.4089 0.5746 0.076 Uiso 1 1 calc R . . C4 C 0.2635(4) 0.2468(4) 0.4893(2) 0.0507(9) Uani 1 1 d . . . C5 C 0.3152(5) 0.1491(5) 0.5074(3) 0.0658(12) Uani 1 1 d . . . H5A H 0.4135 0.1723 0.5483 0.079 Uiso 1 1 calc R . . C6 C 0.2246(5) 0.0233(5) 0.4664(3) 0.0662(13) Uani 1 1 d . . . H6A H 0.2612 -0.0383 0.4806 0.079 Uiso 1 1 calc R . . C7 C 0.0730(5) -0.0171(4) 0.4014(3) 0.0512(9) Uani 1 1 d . . . C8 C -0.0285(6) -0.1450(4) 0.3559(3) 0.0624(11) Uani 1 1 d . . . H8A H -0.0009 -0.2119 0.3679 0.075 Uiso 1 1 calc R . . C9 C -0.1681(5) -0.1701(4) 0.2937(3) 0.0645(12) Uani 1 1 d . . . H9A H -0.2358 -0.2549 0.2630 0.077 Uiso 1 1 calc R . . C10 C -0.2110(4) -0.0705(3) 0.2755(3) 0.0512(9) Uani 1 1 d . . . H10A H -0.3069 -0.0902 0.2326 0.061 Uiso 1 1 calc R . . C11 C 0.0219(4) 0.0788(3) 0.3805(2) 0.0390(7) Uani 1 1 d . . . C12 C 0.1168(4) 0.2100(3) 0.4257(2) 0.0395(7) Uani 1 1 d . . . N8 N 0.2391(3) 0.2873(2) 0.04106(19) 0.0396(6) Uani 1 1 d . . . C13 C -0.2535(4) 0.2134(3) 0.3984(2) 0.0410(7) Uani 1 1 d . . . N3 N -0.3180(4) 0.2157(3) 0.4536(2) 0.0616(9) Uani 1 1 d . . . C14 C -0.1661(4) 0.3690(3) 0.2861(2) 0.0409(7) Uani 1 1 d . . . N4 N -0.1737(4) 0.4641(3) 0.2787(3) 0.0661(9) Uani 1 1 d . . . C15 C -0.3394(4) 0.1205(3) 0.1990(2) 0.0398(7) Uani 1 1 d . . . N5 N -0.4518(3) 0.0627(3) 0.1354(2) 0.0557(8) Uani 1 1 d . . . C16 C -0.0499(3) 0.2059(3) 0.1984(2) 0.0336(7) Uani 1 1 d . . . N6 N 0.0063(3) 0.1923(3) 0.13935(19) 0.0374(6) Uani 1 1 d . . . Ni1 Ni 0.13849(4) 0.12199(3) 0.06799(3) 0.02798(12) Uani 1 1 d . . . N7 N 0.2892(3) 0.1543(2) 0.20035(18) 0.0345(6) Uani 1 1 d . . . C17 C 0.2995(3) 0.0636(3) 0.2357(2) 0.0365(7) Uani 1 1 d . . . H17A H 0.3805 0.0873 0.2927 0.044 Uiso 1 1 calc R . . C18 C 0.2015(3) -0.0722(3) 0.1990(2) 0.0350(7) Uani 1 1 d . . . C19 C 0.2481(4) -0.1528(3) 0.2487(2) 0.0432(8) Uani 1 1 d . . . H19A H 0.3405 -0.1166 0.2991 0.052 Uiso 1 1 calc R . . C20 C 0.1644(4) -0.2822(3) 0.2270(3) 0.0464(8) Uani 1 1 d . . . C21 C 0.0249(4) -0.3329(3) 0.1547(3) 0.0457(8) Uani 1 1 d . . . H21A H -0.0365 -0.4190 0.1415 0.055 Uiso 1 1 calc R . . C22 C -0.0279(4) -0.2593(3) 0.1004(2) 0.0362(7) Uani 1 1 d . . . C23 C 0.0619(3) -0.1270(3) 0.1198(2) 0.0310(6) Uani 1 1 d . . . C24 C 0.2212(5) -0.3647(4) 0.2824(3) 0.0662(12) Uani 1 1 d . . . H24A H 0.3197 -0.3130 0.3295 0.099 Uiso 1 1 calc R . . H24B H 0.2278 -0.4331 0.2368 0.099 Uiso 1 1 calc R . . H24C H 0.1520 -0.4003 0.3161 0.099 Uiso 1 1 calc R . . O1 O 0.0164(2) -0.05686(18) 0.06890(14) 0.0316(4) Uani 1 1 d . . . O2 O 0.2803(3) 0.0509(2) 0.00323(17) 0.0466(6) Uani 1 1 d D . . H1W H 0.374(2) 0.049(3) 0.037(2) 0.060 Uiso 1 1 d D . . H2W H 0.241(4) -0.019(2) -0.0543(16) 0.060 Uiso 1 1 d D . . C25 C 0.4092(4) 0.2836(3) 0.2560(2) 0.0473(9) Uani 1 1 d . . . H25A H 0.4019 0.3063 0.3216 0.057 Uiso 1 1 calc R . . H25B H 0.5073 0.2784 0.2628 0.057 Uiso 1 1 calc R . . C26 C 0.4037(5) 0.3874(4) 0.2119(3) 0.0661(12) Uani 1 1 d . . . H26A H 0.4928 0.4642 0.2507 0.079 Uiso 1 1 calc R . . H26B H 0.3160 0.4046 0.2190 0.079 Uiso 1 1 calc R . . C27 C 0.3963(4) 0.3687(4) 0.1076(3) 0.0643(12) Uani 1 1 d . . . H27A H 0.4645 0.3280 0.0942 0.077 Uiso 1 1 calc R . . H27B H 0.4291 0.4515 0.0950 0.077 Uiso 1 1 calc R . . C28 C 0.1786(4) 0.3262(3) -0.0272(3) 0.0451(8) Uani 1 1 d . . . H28A H 0.2368 0.4060 -0.0310 0.054 Uiso 1 1 calc R . . C29 C 0.2922(7) 0.7322(6) 0.0014(4) 0.0788(14) Uani 1 1 d . . . H29A H 0.345(5) 0.793(4) -0.019(3) 0.060 Uiso 1 1 d . . . H29B H 0.197(5) 0.698(4) 0.008(3) 0.060 Uiso 1 1 d . . . H29C H 0.268(4) 0.662(4) -0.060(3) 0.060 Uiso 1 1 d . . . C30 C 0.3995(6) 0.7074(4) 0.0713(4) 0.0726(13) Uani 1 1 d . . . N9 N 0.4834(6) 0.6892(5) 0.1270(5) 0.119(2) Uani 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 Fe1 0.0313(2) 0.0390(3) 0.0278(2) 0.00615(18) 0.00782(18) 0.0181(2) N1 0.0393(14) 0.0459(15) 0.0283(13) 0.0087(11) 0.0105(11) 0.0210(12) N2 0.0466(16) 0.0424(15) 0.0370(14) 0.0096(12) 0.0188(13) 0.0225(13) C1 0.0423(19) 0.048(2) 0.0349(17) 0.0026(15) 0.0079(15) 0.0160(16) C2 0.049(2) 0.065(2) 0.041(2) -0.0076(18) 0.0013(17) 0.014(2) C3 0.045(2) 0.090(3) 0.037(2) 0.003(2) -0.0027(17) 0.025(2) C4 0.048(2) 0.081(3) 0.0337(17) 0.0171(18) 0.0127(16) 0.039(2) C5 0.067(3) 0.111(4) 0.041(2) 0.026(2) 0.0152(19) 0.060(3) C6 0.091(3) 0.108(4) 0.053(2) 0.047(3) 0.038(2) 0.082(3) C7 0.076(3) 0.066(2) 0.046(2) 0.0307(18) 0.0365(19) 0.050(2) C8 0.099(3) 0.068(3) 0.066(3) 0.039(2) 0.055(3) 0.059(3) C9 0.090(3) 0.045(2) 0.077(3) 0.020(2) 0.051(3) 0.032(2) C10 0.057(2) 0.0399(19) 0.059(2) 0.0111(17) 0.0265(19) 0.0182(17) C11 0.0490(19) 0.0537(19) 0.0316(16) 0.0185(15) 0.0207(15) 0.0327(16) C12 0.0434(18) 0.058(2) 0.0259(15) 0.0121(14) 0.0136(13) 0.0292(16) N8 0.0355(14) 0.0346(14) 0.0369(14) 0.0061(11) 0.0051(12) 0.0057(12) C13 0.0464(19) 0.0471(19) 0.0377(18) 0.0139(15) 0.0133(15) 0.0276(16) N3 0.079(2) 0.077(2) 0.0507(19) 0.0244(17) 0.0346(18) 0.044(2) C14 0.0386(18) 0.049(2) 0.0397(18) 0.0128(15) 0.0135(14) 0.0229(15) N4 0.074(2) 0.061(2) 0.085(3) 0.0348(19) 0.034(2) 0.0402(19) C15 0.0357(18) 0.0504(19) 0.0388(18) 0.0099(15) 0.0162(15) 0.0224(15) N5 0.0334(16) 0.078(2) 0.0452(17) 0.0009(16) 0.0038(14) 0.0241(16) C16 0.0293(15) 0.0360(16) 0.0325(16) 0.0050(13) 0.0042(13) 0.0154(13) N6 0.0341(14) 0.0405(14) 0.0353(14) 0.0027(11) 0.0085(12) 0.0182(12) Ni1 0.0247(2) 0.0284(2) 0.0253(2) 0.00271(15) 0.00383(15) 0.00926(15) N7 0.0272(13) 0.0358(14) 0.0280(13) -0.0032(11) 0.0019(10) 0.0086(11) C17 0.0305(16) 0.0475(18) 0.0256(15) 0.0050(13) 0.0021(12) 0.0157(14) C18 0.0375(17) 0.0433(17) 0.0255(14) 0.0085(13) 0.0079(13) 0.0196(14) C19 0.0462(19) 0.056(2) 0.0313(16) 0.0129(15) 0.0075(14) 0.0281(17) C20 0.059(2) 0.051(2) 0.0419(19) 0.0206(16) 0.0159(17) 0.0327(18) C21 0.060(2) 0.0365(17) 0.0437(18) 0.0147(15) 0.0151(16) 0.0210(16) C22 0.0431(18) 0.0341(16) 0.0300(15) 0.0089(13) 0.0099(13) 0.0148(14) C23 0.0344(16) 0.0361(15) 0.0259(14) 0.0078(12) 0.0119(12) 0.0171(13) C24 0.090(3) 0.065(3) 0.058(2) 0.031(2) 0.016(2) 0.047(2) O1 0.0299(10) 0.0300(10) 0.0286(10) 0.0064(8) 0.0024(8) 0.0099(9) O2 0.0362(12) 0.0568(15) 0.0389(13) -0.0054(11) 0.0074(10) 0.0222(11) C25 0.0428(19) 0.0387(18) 0.0357(18) -0.0065(14) -0.0039(15) 0.0065(15) C26 0.058(2) 0.044(2) 0.060(3) -0.0021(19) -0.007(2) 0.0033(19) C27 0.044(2) 0.053(2) 0.059(2) 0.0126(19) 0.0006(18) -0.0132(18) C28 0.048(2) 0.0314(16) 0.0456(19) 0.0087(14) 0.0105(16) 0.0072(15) C29 0.094(4) 0.081(4) 0.076(3) 0.027(3) 0.039(3) 0.041(3) C30 0.079(3) 0.046(2) 0.088(3) 0.013(2) 0.026(3) 0.023(2) N9 0.098(4) 0.081(3) 0.153(5) 0.039(3) -0.006(4) 0.031(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 Fe1 C15 1.908(3) . ? Fe1 C14 1.924(4) . ? Fe1 C13 1.950(3) . ? Fe1 C16 1.959(3) . ? Fe1 N1 2.001(3) . ? Fe1 N2 2.008(3) . ? N1 C1 1.334(4) . ? N1 C12 1.366(4) . ? N2 C10 1.329(4) . ? N2 C11 1.361(4) . ? C1 C2 1.381(5) . ? C2 C3 1.352(6) . ? C3 C4 1.406(6) . ? C4 C12 1.397(5) . ? C4 C5 1.420(6) . ? C5 C6 1.351(6) . ? C6 C7 1.436(6) . ? C7 C8 1.400(6) . ? C7 C11 1.409(5) . ? C8 C9 1.362(6) . ? C9 C10 1.395(5) . ? C11 C12 1.413(5) . ? N8 C28 1.272(4) . ? N8 C27 1.490(4) . ? N8 Ni1 1.996(3) . ? C13 N3 1.137(4) . ? C14 N4 1.146(4) . ? C15 N5 1.154(4) . ? C16 N6 1.141(4) . ? N6 Ni1 2.105(3) . ? Ni1 O1 2.019(2) . ? Ni1 N7 2.025(3) . ? Ni1 O1 2.035(2) 2 ? Ni1 O2 2.141(2) . ? N7 C17 1.271(4) . ? N7 C25 1.487(4) . ? C17 C18 1.453(4) . ? C18 C19 1.407(4) . ? C18 C23 1.427(4) . ? C19 C20 1.376(5) . ? C20 C21 1.381(5) . ? C20 C24 1.516(5) . ? C21 C22 1.403(4) . ? C22 C23 1.420(4) . ? C22 C28 1.461(4) 2 ? C23 O1 1.310(3) . ? O1 Ni1 2.035(2) 2 ? C25 C26 1.472(5) . ? C26 C27 1.477(6) . ? C28 C22 1.461(4) 2 ? C29 C30 1.430(8) . ? C30 N9 1.120(6) . ? 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 C15 Fe1 C14 88.24(14) . . ? C15 Fe1 C13 89.72(14) . . ? C14 Fe1 C13 89.15(14) . . ? C15 Fe1 C16 88.32(13) . . ? C14 Fe1 C16 90.83(13) . . ? C13 Fe1 C16 178.04(13) . . ? C15 Fe1 N1 175.72(12) . . ? C14 Fe1 N1 95.33(13) . . ? C13 Fe1 N1 92.69(12) . . ? C16 Fe1 N1 89.27(11) . . ? C15 Fe1 N2 94.54(13) . . ? C14 Fe1 N2 176.89(13) . . ? C13 Fe1 N2 92.25(12) . . ? C16 Fe1 N2 87.87(12) . . ? N1 Fe1 N2 81.84(11) . . ? C1 N1 C12 117.5(3) . . ? C1 N1 Fe1 129.7(2) . . ? C12 N1 Fe1 112.7(2) . . ? C10 N2 C11 118.3(3) . . ? C10 N2 Fe1 129.3(3) . . ? C11 N2 Fe1 112.3(2) . . ? N1 C1 C2 122.4(4) . . ? C3 C2 C1 120.3(4) . . ? C2 C3 C4 119.8(3) . . ? C12 C4 C3 116.7(3) . . ? C12 C4 C5 118.4(4) . . ? C3 C4 C5 124.9(4) . . ? C6 C5 C4 121.4(4) . . ? C5 C6 C7 121.3(4) . . ? C8 C7 C11 117.0(4) . . ? C8 C7 C6 125.1(4) . . ? C11 C7 C6 117.9(4) . . ? C9 C8 C7 119.2(4) . . ? C8 C9 C10 120.9(4) . . ? N2 C10 C9 121.5(4) . . ? N2 C11 C7 123.1(3) . . ? N2 C11 C12 116.8(3) . . ? C7 C11 C12 120.1(3) . . ? N1 C12 C4 123.2(3) . . ? N1 C12 C11 116.0(3) . . ? C4 C12 C11 120.8(3) . . ? C28 N8 C27 119.2(3) . . ? C28 N8 Ni1 124.9(2) . . ? C27 N8 Ni1 115.9(2) . . ? N3 C13 Fe1 177.8(3) . . ? N4 C14 Fe1 178.7(4) . . ? N5 C15 Fe1 177.0(3) . . ? N6 C16 Fe1 174.0(3) . . ? C16 N6 Ni1 155.8(2) . . ? N8 Ni1 O1 169.65(9) . . ? N8 Ni1 N7 98.70(11) . . ? O1 Ni1 N7 91.15(10) . . ? N8 Ni1 O1 89.55(10) . 2 ? O1 Ni1 O1 80.34(9) . 2 ? N7 Ni1 O1 169.89(9) . 2 ? N8 Ni1 N6 93.84(11) . . ? O1 Ni1 N6 89.33(10) . . ? N7 Ni1 N6 89.97(10) . . ? O1 Ni1 N6 95.34(9) 2 . ? N8 Ni1 O2 87.13(11) . . ? O1 Ni1 O2 90.24(9) . . ? N7 Ni1 O2 86.89(10) . . ? O1 Ni1 O2 87.69(9) 2 . ? N6 Ni1 O2 176.82(9) . . ? C17 N7 C25 115.2(3) . . ? C17 N7 Ni1 122.4(2) . . ? C25 N7 Ni1 121.9(2) . . ? N7 C17 C18 128.7(3) . . ? C19 C18 C23 118.8(3) . . ? C19 C18 C17 116.2(3) . . ? C23 C18 C17 125.0(3) . . ? C20 C19 C18 123.6(3) . . ? C19 C20 C21 117.1(3) . . ? C19 C20 C24 121.3(3) . . ? C21 C20 C24 121.5(3) . . ? C20 C21 C22 122.5(3) . . ? C21 C22 C23 120.2(3) . . ? C21 C22 C28 116.0(3) . 2 ? C23 C22 C28 123.8(3) . 2 ? O1 C23 C22 121.3(3) . . ? O1 C23 C18 121.1(3) . . ? C22 C23 C18 117.5(3) . . ? C23 O1 Ni1 127.73(18) . . ? C23 O1 Ni1 126.45(18) . 2 ? Ni1 O1 Ni1 99.66(9) . 2 ? C26 C25 N7 115.5(3) . . ? C25 C26 C27 118.6(4) . . ? C26 C27 N8 110.9(3) . . ? N8 C28 C22 127.2(3) . 2 ? N9 C30 C29 179.1(6) . . ? 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 Fe1 C16 N6 Ni1 -32(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 O2 H2W N6 0.945(10) 2.43(3) 3.162(4) 134(3) 2 O2 H1W N5 0.945(10) 1.905(13) 2.826(4) 164(3) 1_655 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.755 _refine_diff_density_min -0.825 _refine_diff_density_rms 0.075 #==END data_3 _database_code_depnum_ccdc_archive 'CCDC 259753' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H26 Cr N9 Ni O2' _chemical_formula_weight 655.31 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' Cr Cr 0.3209 0.6236 '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 10.000(3) _cell_length_b 11.492(3) _cell_length_c 14.669(4) _cell_angle_alpha 101.02(2) _cell_angle_beta 103.63(2) _cell_angle_gamma 109.18(2) _cell_volume 1479.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 15 _cell_measurement_theta_max 30 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 674 _exptl_absorpt_coefficient_mu 1.048 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.6673 _exptl_absorpt_correction_T_max 0.7440 _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 'R3m/V automatic four-circle diffractometer' _diffrn_measurement_method omega/2-theta-scans _diffrn_standards_decay_% 1.3 _diffrn_reflns_number 6213 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.05 _reflns_number_total 5858 _reflns_number_gt 4177 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1027P)^2^+0.0000P] 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 5858 _refine_ls_number_parameters 403 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1541 _refine_ls_wR_factor_gt 0.1450 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _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 Cr1 Cr -0.15177(7) 0.21748(6) 0.30276(4) 0.03409(18) Uani 1 1 d . . . N1 N 0.0607(4) 0.2978(3) 0.4080(2) 0.0389(8) Uani 1 1 d . . . N2 N -0.1204(4) 0.0508(3) 0.3195(3) 0.0435(8) Uani 1 1 d . . . C1 C 0.1493(5) 0.4215(5) 0.4520(3) 0.0473(11) Uani 1 1 d . . . H1A H 0.1119 0.4834 0.4409 0.057 Uiso 1 1 calc R . . C2 C 0.2944(6) 0.4620(6) 0.5134(4) 0.0627(14) Uani 1 1 d . . . H2A H 0.3529 0.5494 0.5425 0.075 Uiso 1 1 calc R . . C3 C 0.3502(6) 0.3724(6) 0.5306(4) 0.0693(16) Uani 1 1 d . . . H3A H 0.4480 0.3986 0.5712 0.083 Uiso 1 1 calc R . . C4 C 0.2618(5) 0.2410(5) 0.4877(3) 0.0523(12) Uani 1 1 d . . . C5 C 0.3085(7) 0.1402(7) 0.5028(4) 0.0694(16) Uani 1 1 d . . . H5A H 0.4053 0.1609 0.5427 0.083 Uiso 1 1 calc R . . C6 C 0.2169(7) 0.0166(7) 0.4614(4) 0.0716(17) Uani 1 1 d . . . H6A H 0.2515 -0.0467 0.4734 0.086 Uiso 1 1 calc R . . C7 C 0.0684(6) -0.0210(5) 0.3996(4) 0.0547(13) Uani 1 1 d . . . C8 C -0.0341(8) -0.1488(6) 0.3530(5) 0.0727(18) Uani 1 1 d . . . H8A H -0.0071 -0.2164 0.3637 0.087 Uiso 1 1 calc R . . C9 C -0.1730(8) -0.1745(5) 0.2921(5) 0.0695(16) Uani 1 1 d . . . H9A H -0.2404 -0.2592 0.2608 0.083 Uiso 1 1 calc R . . C10 C -0.2133(6) -0.0718(5) 0.2771(4) 0.0585(13) Uani 1 1 d . . . H10A H -0.3087 -0.0903 0.2360 0.070 Uiso 1 1 calc R . . C11 C 0.0189(5) 0.0765(4) 0.3808(3) 0.0427(10) Uani 1 1 d . . . C12 C 0.1145(5) 0.2079(4) 0.4263(3) 0.0422(10) Uani 1 1 d . . . N8 N 0.2354(4) 0.2884(3) 0.0404(3) 0.0438(8) Uani 1 1 d . . . C13 C -0.2628(5) 0.2175(4) 0.4052(3) 0.0437(10) Uani 1 1 d . . . N3 N -0.3295(5) 0.2167(5) 0.4580(3) 0.0658(12) Uani 1 1 d . . . C14 C -0.1606(5) 0.3915(5) 0.2937(3) 0.0452(10) Uani 1 1 d . . . N4 N -0.1640(6) 0.4879(5) 0.2896(4) 0.0759(14) Uani 1 1 d . . . C15 C -0.3541(5) 0.1159(4) 0.1925(3) 0.0438(10) Uani 1 1 d . . . N5 N -0.4625(4) 0.0574(4) 0.1297(3) 0.0588(11) Uani 1 1 d . . . C16 C -0.0477(4) 0.2116(4) 0.1962(3) 0.0330(8) Uani 1 1 d . . . N6 N 0.0105(4) 0.1939(3) 0.1399(3) 0.0423(8) Uani 1 1 d . . . Ni1 Ni 0.13709(5) 0.12287(5) 0.06739(3) 0.03118(16) Uani 1 1 d . . . N7 N 0.2883(3) 0.1550(3) 0.1980(2) 0.0369(8) Uani 1 1 d . . . C17 C 0.2980(4) 0.0638(4) 0.2334(3) 0.0403(10) Uani 1 1 d . . . H17A H 0.3784 0.0878 0.2900 0.048 Uiso 1 1 calc R . . C18 C 0.2009(5) -0.0721(4) 0.1976(3) 0.0382(9) Uani 1 1 d . . . C19 C 0.2469(5) -0.1532(5) 0.2468(3) 0.0475(11) Uani 1 1 d . . . H19A H 0.3384 -0.1166 0.2969 0.057 Uiso 1 1 calc R . . C20 C 0.1652(6) -0.2831(5) 0.2255(3) 0.0506(11) Uani 1 1 d . . . C21 C 0.0289(6) -0.3332(5) 0.1536(3) 0.0528(12) Uani 1 1 d . . . H21A H -0.0308 -0.4199 0.1400 0.063 Uiso 1 1 calc R . . C22 C -0.0255(5) -0.2604(4) 0.0995(3) 0.0425(10) Uani 1 1 d . . . C23 C 0.0626(4) -0.1268(4) 0.1190(3) 0.0350(9) Uani 1 1 d . . . C24 C 0.2220(7) -0.3658(6) 0.2808(4) 0.0735(16) Uani 1 1 d . . . H24A H 0.1499 -0.4532 0.2559 0.110 Uiso 1 1 calc R . . H24B H 0.2368 -0.3336 0.3494 0.110 Uiso 1 1 calc R . . H24C H 0.3151 -0.3628 0.2721 0.110 Uiso 1 1 calc R . . O1 O 0.0178(3) -0.0573(2) 0.06824(18) 0.0342(6) Uani 1 1 d . . . O2 O 0.2739(3) 0.0511(3) -0.0002(2) 0.0514(8) Uani 1 1 d D . . H1W H 0.357(3) 0.040(4) 0.038(3) 0.060 Uiso 1 1 d D . . H2W H 0.230(4) -0.018(3) -0.0599(18) 0.060 Uiso 1 1 d D . . C25 C 0.4069(5) 0.2839(4) 0.2522(3) 0.0528(12) Uani 1 1 d . . . H25A H 0.3996 0.3080 0.3174 0.063 Uiso 1 1 calc R . . H25B H 0.5029 0.2772 0.2598 0.063 Uiso 1 1 calc R . . C26 C 0.4062(7) 0.3866(6) 0.2096(5) 0.089(2) Uani 1 1 d . . . H26A H 0.4986 0.4602 0.2470 0.107 Uiso 1 1 calc R . . H26B H 0.3255 0.4099 0.2211 0.107 Uiso 1 1 calc R . . C27 C 0.3910(6) 0.3715(6) 0.1059(4) 0.0767(18) Uani 1 1 d . . . H27A H 0.4588 0.3339 0.0890 0.092 Uiso 1 1 calc R . . H27B H 0.4193 0.4558 0.0952 0.092 Uiso 1 1 calc R . . C28 C 0.1745(5) 0.3272(4) -0.0273(3) 0.0506(11) Uani 1 1 d . . . H28A H 0.2315 0.4073 -0.0312 0.061 Uiso 1 1 calc R . . C29 C 0.2908(9) 0.7281(7) -0.0001(6) 0.0828(19) Uani 1 1 d . . . H29A H 0.334(6) 0.811(5) -0.001(4) 0.060 Uiso 1 1 d . . . H29B H 0.183(6) 0.716(5) -0.003(4) 0.060 Uiso 1 1 d . . . H29C H 0.272(5) 0.658(5) -0.071(4) 0.060 Uiso 1 1 d . . . C30 C 0.3989(8) 0.7094(6) 0.0696(6) 0.0811(18) Uani 1 1 d . . . N9 N 0.4824(8) 0.6924(7) 0.1252(7) 0.139(3) Uani 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 Cr1 0.0327(3) 0.0394(4) 0.0309(3) 0.0052(3) 0.0087(3) 0.0190(3) N1 0.0412(19) 0.046(2) 0.0312(17) 0.0069(15) 0.0093(15) 0.0227(16) N2 0.051(2) 0.043(2) 0.043(2) 0.0117(16) 0.0216(17) 0.0231(18) C1 0.042(2) 0.053(3) 0.039(2) 0.002(2) 0.0059(19) 0.020(2) C2 0.053(3) 0.067(3) 0.048(3) -0.004(2) 0.005(2) 0.018(3) C3 0.047(3) 0.102(5) 0.041(3) -0.003(3) -0.003(2) 0.031(3) C4 0.051(3) 0.084(4) 0.036(2) 0.020(2) 0.018(2) 0.040(3) C5 0.074(4) 0.113(5) 0.048(3) 0.029(3) 0.020(3) 0.067(4) C6 0.102(5) 0.107(5) 0.062(3) 0.048(4) 0.043(3) 0.087(4) C7 0.083(4) 0.066(3) 0.055(3) 0.033(3) 0.046(3) 0.053(3) C8 0.121(5) 0.067(4) 0.083(4) 0.043(3) 0.071(4) 0.063(4) C9 0.100(5) 0.044(3) 0.080(4) 0.017(3) 0.055(4) 0.032(3) C10 0.070(3) 0.047(3) 0.062(3) 0.014(2) 0.031(3) 0.021(3) C11 0.054(3) 0.056(3) 0.038(2) 0.021(2) 0.025(2) 0.036(2) C12 0.047(2) 0.059(3) 0.030(2) 0.0130(19) 0.0146(18) 0.030(2) N8 0.0383(19) 0.041(2) 0.0387(19) 0.0053(16) 0.0065(16) 0.0063(16) C13 0.047(2) 0.051(3) 0.041(2) 0.015(2) 0.016(2) 0.026(2) N3 0.077(3) 0.087(3) 0.058(3) 0.029(2) 0.036(2) 0.049(3) C14 0.043(2) 0.051(3) 0.046(3) 0.012(2) 0.016(2) 0.025(2) N4 0.092(4) 0.061(3) 0.106(4) 0.039(3) 0.051(3) 0.046(3) C15 0.040(2) 0.051(3) 0.042(2) 0.005(2) 0.015(2) 0.022(2) N5 0.036(2) 0.079(3) 0.050(2) -0.002(2) 0.0051(19) 0.026(2) C16 0.0290(19) 0.036(2) 0.0303(19) 0.0038(16) 0.0069(16) 0.0125(17) N6 0.0363(18) 0.043(2) 0.0391(19) 0.0007(16) 0.0061(16) 0.0159(16) Ni1 0.0264(3) 0.0319(3) 0.0286(3) 0.0011(2) 0.00534(19) 0.0101(2) N7 0.0316(17) 0.0408(19) 0.0286(17) -0.0030(15) 0.0067(14) 0.0116(15) C17 0.035(2) 0.055(3) 0.0268(19) 0.0043(19) 0.0052(17) 0.020(2) C18 0.041(2) 0.048(2) 0.029(2) 0.0079(18) 0.0133(17) 0.0213(19) C19 0.047(2) 0.065(3) 0.034(2) 0.014(2) 0.0101(19) 0.029(2) C20 0.061(3) 0.060(3) 0.046(3) 0.024(2) 0.020(2) 0.034(3) C21 0.070(3) 0.044(3) 0.046(3) 0.014(2) 0.021(2) 0.023(2) C22 0.051(3) 0.039(2) 0.039(2) 0.0125(19) 0.015(2) 0.020(2) C23 0.040(2) 0.040(2) 0.0265(19) 0.0064(16) 0.0136(17) 0.0185(18) C24 0.096(4) 0.078(4) 0.070(4) 0.039(3) 0.026(3) 0.054(4) O1 0.0321(14) 0.0321(14) 0.0295(13) 0.0041(11) 0.0024(11) 0.0097(12) O2 0.0376(16) 0.065(2) 0.0445(18) -0.0056(15) 0.0091(14) 0.0256(16) C25 0.044(3) 0.047(3) 0.040(2) -0.009(2) -0.002(2) 0.008(2) C26 0.077(4) 0.052(3) 0.084(4) 0.004(3) -0.016(4) -0.004(3) C27 0.055(3) 0.061(3) 0.068(4) 0.008(3) 0.006(3) -0.018(3) C28 0.058(3) 0.032(2) 0.053(3) 0.011(2) 0.019(2) 0.008(2) C29 0.094(5) 0.076(4) 0.088(5) 0.022(4) 0.039(4) 0.039(4) C30 0.087(5) 0.046(3) 0.101(5) 0.017(3) 0.027(4) 0.019(3) N9 0.101(5) 0.080(4) 0.198(9) 0.048(5) -0.004(5) 0.023(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 Cr1 C14 2.058(5) . ? Cr1 C15 2.063(5) . ? Cr1 C13 2.069(5) . ? Cr1 C16 2.075(4) . ? Cr1 N2 2.089(4) . ? Cr1 N1 2.091(3) . ? N1 C1 1.332(6) . ? N1 C12 1.353(5) . ? N2 C10 1.329(6) . ? N2 C11 1.369(6) . ? C1 C2 1.383(6) . ? C2 C3 1.359(8) . ? C3 C4 1.398(8) . ? C4 C12 1.414(6) . ? C4 C5 1.419(7) . ? C5 C6 1.334(9) . ? C6 C7 1.418(8) . ? C7 C8 1.404(8) . ? C7 C11 1.413(6) . ? C8 C9 1.364(8) . ? C9 C10 1.405(8) . ? C11 C12 1.416(6) . ? N8 C28 1.273(6) . ? N8 C27 1.491(6) . ? N8 Ni1 1.996(4) . ? C13 N3 1.133(6) . ? C14 N4 1.132(6) . ? C15 N5 1.136(5) . ? C16 N6 1.141(5) . ? N6 Ni1 2.093(4) . ? Ni1 N7 2.022(3) . ? Ni1 O1 2.026(3) . ? Ni1 O1 2.033(3) 2 ? Ni1 O2 2.146(3) . ? N7 C17 1.276(5) . ? N7 C25 1.478(5) . ? C17 C18 1.452(6) . ? C18 C19 1.409(6) . ? C18 C23 1.427(6) . ? C19 C20 1.376(7) . ? C20 C21 1.370(7) . ? C20 C24 1.522(6) . ? C21 C22 1.405(6) . ? C22 C23 1.428(6) . ? C22 C28 1.458(6) 2 ? C23 O1 1.303(5) . ? O1 Ni1 2.033(3) 2 ? C25 C26 1.438(8) . ? C26 C27 1.462(8) . ? C28 C22 1.458(6) 2 ? C29 C30 1.405(10) . ? C30 N9 1.118(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 Cr1 C15 92.10(18) . . ? C14 Cr1 C13 89.30(17) . . ? C15 Cr1 C13 89.73(17) . . ? C14 Cr1 C16 91.47(16) . . ? C15 Cr1 C16 88.17(16) . . ? C13 Cr1 C16 177.79(16) . . ? C14 Cr1 N2 174.36(16) . . ? C15 Cr1 N2 93.31(17) . . ? C13 Cr1 N2 92.34(16) . . ? C16 Cr1 N2 87.10(15) . . ? C14 Cr1 N1 95.11(16) . . ? C15 Cr1 N1 171.84(15) . . ? C13 Cr1 N1 94.18(15) . . ? C16 Cr1 N1 87.82(14) . . ? N2 Cr1 N1 79.40(14) . . ? C1 N1 C12 118.2(4) . . ? C1 N1 Cr1 129.0(3) . . ? C12 N1 Cr1 112.6(3) . . ? C10 N2 C11 118.1(4) . . ? C10 N2 Cr1 129.1(4) . . ? C11 N2 Cr1 112.7(3) . . ? N1 C1 C2 123.1(5) . . ? C3 C2 C1 119.1(5) . . ? C2 C3 C4 120.5(5) . . ? C3 C4 C12 116.8(5) . . ? C3 C4 C5 124.8(5) . . ? C12 C4 C5 118.5(5) . . ? C6 C5 C4 121.7(5) . . ? C5 C6 C7 121.8(5) . . ? C8 C7 C11 116.6(5) . . ? C8 C7 C6 125.1(5) . . ? C11 C7 C6 118.2(5) . . ? C9 C8 C7 120.4(5) . . ? C8 C9 C10 119.4(5) . . ? N2 C10 C9 122.5(5) . . ? N2 C11 C7 123.0(5) . . ? N2 C11 C12 116.8(4) . . ? C7 C11 C12 120.2(4) . . ? N1 C12 C4 122.4(4) . . ? N1 C12 C11 118.0(4) . . ? C4 C12 C11 119.6(4) . . ? C28 N8 C27 118.7(4) . . ? C28 N8 Ni1 124.7(3) . . ? C27 N8 Ni1 116.6(3) . . ? N3 C13 Cr1 176.8(4) . . ? N4 C14 Cr1 179.3(5) . . ? N5 C15 Cr1 177.0(4) . . ? N6 C16 Cr1 171.0(4) . . ? C16 N6 Ni1 160.0(3) . . ? N8 Ni1 N7 98.61(14) . . ? N8 Ni1 O1 169.62(12) . . ? N7 Ni1 O1 91.11(13) . . ? N8 Ni1 O1 89.64(13) . 2 ? N7 Ni1 O1 169.69(12) . 2 ? O1 Ni1 O1 80.31(11) . 2 ? N8 Ni1 N6 93.77(15) . . ? N7 Ni1 N6 90.14(13) . . ? O1 Ni1 N6 89.81(13) . . ? O1 Ni1 N6 95.50(12) 2 . ? N8 Ni1 O2 86.84(15) . . ? N7 Ni1 O2 87.15(13) . . ? O1 Ni1 O2 90.04(13) . . ? O1 Ni1 O2 87.15(11) 2 . ? N6 Ni1 O2 177.27(13) . . ? C17 N7 C25 115.6(4) . . ? C17 N7 Ni1 122.4(3) . . ? C25 N7 Ni1 121.6(3) . . ? N7 C17 C18 129.0(4) . . ? C19 C18 C23 118.8(4) . . ? C19 C18 C17 116.5(4) . . ? C23 C18 C17 124.6(4) . . ? C20 C19 C18 124.1(4) . . ? C21 C20 C19 116.5(4) . . ? C21 C20 C24 121.9(5) . . ? C19 C20 C24 121.6(5) . . ? C20 C21 C22 123.4(4) . . ? C21 C22 C23 119.9(4) . . ? C21 C22 C28 116.7(4) . 2 ? C23 C22 C28 123.5(4) . 2 ? O1 C23 C18 121.4(4) . . ? O1 C23 C22 121.5(4) . . ? C18 C23 C22 117.1(4) . . ? C23 O1 Ni1 128.0(2) . . ? C23 O1 Ni1 126.7(2) . 2 ? Ni1 O1 Ni1 99.69(11) . 2 ? C26 C25 N7 116.8(4) . . ? C25 C26 C27 121.7(6) . . ? C26 C27 N8 112.2(5) . . ? N8 C28 C22 127.3(4) . 2 ? N9 C30 C29 178.5(9) . . ? 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 Cr1 C16 N6 Ni1 -21(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 O2 H1W N5 0.948(10) 1.905(14) 2.835(5) 167(4) 1_655 O2 H2W N6 0.953(10) 2.41(3) 3.162(5) 135(4) 2 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.644 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.090 #==END