# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H32 Co N10 Ni2 O4' _chemical_formula_sum 'C38 H32 Co N10 Ni2 O4' _chemical_formula_weight 869.05 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' Co Co 0.3494 0.9721 '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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.288(5) _cell_length_b 10.715(5) _cell_length_c 21.808(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 107.542(5) _cell_angle_gamma 90.000(5) _cell_volume 3629(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.31 _cell_measurement_theta_max 25.03 _exptl_crystal_description rectangular _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1780 _exptl_absorpt_coefficient_mu 1.536 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5786 _exptl_absorpt_correction_T_max 0.7487 _exptl_absorpt_process_details sadabs _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 '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 24468 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6377 _reflns_number_gt 4605 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX2' _computing_cell_refinement 'Bruker SMART APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WINGX V1.80.03' _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^)+(0.0460P)^2^+0.4155P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6377 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1008 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 Co1 Co 0.74061(3) 0.12820(4) 0.75172(2) 0.02959(13) Uani 1 1 d . . . Ni2 Ni 0.81931(3) -0.12086(4) 0.80862(2) 0.03654(14) Uani 1 1 d . . . Ni1 Ni 0.63496(3) -0.05861(4) 0.66249(2) 0.03944(15) Uani 1 1 d . . . C35 C 0.6553(2) 0.3501(3) 0.80966(18) 0.0384(9) Uani 1 1 d . . . O1 O 0.66215(15) 0.1235(2) 0.65843(11) 0.0357(6) Uani 1 1 d . . . O4 O 0.78666(16) -0.0504(2) 0.71822(11) 0.0392(6) Uani 1 1 d . . . O3 O 0.81151(16) 0.0539(2) 0.83607(11) 0.0397(6) Uani 1 1 d . . . O2 O 0.65195(18) -0.0151(2) 0.75376(12) 0.0547(8) Uani 1 1 d . . . N1 N 0.6440(2) -0.0881(3) 0.57340(16) 0.0483(9) Uani 1 1 d . . . N3 N 0.8167(2) -0.1808(3) 0.89572(15) 0.0456(8) Uani 1 1 d . . . N5 N 0.6836(2) 0.2722(3) 0.78678(15) 0.0439(8) Uani 1 1 d . . . N6 N 0.8352(2) 0.2428(3) 0.73871(15) 0.0445(8) Uani 1 1 d . . . N4 N 0.8134(2) -0.2932(3) 0.76823(16) 0.0452(8) Uani 1 1 d . . . N7 N 0.5016(2) -0.0351(3) 0.63456(16) 0.0491(9) Uani 1 1 d . . . N2 N 0.61268(19) -0.2390(3) 0.68324(16) 0.0454(8) Uani 1 1 d . . . N8 N 0.3690(2) -0.0524(3) 0.66405(19) 0.0607(10) Uani 1 1 d . . . C34 C 0.8340(2) -0.0849(3) 0.68074(17) 0.0389(9) Uani 1 1 d . . . C6 C 0.6640(2) 0.1328(4) 0.54906(18) 0.0463(10) Uani 1 1 d . . . C1 C 0.6696(2) 0.1884(3) 0.60875(17) 0.0366(9) Uani 1 1 d . . . C19 C 0.8640(2) 0.2248(4) 0.90531(18) 0.0471(10) Uani 1 1 d . . . H19 H 0.8509 0.2793 0.8705 0.057 Uiso 1 1 calc R . . N10 N 1.0824(3) -0.1003(3) 0.7988(2) 0.0786(13) Uani 1 1 d . . . C12 C 0.5746(2) -0.1835(3) 0.78016(18) 0.0404(9) Uani 1 1 d . . . C9 C 0.5801(3) -0.3010(4) 0.5696(2) 0.0634(13) Uani 1 1 d . . . H9A H 0.5253 -0.2592 0.5633 0.076 Uiso 1 1 calc R . . H9B H 0.5694 -0.3754 0.5430 0.076 Uiso 1 1 calc R . . C33 C 0.8573(3) 0.0006(4) 0.64037(18) 0.0514(11) Uani 1 1 d . . . H33 H 0.8414 0.0839 0.6410 0.062 Uiso 1 1 calc R . . C36 C 0.8780(2) 0.3110(4) 0.72144(19) 0.0447(10) Uani 1 1 d . . . C18 C 0.8467(2) 0.0974(3) 0.89468(17) 0.0367(9) Uani 1 1 d . . . C2 C 0.6847(2) 0.3172(4) 0.61469(19) 0.0455(10) Uani 1 1 d . . . H2 H 0.6859 0.3571 0.6528 0.055 Uiso 1 1 calc R . . N9 N 0.9494(2) -0.1144(3) 0.82541(15) 0.0471(8) Uani 1 1 d . . . C16 C 0.6105(2) -0.0024(4) 0.84786(17) 0.0451(10) Uani 1 1 d . . . H16 H 0.6372 0.0749 0.8576 0.054 Uiso 1 1 calc R . . C23 C 0.8655(2) 0.0171(4) 0.94939(17) 0.0454(10) Uani 1 1 d . . . C29 C 0.8607(3) -0.2102(4) 0.68009(19) 0.0471(10) Uani 1 1 d . . . C17 C 0.6138(2) -0.0643(3) 0.79300(17) 0.0391(9) Uani 1 1 d . . . C28 C 0.8408(3) -0.3066(4) 0.7200(2) 0.0522(11) Uani 1 1 d . . . H28 H 0.8492 -0.3884 0.7089 0.063 Uiso 1 1 calc R . . C37 C 0.4407(3) -0.0495(3) 0.64986(18) 0.0394(9) Uani 1 1 d . . . C13 C 0.5316(2) -0.2295(4) 0.8221(2) 0.0521(11) Uani 1 1 d . . . H13 H 0.5039 -0.3062 0.8130 0.062 Uiso 1 1 calc R . . C24 C 0.8429(3) -0.1123(4) 0.9458(2) 0.0529(11) Uani 1 1 d . . . H24 H 0.8478 -0.1514 0.9848 0.064 Uiso 1 1 calc R . . C21 C 0.9205(3) 0.1943(4) 1.0192(2) 0.0669(13) Uani 1 1 d . . . H21 H 0.9455 0.2264 1.0603 0.080 Uiso 1 1 calc R . . C26 C 0.8327(3) -0.4038(4) 0.8708(2) 0.0650(13) Uani 1 1 d . . . H26A H 0.8937 -0.3855 0.8815 0.078 Uiso 1 1 calc R . . H26B H 0.8269 -0.4863 0.8873 0.078 Uiso 1 1 calc R . . C15 C 0.5687(3) -0.0522(4) 0.88842(19) 0.0536(11) Uani 1 1 d . . . H15 H 0.5676 -0.0079 0.9249 0.064 Uiso 1 1 calc R . . C3 C 0.6976(3) 0.3856(4) 0.5651(2) 0.0595(12) Uani 1 1 d . . . H3 H 0.7088 0.4706 0.5706 0.071 Uiso 1 1 calc R . . C22 C 0.9032(3) 0.0696(4) 1.0101(2) 0.0640(13) Uani 1 1 d . . . H22 H 0.9172 0.0174 1.0459 0.077 Uiso 1 1 calc R . . C14 C 0.5283(3) -0.1668(4) 0.8758(2) 0.0574(12) Uani 1 1 d . . . H14 H 0.4998 -0.2003 0.9031 0.069 Uiso 1 1 calc R . . C32 C 0.9025(3) -0.0354(5) 0.6004(2) 0.0701(14) Uani 1 1 d . . . H32 H 0.9171 0.0234 0.5741 0.084 Uiso 1 1 calc R . . C8 C 0.6389(3) -0.2156(4) 0.5471(2) 0.0701(14) Uani 1 1 d . . . H8A H 0.6963 -0.2515 0.5594 0.084 Uiso 1 1 calc R . . H8B H 0.6188 -0.2111 0.5005 0.084 Uiso 1 1 calc R . . C25 C 0.7915(3) -0.3094(4) 0.9045(2) 0.0601(12) Uani 1 1 d . . . H25A H 0.7294 -0.3167 0.8878 0.072 Uiso 1 1 calc R . . H25B H 0.8082 -0.3284 0.9501 0.072 Uiso 1 1 calc R . . C5 C 0.6772(3) 0.2068(5) 0.5000(2) 0.0655(13) Uani 1 1 d . . . H5 H 0.6741 0.1699 0.4608 0.079 Uiso 1 1 calc R . . C20 C 0.9001(3) 0.2707(4) 0.96658(19) 0.0583(12) Uani 1 1 d . . . H20 H 0.9109 0.3558 0.9722 0.070 Uiso 1 1 calc R . . C10 C 0.6145(3) -0.3394(4) 0.6385(2) 0.0622(13) Uani 1 1 d . . . H10A H 0.5808 -0.4090 0.6462 0.075 Uiso 1 1 calc R . . H10B H 0.6734 -0.3678 0.6469 0.075 Uiso 1 1 calc R . . C27 C 0.7948(3) -0.4058(4) 0.7986(2) 0.0613(12) Uani 1 1 d . . . H27A H 0.8174 -0.4772 0.7816 0.074 Uiso 1 1 calc R . . H27B H 0.7328 -0.4159 0.7876 0.074 Uiso 1 1 calc R . . C11 C 0.5814(2) -0.2647(4) 0.7289(2) 0.0483(10) Uani 1 1 d . . . H11 H 0.5605 -0.3454 0.7292 0.058 Uiso 1 1 calc R . . C30 C 0.9068(3) -0.2456(5) 0.6383(2) 0.0661(13) Uani 1 1 d . . . H30 H 0.9238 -0.3283 0.6372 0.079 Uiso 1 1 calc R . . C4 C 0.6943(3) 0.3303(5) 0.5077(2) 0.0689(14) Uani 1 1 d . . . H4 H 0.7036 0.3771 0.4745 0.083 Uiso 1 1 calc R . . C31 C 0.9273(3) -0.1584(5) 0.5983(2) 0.0776(15) Uani 1 1 d . . . H31 H 0.9576 -0.1824 0.5703 0.093 Uiso 1 1 calc R . . C38 C 1.0110(3) -0.1144(3) 0.81113(18) 0.0406(9) Uani 1 1 d . . . C7 C 0.6517(3) -0.0005(4) 0.53618(19) 0.0525(11) Uani 1 1 d . . . H7 H 0.6493 -0.0250 0.4948 0.063 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 Co1 0.0329(3) 0.0264(3) 0.0314(3) -0.0001(2) 0.0127(2) -0.0025(2) Ni2 0.0378(3) 0.0313(3) 0.0444(3) 0.0004(2) 0.0182(2) 0.0023(2) Ni1 0.0432(3) 0.0368(3) 0.0443(3) -0.0113(2) 0.0222(2) -0.0102(2) C35 0.032(2) 0.037(2) 0.047(2) 0.0025(19) 0.0143(18) -0.0093(18) O1 0.0406(14) 0.0356(14) 0.0339(13) 0.0001(11) 0.0160(11) -0.0002(11) O4 0.0442(15) 0.0367(14) 0.0432(15) -0.0009(12) 0.0232(12) 0.0066(12) O3 0.0515(16) 0.0346(14) 0.0309(14) -0.0012(11) 0.0091(11) 0.0085(12) O2 0.074(2) 0.0555(17) 0.0476(16) -0.0200(14) 0.0383(15) -0.0399(15) N1 0.045(2) 0.054(2) 0.047(2) -0.0193(17) 0.0160(16) -0.0118(16) N3 0.045(2) 0.0440(19) 0.049(2) 0.0077(17) 0.0170(16) 0.0035(16) N5 0.0419(19) 0.0401(19) 0.053(2) -0.0047(16) 0.0197(16) -0.0004(15) N6 0.0391(19) 0.0431(19) 0.057(2) -0.0019(16) 0.0236(16) -0.0055(16) N4 0.051(2) 0.0296(18) 0.059(2) 0.0007(16) 0.0228(17) 0.0023(15) N7 0.049(2) 0.045(2) 0.060(2) -0.0052(16) 0.0256(18) -0.0070(16) N2 0.0400(19) 0.0369(19) 0.059(2) -0.0147(16) 0.0146(16) -0.0076(15) N8 0.054(2) 0.037(2) 0.106(3) 0.019(2) 0.048(2) 0.0097(17) C34 0.040(2) 0.042(2) 0.035(2) -0.0046(17) 0.0105(17) 0.0047(17) C6 0.038(2) 0.066(3) 0.035(2) 0.002(2) 0.0105(17) -0.001(2) C1 0.0249(19) 0.046(2) 0.039(2) 0.0046(18) 0.0097(16) 0.0041(16) C19 0.052(3) 0.044(2) 0.043(2) -0.0018(19) 0.0117(19) 0.0005(19) N10 0.064(3) 0.040(2) 0.158(4) -0.025(2) 0.072(3) -0.0091(19) C12 0.034(2) 0.036(2) 0.050(2) 0.0114(18) 0.0098(18) -0.0045(17) C9 0.063(3) 0.052(3) 0.072(3) -0.031(2) 0.014(2) -0.009(2) C33 0.056(3) 0.053(3) 0.047(2) 0.001(2) 0.019(2) -0.002(2) C36 0.039(2) 0.041(2) 0.060(3) -0.006(2) 0.022(2) 0.0062(19) C18 0.035(2) 0.041(2) 0.034(2) -0.0021(17) 0.0113(17) 0.0065(16) C2 0.047(2) 0.046(2) 0.046(2) 0.0121(19) 0.0185(19) 0.0071(19) N9 0.042(2) 0.049(2) 0.053(2) 0.0013(16) 0.0183(17) 0.0076(16) C16 0.050(2) 0.047(2) 0.044(2) 0.0012(19) 0.0225(19) -0.004(2) C23 0.049(2) 0.051(3) 0.035(2) 0.0029(19) 0.0110(18) 0.0069(19) C29 0.047(2) 0.046(2) 0.050(2) -0.009(2) 0.016(2) 0.0049(19) C17 0.034(2) 0.044(2) 0.042(2) 0.0033(18) 0.0146(17) -0.0059(18) C28 0.056(3) 0.036(2) 0.065(3) -0.013(2) 0.019(2) 0.001(2) C37 0.047(3) 0.025(2) 0.046(2) -0.0023(16) 0.0140(19) -0.0019(18) C13 0.039(2) 0.047(2) 0.067(3) 0.027(2) 0.010(2) -0.0076(19) C24 0.061(3) 0.056(3) 0.043(2) 0.010(2) 0.017(2) 0.007(2) C21 0.087(4) 0.067(3) 0.039(3) -0.013(2) 0.007(2) 0.003(3) C26 0.074(3) 0.034(2) 0.086(4) 0.019(2) 0.022(3) 0.006(2) C15 0.050(3) 0.070(3) 0.045(2) 0.009(2) 0.020(2) 0.002(2) C3 0.061(3) 0.056(3) 0.064(3) 0.020(2) 0.024(2) 0.012(2) C22 0.082(3) 0.068(3) 0.038(2) 0.003(2) 0.012(2) 0.009(3) C14 0.046(3) 0.076(3) 0.055(3) 0.026(2) 0.023(2) -0.004(2) C32 0.080(4) 0.084(4) 0.058(3) 0.008(3) 0.036(3) 0.003(3) C8 0.078(3) 0.078(3) 0.062(3) -0.033(3) 0.032(3) -0.012(3) C25 0.075(3) 0.047(3) 0.062(3) 0.016(2) 0.026(2) -0.007(2) C5 0.062(3) 0.097(4) 0.038(2) 0.011(3) 0.016(2) 0.005(3) C20 0.070(3) 0.052(3) 0.049(3) -0.014(2) 0.013(2) -0.003(2) C10 0.062(3) 0.045(3) 0.080(3) -0.025(2) 0.023(3) -0.006(2) C27 0.072(3) 0.031(2) 0.085(4) 0.000(2) 0.030(3) -0.001(2) C11 0.038(2) 0.033(2) 0.068(3) 0.002(2) 0.006(2) -0.0083(18) C30 0.075(3) 0.068(3) 0.065(3) -0.013(3) 0.035(3) 0.011(3) C4 0.073(3) 0.083(4) 0.055(3) 0.029(3) 0.025(3) 0.008(3) C31 0.083(4) 0.098(4) 0.068(3) -0.010(3) 0.047(3) 0.012(3) C38 0.038(2) 0.033(2) 0.055(3) -0.0021(18) 0.020(2) 0.0014(18) C7 0.047(3) 0.077(3) 0.036(2) -0.011(2) 0.0154(19) -0.003(2) _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 Co1 O3 2.018(2) . ? Co1 O1 2.051(2) . ? Co1 N6 2.055(3) . ? Co1 N5 2.063(3) . ? Co1 O2 2.118(2) . ? Co1 O4 2.256(2) . ? Co1 Ni1 2.9556(9) . ? Ni2 O3 1.982(2) . ? Ni2 N3 2.018(3) . ? Ni2 O4 2.027(2) . ? Ni2 N4 2.036(3) . ? Ni2 N9 2.040(3) . ? Ni1 O2 1.981(2) . ? Ni1 O1 2.009(2) . ? Ni1 N1 2.017(3) . ? Ni1 N2 2.042(3) . ? Ni1 N7 2.087(4) . ? Ni1 O4 2.404(3) . ? C35 N5 1.140(4) . ? C35 N8 1.309(5) 2_656 ? O1 C1 1.323(4) . ? O4 C34 1.334(4) . ? O3 C18 1.318(4) . ? O2 C17 1.310(4) . ? N1 C7 1.272(5) . ? N1 C8 1.475(5) . ? N3 C24 1.278(5) . ? N3 C25 1.466(5) . ? N6 C36 1.149(5) . ? N4 C28 1.268(5) . ? N4 C27 1.451(5) . ? N7 C37 1.147(5) . ? N2 C11 1.277(5) . ? N2 C10 1.458(5) . ? N8 C37 1.297(5) . ? N8 C35 1.309(5) 2_646 ? C34 C33 1.400(5) . ? C34 C29 1.412(5) . ? C6 C5 1.400(6) . ? C6 C1 1.410(5) . ? C6 C7 1.457(6) . ? C1 C2 1.400(5) . ? C19 C20 1.378(5) . ? C19 C18 1.398(5) . ? N10 C38 1.279(5) . ? N10 C36 1.299(5) 2_746 ? C12 C13 1.399(5) . ? C12 C17 1.418(5) . ? C12 C11 1.447(5) . ? C9 C10 1.495(6) . ? C9 C8 1.510(6) . ? C33 C32 1.356(6) . ? C36 N10 1.299(5) 2_756 ? C18 C23 1.427(5) . ? C2 C3 1.373(5) . ? N9 C38 1.136(5) . ? C16 C15 1.376(5) . ? C16 C17 1.383(5) . ? C23 C22 1.399(5) . ? C23 C24 1.430(6) . ? C29 C30 1.397(5) . ? C29 C28 1.450(5) . ? C13 C14 1.364(6) . ? C21 C20 1.367(6) . ? C21 C22 1.367(6) . ? C26 C27 1.509(6) . ? C26 C25 1.519(6) . ? C15 C14 1.381(6) . ? C3 C4 1.372(6) . ? C32 C31 1.384(6) . ? C5 C4 1.352(6) . ? C30 C31 1.386(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 O3 Co1 O1 155.37(9) . . ? O3 Co1 N6 96.59(12) . . ? O1 Co1 N6 98.42(11) . . ? O3 Co1 N5 98.92(11) . . ? O1 Co1 N5 99.81(11) . . ? N6 Co1 N5 92.54(13) . . ? O3 Co1 O2 84.34(11) . . ? O1 Co1 O2 77.19(10) . . ? N6 Co1 O2 168.61(11) . . ? N5 Co1 O2 98.54(12) . . ? O3 Co1 O4 78.80(9) . . ? O1 Co1 O4 80.02(9) . . ? N6 Co1 O4 97.22(11) . . ? N5 Co1 O4 170.15(11) . . ? O2 Co1 O4 71.76(10) . . ? O3 Co1 Ni1 113.12(7) . . ? O1 Co1 Ni1 42.74(7) . . ? N6 Co1 Ni1 128.72(9) . . ? N5 Co1 Ni1 120.84(9) . . ? O2 Co1 Ni1 42.04(7) . . ? O4 Co1 Ni1 52.90(7) . . ? O3 Ni2 N3 89.72(12) . . ? O3 Ni2 O4 85.41(9) . . ? N3 Ni2 O4 163.86(11) . . ? O3 Ni2 N4 171.47(11) . . ? N3 Ni2 N4 96.12(13) . . ? O4 Ni2 N4 87.29(11) . . ? O3 Ni2 N9 94.10(12) . . ? N3 Ni2 N9 99.04(13) . . ? O4 Ni2 N9 96.65(12) . . ? N4 Ni2 N9 91.12(13) . . ? O2 Ni1 O1 81.37(10) . . ? O2 Ni1 N1 167.46(12) . . ? O1 Ni1 N1 91.65(12) . . ? O2 Ni1 N2 88.87(12) . . ? O1 Ni1 N2 170.16(11) . . ? N1 Ni1 N2 97.73(14) . . ? O2 Ni1 N7 94.75(13) . . ? O1 Ni1 N7 95.39(11) . . ? N1 Ni1 N7 96.27(13) . . ? N2 Ni1 N7 86.55(12) . . ? O2 Ni1 O4 70.87(10) . . ? O1 Ni1 O4 77.30(8) . . ? N1 Ni1 O4 97.51(11) . . ? N2 Ni1 O4 98.44(10) . . ? N7 Ni1 O4 164.56(11) . . ? O2 Ni1 Co1 45.72(7) . . ? O1 Ni1 Co1 43.85(7) . . ? N1 Ni1 Co1 122.91(9) . . ? N2 Ni1 Co1 127.02(9) . . ? N7 Ni1 Co1 117.31(9) . . ? O4 Ni1 Co1 48.44(6) . . ? N5 C35 N8 173.0(4) . 2_656 ? C1 O1 Ni1 128.5(2) . . ? C1 O1 Co1 128.0(2) . . ? Ni1 O1 Co1 93.41(9) . . ? C34 O4 Ni2 117.5(2) . . ? C34 O4 Co1 138.0(2) . . ? Ni2 O4 Co1 90.94(9) . . ? C34 O4 Ni1 112.1(2) . . ? Ni2 O4 Ni1 113.98(10) . . ? Co1 O4 Ni1 78.66(7) . . ? C18 O3 Ni2 125.3(2) . . ? C18 O3 Co1 135.0(2) . . ? Ni2 O3 Co1 99.71(10) . . ? C17 O2 Ni1 127.7(2) . . ? C17 O2 Co1 140.0(2) . . ? Ni1 O2 Co1 92.25(10) . . ? C7 N1 C8 116.1(4) . . ? C7 N1 Ni1 123.3(3) . . ? C8 N1 Ni1 120.5(3) . . ? C24 N3 C25 117.6(3) . . ? C24 N3 Ni2 121.7(3) . . ? C25 N3 Ni2 120.5(3) . . ? C35 N5 Co1 176.0(3) . . ? C36 N6 Co1 168.3(3) . . ? C28 N4 C27 117.3(3) . . ? C28 N4 Ni2 118.6(3) . . ? C27 N4 Ni2 123.1(3) . . ? C37 N7 Ni1 144.4(3) . . ? C11 N2 C10 117.1(4) . . ? C11 N2 Ni1 121.1(3) . . ? C10 N2 Ni1 120.6(3) . . ? C37 N8 C35 122.4(3) . 2_646 ? O4 C34 C33 121.3(3) . . ? O4 C34 C29 120.4(3) . . ? C33 C34 C29 118.2(4) . . ? C5 C6 C1 118.9(4) . . ? C5 C6 C7 116.8(4) . . ? C1 C6 C7 124.1(4) . . ? O1 C1 C2 119.9(3) . . ? O1 C1 C6 122.5(3) . . ? C2 C1 C6 117.6(3) . . ? C20 C19 C18 121.0(4) . . ? C38 N10 C36 124.1(4) . 2_746 ? C13 C12 C17 118.2(4) . . ? C13 C12 C11 117.7(4) . . ? C17 C12 C11 124.0(3) . . ? C10 C9 C8 114.3(4) . . ? C32 C33 C34 121.4(4) . . ? N6 C36 N10 171.7(4) . 2_756 ? O3 C18 C19 120.8(3) . . ? O3 C18 C23 121.2(3) . . ? C19 C18 C23 117.9(3) . . ? C3 C2 C1 121.1(4) . . ? C38 N9 Ni2 154.9(3) . . ? C15 C16 C17 121.8(4) . . ? C22 C23 C18 118.1(4) . . ? C22 C23 C24 118.3(4) . . ? C18 C23 C24 123.5(3) . . ? C30 C29 C34 119.5(4) . . ? C30 C29 C28 117.4(4) . . ? C34 C29 C28 123.1(4) . . ? O2 C17 C16 121.5(3) . . ? O2 C17 C12 120.5(3) . . ? C16 C17 C12 118.0(3) . . ? N4 C28 C29 128.0(4) . . ? N7 C37 N8 172.9(4) . . ? C14 C13 C12 123.0(4) . . ? N3 C24 C23 128.2(4) . . ? C20 C21 C22 118.4(4) . . ? C27 C26 C25 114.4(4) . . ? C16 C15 C14 120.9(4) . . ? C4 C3 C2 121.0(4) . . ? C21 C22 C23 122.9(4) . . ? C13 C14 C15 118.0(4) . . ? C33 C32 C31 120.9(5) . . ? N1 C8 C9 113.6(3) . . ? N3 C25 C26 112.4(4) . . ? C4 C5 C6 122.2(4) . . ? C21 C20 C19 121.7(4) . . ? N2 C10 C9 113.1(4) . . ? N4 C27 C26 112.8(3) . . ? N2 C11 C12 127.9(4) . . ? C31 C30 C29 120.4(4) . . ? C5 C4 C3 119.1(4) . . ? C32 C31 C30 119.6(4) . . ? N9 C38 N10 172.3(4) . . ? N1 C7 C6 129.4(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.331 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.067 _database_code_depnum_ccdc_archive 'CCDC 939761' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H32 Co N10 Ni2 O4, C2 H3 N' _chemical_formula_sum 'C40 H35 Co N11 Ni2 O4' _chemical_formula_weight 910.10 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' Co Co 0.3494 0.9721 '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 tetragonal _symmetry_space_group_name_H-M 'P 41 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, -z+3/4' '-x+1/2, y+1/2, -z+1/4' '-y, -x, -z+1/2' 'y, x, -z' 'y+1/2, -x+1/2, z+3/4' '-y+1/2, x+1/2, z+1/4' _cell_length_a 10.453(5) _cell_length_b 10.453(5) _cell_length_c 35.841(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 3916(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.03 _cell_measurement_theta_max 26.68 _exptl_crystal_description rectangular _exptl_crystal_colour green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1780 _exptl_absorpt_coefficient_mu 1.428 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5364 _exptl_absorpt_correction_T_max 0.6748 _exptl_absorpt_process_details sadabs _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 '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 26677 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 26.68 _reflns_number_total 3898 _reflns_number_gt 3536 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX2' _computing_cell_refinement 'Bruker SMART APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WINGX V1.80.03' _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^)+(0.0584P)^2^+1.3038P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(2) _refine_ls_number_reflns 3898 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.1030 _refine_ls_wR_factor_gt 0.0987 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _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 Co1 Co 0.03610(4) 0.03610(4) 0.0000 0.02930(15) Uani 1 2 d S . . Ni1 Ni -0.12356(4) 0.27170(4) 0.003286(13) 0.03733(14) Uani 1 1 d . . . O1 O 0.0408(2) 0.2204(2) -0.02032(6) 0.0367(5) Uani 1 1 d . . . N2 N -0.2946(3) 0.2695(3) 0.02938(10) 0.0498(8) Uani 1 1 d . . . O2 O -0.0555(2) 0.1449(2) 0.04048(6) 0.0377(5) Uani 1 1 d . . . N3 N -0.1444(3) 0.0208(4) -0.02493(10) 0.0516(8) Uani 1 1 d . . . N1 N -0.1842(4) 0.3436(3) -0.04605(9) 0.0529(9) Uani 1 1 d . . . C1 C -0.1018(4) 0.1136(4) 0.07316(9) 0.0399(7) Uani 1 1 d . . . C5 C -0.2667(5) 0.1163(6) 0.12037(14) 0.0754(15) Uani 1 1 d . . . H5 H -0.3468 0.1436 0.1284 0.091 Uiso 1 1 calc R . . C14 C 0.2134(5) 0.3504(5) -0.11638(11) 0.0673(13) Uani 1 1 d . . . H14 H 0.2529 0.3781 -0.1382 0.081 Uiso 1 1 calc R . . C13 C 0.0887(5) 0.3755(5) -0.11011(11) 0.0574(11) Uani 1 1 d . . . H13 H 0.0430 0.4215 -0.1279 0.069 Uiso 1 1 calc R . . C10 C -0.3176(6) 0.3859(7) -0.05131(14) 0.088(2) Uani 1 1 d . . . H10A H -0.3223 0.4769 -0.0461 0.105 Uiso 1 1 calc R . . H10B H -0.3406 0.3736 -0.0773 0.105 Uiso 1 1 calc R . . C12 C 0.0252(4) 0.3347(4) -0.07755(10) 0.0465(9) Uani 1 1 d . . . C4 C -0.1949(5) 0.0423(6) 0.14387(13) 0.0774(16) Uani 1 1 d . . . H4 H -0.2267 0.0178 0.1670 0.093 Uiso 1 1 calc R . . C17 C 0.0944(4) 0.2650(3) -0.05074(9) 0.0380(8) Uani 1 1 d . . . C16 C 0.2236(4) 0.2404(4) -0.05746(10) 0.0441(8) Uani 1 1 d . . . H16 H 0.2711 0.1950 -0.0400 0.053 Uiso 1 1 calc R . . C9 C -0.4113(5) 0.3209(6) -0.02830(18) 0.0828(18) Uani 1 1 d . . . H9A H -0.4052 0.2300 -0.0335 0.099 Uiso 1 1 calc R . . H9B H -0.4955 0.3485 -0.0363 0.099 Uiso 1 1 calc R . . C6 C -0.2252(4) 0.1525(4) 0.08501(11) 0.0527(9) Uani 1 1 d . . . C11 C -0.1092(5) 0.3638(4) -0.07391(10) 0.0541(11) Uani 1 1 d . . . H11 H -0.1467 0.4025 -0.0945 0.065 Uiso 1 1 calc R . . C18 C -0.2459(4) 0.0014(4) -0.03616(9) 0.0419(8) Uani 1 1 d . . . C15 C 0.2818(4) 0.2827(5) -0.08970(11) 0.0558(10) Uani 1 1 d . . . H15 H 0.3680 0.2655 -0.0936 0.067 Uiso 1 1 calc R . . C2 C -0.0283(4) 0.0404(4) 0.09792(10) 0.0452(8) Uani 1 1 d . . . H2 H 0.0536 0.0150 0.0909 0.054 Uiso 1 1 calc R . . C7 C -0.3127(4) 0.2210(5) 0.06167(13) 0.0602(11) Uani 1 1 d . . . H7 H -0.3944 0.2318 0.0714 0.072 Uiso 1 1 calc R . . C8 C -0.4035(5) 0.3381(5) 0.01269(13) 0.0675(13) Uani 1 1 d . . . H8A H -0.3956 0.4286 0.0182 0.081 Uiso 1 1 calc R . . H8B H -0.4822 0.3077 0.0240 0.081 Uiso 1 1 calc R . . C3 C -0.0745(5) 0.0049(5) 0.13258(11) 0.0584(11) Uani 1 1 d . . . H3 H -0.0241 -0.0445 0.1484 0.070 Uiso 1 1 calc R . . N4 N -0.3536(3) -0.0174(4) -0.05311(8) 0.0550(9) Uani 1 1 d . . . N5 N -0.0671(3) 0.4406(3) 0.02510(10) 0.0497(8) Uani 1 1 d . . . C19 C -0.0442(4) 0.5398(4) 0.03619(10) 0.0438(9) Uani 1 1 d . . . C51 C -0.1435(13) -0.3034(12) -0.0577(4) 0.102(4) Uani 0.50 1 d P . . H51A H -0.0945 -0.2261 -0.0555 0.154 Uiso 0.50 1 calc PR . . H51B H -0.1879 -0.3041 -0.0811 0.154 Uiso 0.50 1 calc PR . . H51C H -0.0872 -0.3758 -0.0563 0.154 Uiso 0.50 1 calc PR . . N50 N -0.3095(6) -0.3095(6) 0.0000 0.120(3) Uani 1 2 d S . . C50 C -0.2347(11) -0.3097(12) -0.0277(3) 0.080(3) Uani 0.50 1 d P . . 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 Co1 0.02848(19) 0.02848(19) 0.0310(3) 0.00041(18) -0.00041(18) 0.0024(2) Ni1 0.0383(2) 0.0339(2) 0.0398(2) 0.00034(19) -0.00163(19) 0.00452(18) O1 0.0408(13) 0.0343(12) 0.0350(11) 0.0062(10) 0.0062(10) 0.0039(11) N2 0.0326(17) 0.0476(19) 0.069(2) 0.0024(16) 0.0048(15) 0.0079(14) O2 0.0394(13) 0.0387(13) 0.0351(11) 0.0033(10) 0.0063(10) 0.0086(10) N3 0.0383(19) 0.066(2) 0.0509(17) 0.0029(16) -0.0047(15) -0.0021(17) N1 0.061(2) 0.052(2) 0.0463(17) 0.0005(15) -0.0114(16) 0.0181(16) C1 0.042(2) 0.039(2) 0.0388(17) -0.0017(15) 0.0055(15) -0.0016(15) C5 0.064(3) 0.099(4) 0.064(3) 0.009(3) 0.028(2) 0.015(3) C14 0.090(4) 0.074(3) 0.038(2) 0.010(2) 0.008(2) -0.018(3) C13 0.078(3) 0.057(3) 0.0366(19) 0.0100(19) -0.0067(19) -0.007(2) C10 0.081(4) 0.125(5) 0.056(3) 0.003(3) -0.010(3) 0.052(4) C12 0.064(3) 0.039(2) 0.0366(17) 0.0008(15) -0.0075(17) -0.0036(18) C4 0.074(3) 0.108(5) 0.049(2) 0.018(3) 0.022(2) 0.013(3) C17 0.048(2) 0.0301(17) 0.0362(16) -0.0031(14) 0.0010(15) -0.0054(15) C16 0.045(2) 0.046(2) 0.0419(18) -0.0016(16) -0.0004(16) -0.0056(16) C9 0.060(3) 0.084(4) 0.104(4) -0.016(3) -0.034(3) 0.029(3) C6 0.046(2) 0.056(3) 0.055(2) 0.0044(19) 0.0131(18) 0.0070(18) C11 0.072(3) 0.052(2) 0.0377(19) 0.0011(18) -0.0131(19) 0.013(2) C18 0.045(2) 0.048(2) 0.0327(17) 0.0002(15) 0.0043(16) 0.0018(17) C15 0.057(3) 0.061(3) 0.049(2) -0.002(2) 0.012(2) -0.0128(19) C2 0.041(2) 0.052(2) 0.0428(18) 0.0026(17) 0.0027(16) -0.0002(15) C7 0.046(2) 0.066(3) 0.069(3) 0.003(2) 0.023(2) 0.006(2) C8 0.050(3) 0.075(3) 0.077(3) 0.007(2) 0.002(2) 0.023(2) C3 0.064(3) 0.072(3) 0.039(2) 0.0102(19) 0.0026(19) 0.000(2) N4 0.0349(17) 0.094(3) 0.0362(15) 0.0063(17) -0.0029(13) -0.0143(17) N5 0.061(2) 0.0318(18) 0.0561(18) -0.0021(15) -0.0024(16) -0.0006(15) C19 0.050(2) 0.044(2) 0.0374(17) 0.0067(16) 0.0011(16) -0.0040(18) C51 0.089(9) 0.074(8) 0.145(12) -0.015(8) 0.022(9) -0.023(7) N50 0.102(4) 0.102(4) 0.155(8) 0.021(5) -0.021(5) -0.017(5) C50 0.058(6) 0.082(7) 0.101(8) 0.000(7) 0.012(6) -0.007(5) _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 Co1 O1 2.060(2) 6 ? Co1 O1 2.060(2) . ? Co1 O2 2.077(2) 6 ? Co1 O2 2.077(2) . ? Co1 N3 2.094(3) 6 ? Co1 N3 2.094(3) . ? Co1 Ni1 2.9772(15) . ? Co1 Ni1 2.9772(15) 6 ? Ni1 O1 1.989(3) . ? Ni1 O2 2.010(2) . ? Ni1 N2 2.018(3) . ? Ni1 N5 2.019(3) . ? Ni1 N1 2.024(3) . ? O1 C17 1.312(4) . ? N2 C7 1.277(5) . ? N2 C8 1.472(5) . ? O2 C1 1.309(4) . ? N3 C18 1.153(5) . ? N1 C11 1.287(6) . ? N1 C10 1.475(6) . ? C1 C2 1.402(5) . ? C1 C6 1.417(5) . ? C5 C4 1.367(7) . ? C5 C6 1.392(6) . ? C14 C13 1.348(7) . ? C14 C15 1.388(7) . ? C13 C12 1.409(6) . ? C10 C9 1.450(9) . ? C12 C17 1.406(5) . ? C12 C11 1.443(7) . ? C4 C3 1.379(7) . ? C17 C16 1.396(6) . ? C16 C15 1.378(5) . ? C9 C8 1.482(8) . ? C6 C7 1.431(6) . ? C18 N4 1.294(5) . ? C2 C3 1.384(5) . ? N4 C19 1.299(5) 6_455 ? N5 C19 1.136(5) . ? C19 N4 1.299(5) 6_565 ? C51 C50 1.438(16) . ? N50 C50 1.263(12) 6 ? N50 C50 1.263(12) . ? 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 O1 Co1 O1 94.62(14) 6 . ? O1 Co1 O2 75.29(9) 6 6 ? O1 Co1 O2 99.83(9) . 6 ? O1 Co1 O2 99.83(9) 6 . ? O1 Co1 O2 75.29(9) . . ? O2 Co1 O2 172.97(15) 6 . ? O1 Co1 N3 86.67(12) 6 6 ? O1 Co1 N3 174.49(12) . 6 ? O2 Co1 N3 85.68(12) 6 6 ? O2 Co1 N3 99.21(12) . 6 ? O1 Co1 N3 174.49(12) 6 . ? O1 Co1 N3 86.67(12) . . ? O2 Co1 N3 99.21(12) 6 . ? O2 Co1 N3 85.68(12) . . ? N3 Co1 N3 92.6(2) 6 . ? O1 Co1 Ni1 119.37(7) 6 . ? O1 Co1 Ni1 41.74(7) . . ? O2 Co1 Ni1 135.69(7) 6 . ? O2 Co1 Ni1 42.38(6) . . ? N3 Co1 Ni1 133.30(11) 6 . ? N3 Co1 Ni1 64.84(11) . . ? O1 Co1 Ni1 41.74(7) 6 6 ? O1 Co1 Ni1 119.37(7) . 6 ? O2 Co1 Ni1 42.38(6) 6 6 ? O2 Co1 Ni1 135.69(7) . 6 ? N3 Co1 Ni1 64.84(11) 6 6 ? N3 Co1 Ni1 133.30(11) . 6 ? Ni1 Co1 Ni1 158.26(3) . 6 ? O1 Ni1 O2 78.37(9) . . ? O1 Ni1 N2 163.64(12) . . ? O2 Ni1 N2 89.94(12) . . ? O1 Ni1 N5 98.54(13) . . ? O2 Ni1 N5 102.50(12) . . ? N2 Ni1 N5 95.12(15) . . ? O1 Ni1 N1 89.94(12) . . ? O2 Ni1 N1 159.31(12) . . ? N2 Ni1 N1 97.57(15) . . ? N5 Ni1 N1 96.02(14) . . ? O1 Ni1 Co1 43.59(7) . . ? O2 Ni1 Co1 44.13(7) . . ? N2 Ni1 Co1 120.37(10) . . ? N5 Ni1 Co1 125.10(10) . . ? N1 Ni1 Co1 116.64(10) . . ? C17 O1 Ni1 128.8(2) . . ? C17 O1 Co1 129.6(2) . . ? Ni1 O1 Co1 94.67(10) . . ? C7 N2 C8 116.5(4) . . ? C7 N2 Ni1 123.7(3) . . ? C8 N2 Ni1 119.4(3) . . ? C1 O2 Ni1 128.8(2) . . ? C1 O2 Co1 131.2(2) . . ? Ni1 O2 Co1 93.49(10) . . ? C18 N3 Co1 172.7(4) . . ? C11 N1 C10 115.3(4) . . ? C11 N1 Ni1 123.2(3) . . ? C10 N1 Ni1 121.3(3) . . ? O2 C1 C2 120.0(3) . . ? O2 C1 C6 122.2(3) . . ? C2 C1 C6 117.8(3) . . ? C4 C5 C6 122.9(5) . . ? C13 C14 C15 118.8(4) . . ? C14 C13 C12 122.3(4) . . ? C9 C10 N1 115.2(5) . . ? C17 C12 C13 118.7(4) . . ? C17 C12 C11 123.3(4) . . ? C13 C12 C11 118.0(4) . . ? C5 C4 C3 118.7(4) . . ? O1 C17 C16 119.4(3) . . ? O1 C17 C12 122.2(3) . . ? C16 C17 C12 118.4(3) . . ? C15 C16 C17 120.8(4) . . ? C10 C9 C8 118.0(5) . . ? C5 C6 C1 118.6(4) . . ? C5 C6 C7 118.0(4) . . ? C1 C6 C7 123.3(4) . . ? N1 C11 C12 129.0(4) . . ? N3 C18 N4 172.4(4) . . ? C16 C15 C14 120.9(5) . . ? C3 C2 C1 121.5(4) . . ? N2 C7 C6 129.3(4) . . ? N2 C8 C9 112.7(4) . . ? C4 C3 C2 120.4(4) . . ? C18 N4 C19 124.1(3) . 6_455 ? C19 N5 Ni1 174.4(3) . . ? N5 C19 N4 172.6(4) . 6_565 ? C50 N50 C50 128.2(14) 6 . ? N50 C50 C51 175.7(13) . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 26.68 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.630 _refine_diff_density_min -0.534 _refine_diff_density_rms 0.071 _database_code_depnum_ccdc_archive 'CCDC 939762'