# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Zhiqiang Liang' _publ_contact_author_email liangzq@jlu.edu.cn loop_ _publ_author_name 'Lei Wang' 'Yi Li' 'Yu Peng' 'Zhiqiang Liang' 'Jihong Yu' 'Ruren Xu' data_f _database_code_depnum_ccdc_archive 'CCDC 855885' #TrackingRef '- f-0320.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C119.50 H89.50 Co10 N14.50 O26.50' _chemical_formula_weight 2741.86 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' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M pa-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 28.0546(4) _cell_length_b 28.0546(4) _cell_length_c 28.0546(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 22080.7(5) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.45 _cell_measurement_theta_max 28.29 _exptl_crystal_description rhombus _exptl_crystal_colour red _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11120 _exptl_absorpt_coefficient_mu 1.546 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6627 _exptl_absorpt_correction_T_max 0.7577 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9156 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1174 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 2 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 28.29 _reflns_number_total 9156 _reflns_number_gt 3384 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. In order to avoid the large difference of the thermal displacement parameters between two disordered positions of C20-C25, EADP instructions were used to constrain these disordered C atoms with the equal displacement parameters. ; _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^)+(0.0400P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9156 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1864 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1391 _refine_ls_wR_factor_gt 0.1205 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _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 0.64009(2) 0.84777(3) 0.27511(2) 0.0499(2) Uani 1 1 d . . . Co2 Co 0.51214(2) 0.85318(2) 0.13987(2) 0.0448(2) Uani 1 1 d . . . Co3 Co 0.58216(2) 0.91784(2) 0.08216(2) 0.0388(3) Uani 1 3 d S . . Co4 Co 0.58083(2) 0.78710(2) 0.19985(2) 0.0454(2) Uani 1 1 d . . . O1 O 0.58088(12) 0.80119(12) 0.27151(12) 0.0554(10) Uani 1 1 d . . . O2 O 0.69589(12) 0.89835(12) 0.28390(11) 0.0529(9) Uani 1 1 d . . . O3 O 0.51107(12) 0.78900(12) 0.17756(12) 0.0503(9) Uani 1 1 d . . . O4 O 0.51099(11) 0.91521(11) 0.09908(11) 0.0416(8) Uani 1 1 d . . . O5 O 0.65328(11) 0.80358(11) 0.21684(11) 0.0480(9) Uani 1 1 d . . . O6 O 0.59322(11) 0.92959(11) 0.15737(11) 0.0430(8) Uani 1 1 d . . . O7 O 0.62704(12) 0.90022(11) 0.22291(11) 0.0465(9) Uani 1 1 d . . . O8 O 0.56569(11) 0.86298(12) 0.19013(11) 0.0458(9) Uani 1 1 d . . . N1 N 0.59635(18) 0.87546(19) 0.32847(16) 0.0638(14) Uani 1 1 d . . . N2 N 0.69030(16) 0.80842(17) 0.31537(15) 0.0563(12) Uani 1 1 d . . . N3 N 0.46084(15) 0.81547(16) 0.10183(16) 0.0567(12) Uani 1 1 d . B . N4 N 0.46176(15) 0.89367(16) 0.17756(16) 0.0546(12) Uani 1 1 d . . . C1 C 0.6055(2) 0.9118(2) 0.3574(2) 0.080(2) Uani 1 1 d . . . H1A H 0.6357 0.9255 0.3567 0.096 Uiso 1 1 calc R . . C2 C 0.5720(3) 0.9300(3) 0.3886(3) 0.110(3) Uani 1 1 d . . . H2A H 0.5793 0.9561 0.4078 0.132 Uiso 1 1 calc R . . C3 C 0.5272(3) 0.9088(3) 0.3907(3) 0.116(3) Uani 1 1 d . . . H3A H 0.5047 0.9202 0.4123 0.140 Uiso 1 1 calc R . . C4 C 0.5153(3) 0.8703(3) 0.3608(2) 0.083(2) Uani 1 1 d . . . C5 C 0.4705(3) 0.8470(3) 0.3584(3) 0.106(3) Uani 1 1 d . . . H5A H 0.4461 0.8565 0.3788 0.127 Uiso 1 1 calc R . . C6 C 0.4627(2) 0.8118(3) 0.3276(3) 0.095(2) Uani 1 1 d . . . H6A H 0.4327 0.7979 0.3258 0.114 Uiso 1 1 calc R . . C7 C 0.4994(2) 0.7955(2) 0.2976(2) 0.0713(18) Uani 1 1 d . . . H7A H 0.4932 0.7703 0.2769 0.086 Uiso 1 1 calc R . . C8 C 0.5447(2) 0.8157(2) 0.2979(2) 0.0558(15) Uani 1 1 d . . . C9 C 0.5523(2) 0.8543(2) 0.3299(2) 0.0635(16) Uani 1 1 d . . . C10 C 0.6879(2) 0.7637(2) 0.3280(2) 0.0757(19) Uani 1 1 d . . . H10A H 0.6613 0.7460 0.3192 0.091 Uiso 1 1 calc R . . C11 C 0.7237(3) 0.7416(2) 0.3544(2) 0.083(2) Uani 1 1 d . . . H11A H 0.7207 0.7098 0.3635 0.099 Uiso 1 1 calc R . . C12 C 0.7634(2) 0.7672(3) 0.3666(2) 0.082(2) Uani 1 1 d . . . H12A H 0.7875 0.7525 0.3840 0.099 Uiso 1 1 calc R . . C13 C 0.7682(2) 0.8150(2) 0.3533(2) 0.0670(17) Uani 1 1 d . . . C14 C 0.8075(2) 0.8443(3) 0.3639(2) 0.080(2) Uani 1 1 d . . . H14A H 0.8329 0.8323 0.3815 0.095 Uiso 1 1 calc R . . C15 C 0.8083(2) 0.8888(3) 0.3487(2) 0.081(2) Uani 1 1 d . . . H15A H 0.8342 0.9079 0.3566 0.097 Uiso 1 1 calc R . . C16 C 0.7717(2) 0.9084(2) 0.3213(2) 0.0702(18) Uani 1 1 d . . . H16A H 0.7742 0.9397 0.3106 0.084 Uiso 1 1 calc R . . C17 C 0.7326(2) 0.8822(2) 0.30991(18) 0.0529(14) Uani 1 1 d . . . C18 C 0.7303(2) 0.8344(2) 0.32753(19) 0.0584(16) Uani 1 1 d . . . C19 C 0.4359(2) 0.8295(2) 0.0649(2) 0.0765(19) Uani 1 1 d . . . H19A H 0.4451 0.8568 0.0485 0.092 Uiso 1 1 calc R A 1 C20A C 0.3952(5) 0.8037(5) 0.0493(5) 0.068(3) Uiso 0.50 1 d P B 1 H20A H 0.3752 0.8162 0.0260 0.081 Uiso 0.50 1 calc PR B 1 C21A C 0.3859(5) 0.7610(5) 0.0689(5) 0.080(3) Uiso 0.50 1 d P B 1 H21A H 0.3606 0.7429 0.0574 0.097 Uiso 0.50 1 calc PR B 1 C22A C 0.4133(5) 0.7435(5) 0.1055(5) 0.071(3) Uiso 0.50 1 d P B 1 C23A C 0.4744(4) 0.7152(4) 0.1809(4) 0.061(2) Uiso 0.50 1 d P B 1 H23A H 0.4919 0.7055 0.2073 0.073 Uiso 0.50 1 calc PR B 1 C24A C 0.4081(5) 0.6994(5) 0.1272(5) 0.093(3) Uiso 0.50 1 d P B 1 H24A H 0.3846 0.6785 0.1166 0.112 Uiso 0.50 1 calc PR B 1 C25A C 0.4366(5) 0.6870(5) 0.1631(5) 0.082(3) Uiso 0.50 1 d P B 1 H25A H 0.4312 0.6576 0.1775 0.099 Uiso 0.50 1 calc PR B 1 C20B C 0.4092(5) 0.7978(5) 0.0343(5) 0.068(3) Uiso 0.50 1 d P B 2 H20B H 0.3960 0.8078 0.0056 0.081 Uiso 0.50 1 calc PR B 2 C21B C 0.4049(5) 0.7528(5) 0.0504(5) 0.080(3) Uiso 0.50 1 d P B 2 H21B H 0.3808 0.7339 0.0376 0.097 Uiso 0.50 1 calc PR B 2 C22B C 0.4361(5) 0.7315(5) 0.0868(5) 0.071(3) Uiso 0.50 1 d P B 2 C23B C 0.4920(4) 0.7037(4) 0.1647(4) 0.061(2) Uiso 0.50 1 d P B 2 H23B H 0.5152 0.6929 0.1858 0.073 Uiso 0.50 1 calc PR B 2 C24B C 0.4392(5) 0.6834(5) 0.1023(5) 0.093(3) Uiso 0.50 1 d P B 2 H24B H 0.4228 0.6598 0.0859 0.112 Uiso 0.50 1 calc PR B 2 C25B C 0.4653(5) 0.6717(5) 0.1400(5) 0.082(3) Uiso 0.50 1 d P B 2 H25B H 0.4654 0.6400 0.1499 0.099 Uiso 0.50 1 calc PR B 2 C26 C 0.4842(2) 0.7565(2) 0.1583(2) 0.0692(18) Uani 1 1 d . . . C27 C 0.4551(2) 0.7704(2) 0.1189(2) 0.077(2) Uani 1 1 d . B . C28 C 0.4377(2) 0.8819(2) 0.2161(2) 0.080(2) Uani 1 1 d . . . H28A H 0.4425 0.8520 0.2296 0.096 Uiso 1 1 calc R . . C29 C 0.4050(3) 0.9132(3) 0.2373(3) 0.105(3) Uani 1 1 d . . . H29A H 0.3875 0.9032 0.2637 0.126 Uiso 1 1 calc R . . C30 C 0.3988(2) 0.9575(3) 0.2200(2) 0.090(2) Uani 1 1 d . . . H30A H 0.3783 0.9786 0.2351 0.108 Uiso 1 1 calc R . . C31 C 0.4238(2) 0.9718(2) 0.1783(2) 0.0640(17) Uani 1 1 d . . . C32 C 0.4202(2) 1.0174(2) 0.1575(2) 0.0697(18) Uani 1 1 d . . . H32A H 0.3990 1.0398 0.1698 0.084 Uiso 1 1 calc R . . C33 C 0.4481(2) 1.0283(2) 0.1195(2) 0.0629(16) Uani 1 1 d . . . H33A H 0.4465 1.0586 0.1062 0.075 Uiso 1 1 calc R . . C34 C 0.47952(18) 0.99388(19) 0.09967(19) 0.0523(14) Uani 1 1 d . . . H34A H 0.4981 1.0025 0.0736 0.063 Uiso 1 1 calc R . . C35 C 0.48351(17) 0.94886(19) 0.11725(18) 0.0433(13) Uani 1 1 d . . . C36 C 0.45546(17) 0.93795(18) 0.15812(19) 0.0477(14) Uani 1 1 d . . . C37 C 0.68874(16) 0.81126(16) 0.18874(16) 0.045(2) Uani 1 3 d S . . C38 C 0.59547(18) 0.89829(19) 0.18985(18) 0.0418(12) 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 Co1 0.0517(5) 0.0587(5) 0.0393(4) 0.0030(4) -0.0023(3) 0.0012(4) Co2 0.0399(4) 0.0433(4) 0.0513(5) 0.0072(3) -0.0006(3) -0.0012(3) Co3 0.0388(3) 0.0388(3) 0.0388(3) 0.0001(3) -0.0001(3) 0.0001(3) Co4 0.0463(4) 0.0449(4) 0.0451(4) 0.0061(3) -0.0008(3) -0.0002(3) O1 0.048(2) 0.067(3) 0.051(2) 0.0128(19) 0.0049(19) 0.0042(19) O2 0.052(2) 0.060(2) 0.047(2) 0.0028(18) -0.0073(19) 0.0007(19) O3 0.047(2) 0.046(2) 0.059(2) 0.0111(18) 0.0009(18) -0.0108(18) O4 0.041(2) 0.041(2) 0.042(2) 0.0024(16) -0.0002(16) 0.0017(17) O5 0.049(2) 0.053(2) 0.042(2) 0.0008(17) -0.0008(17) -0.0035(18) O6 0.048(2) 0.042(2) 0.040(2) 0.0048(17) -0.0026(16) -0.0025(16) O7 0.050(2) 0.046(2) 0.044(2) -0.0014(17) -0.0068(18) -0.0003(17) O8 0.044(2) 0.048(2) 0.045(2) 0.0064(17) -0.0054(17) 0.0008(18) N1 0.069(4) 0.075(4) 0.048(3) 0.002(3) 0.002(3) 0.011(3) N2 0.064(3) 0.061(3) 0.044(3) 0.005(2) -0.004(2) 0.003(3) N3 0.053(3) 0.052(3) 0.065(3) 0.011(3) -0.011(3) -0.004(2) N4 0.052(3) 0.057(3) 0.055(3) 0.008(2) 0.009(2) -0.001(2) C1 0.084(5) 0.089(5) 0.067(5) -0.010(4) 0.011(4) 0.014(4) C2 0.121(7) 0.114(7) 0.094(6) -0.034(5) 0.019(6) 0.005(6) C3 0.116(7) 0.124(8) 0.109(7) -0.019(6) 0.041(6) 0.034(6) C4 0.088(6) 0.090(6) 0.073(5) -0.008(4) 0.009(4) 0.017(5) C5 0.069(6) 0.151(8) 0.098(6) -0.012(6) 0.029(5) 0.006(5) C6 0.059(5) 0.150(8) 0.076(5) 0.005(5) 0.010(4) -0.004(5) C7 0.059(4) 0.088(5) 0.068(4) 0.009(4) 0.009(3) 0.001(4) C8 0.051(4) 0.060(4) 0.056(4) 0.017(3) -0.001(3) 0.005(3) C9 0.061(4) 0.075(5) 0.055(4) 0.009(3) 0.008(3) 0.011(4) C10 0.076(5) 0.087(5) 0.063(4) 0.018(4) -0.008(4) 0.010(4) C11 0.094(6) 0.070(5) 0.084(5) 0.010(4) -0.003(4) 0.010(4) C12 0.076(5) 0.096(6) 0.075(5) 0.012(4) -0.024(4) 0.025(4) C13 0.076(5) 0.073(5) 0.053(4) 0.006(3) -0.010(3) 0.016(4) C14 0.064(5) 0.100(6) 0.074(5) 0.004(4) -0.029(4) 0.016(4) C15 0.074(5) 0.089(6) 0.080(5) 0.000(4) -0.032(4) -0.008(4) C16 0.061(4) 0.085(5) 0.065(4) -0.002(3) -0.020(3) -0.013(4) C17 0.053(4) 0.068(4) 0.038(3) -0.005(3) -0.006(3) -0.005(3) C18 0.060(4) 0.070(4) 0.045(4) -0.002(3) -0.011(3) -0.001(3) C19 0.073(5) 0.067(4) 0.089(5) 0.024(4) -0.030(4) -0.024(4) C26 0.081(5) 0.057(4) 0.070(4) 0.023(3) -0.008(4) -0.018(4) C27 0.088(5) 0.066(5) 0.078(5) 0.020(4) -0.038(4) -0.031(4) C28 0.094(5) 0.070(5) 0.077(5) 0.017(4) 0.028(4) 0.010(4) C29 0.107(6) 0.102(6) 0.106(6) 0.015(5) 0.051(5) 0.003(5) C30 0.086(5) 0.080(5) 0.103(6) 0.002(5) 0.039(4) 0.016(4) C31 0.053(4) 0.059(4) 0.080(5) 0.004(3) 0.017(3) 0.002(3) C32 0.060(4) 0.058(4) 0.091(5) -0.001(4) 0.011(4) 0.021(3) C33 0.067(4) 0.053(4) 0.069(4) 0.010(3) -0.007(3) 0.008(3) C34 0.053(4) 0.050(4) 0.054(4) 0.003(3) 0.003(3) 0.006(3) C35 0.036(3) 0.049(4) 0.046(3) -0.001(3) -0.001(3) 0.001(3) C36 0.043(3) 0.039(3) 0.061(4) 0.001(3) -0.001(3) 0.003(3) C37 0.045(2) 0.045(2) 0.045(2) 0.009(2) -0.009(2) 0.009(2) C38 0.041(3) 0.043(3) 0.042(3) 0.003(3) 0.001(3) -0.001(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 Co1 O5 2.085(3) . ? Co1 N1 2.086(5) . ? Co1 O7 2.108(3) . ? Co1 N2 2.116(4) . ? Co1 O1 2.116(3) . ? Co1 O2 2.127(3) . ? Co2 O8 2.079(3) . ? Co2 N3 2.080(4) . ? Co2 O4 2.083(3) . ? Co2 O3 2.088(3) . ? Co2 N4 2.099(4) . ? Co2 O6 2.115(3) 12_664 ? Co3 O4 2.054(3) 6_566 ? Co3 O4 2.054(3) . ? Co3 O4 2.054(3) 12_664 ? Co3 O6 2.158(3) . ? Co3 O6 2.158(3) 12_664 ? Co3 O6 2.158(3) 6_566 ? Co4 O1 2.049(3) . ? Co4 O3 2.055(3) . ? Co4 O2 2.079(3) 12_664 ? Co4 O7 2.129(3) 12_664 ? Co4 O5 2.138(3) . ? Co4 O8 2.188(3) . ? O1 C8 1.319(6) . ? O2 C17 1.340(6) . ? O2 Co4 2.079(3) 6_566 ? O3 C26 1.301(6) . ? O4 C35 1.321(5) . ? O5 C37 1.287(3) . ? O6 C38 1.267(5) . ? O6 Co2 2.115(3) 6_566 ? O7 C38 1.283(5) . ? O7 Co4 2.129(3) 6_566 ? O8 C38 1.296(5) . ? N1 C1 1.328(7) . ? N1 C9 1.372(7) . ? N2 C10 1.305(7) . ? N2 C18 1.382(6) . ? N3 C19 1.311(6) . ? N3 C27 1.362(6) . ? N4 C28 1.316(6) . ? N4 C36 1.368(6) . ? C1 C2 1.383(8) . ? C2 C3 1.393(10) . ? C3 C4 1.408(9) . ? C4 C5 1.417(9) . ? C4 C9 1.425(8) . ? C5 C6 1.331(9) . ? C6 C7 1.405(8) . ? C7 C8 1.393(7) . ? C8 C9 1.423(8) . ? C10 C11 1.394(8) . ? C11 C12 1.369(8) . ? C12 C13 1.401(8) . ? C13 C18 1.396(7) . ? C13 C14 1.408(8) . ? C14 C15 1.320(8) . ? C15 C16 1.394(8) . ? C16 C17 1.360(7) . ? C17 C18 1.430(7) . ? C19 C20A 1.421(14) . ? C19 C20B 1.443(15) . ? C20A C21A 1.345(17) . ? C21A C22A 1.374(16) . ? C22A C24A 1.385(16) . ? C22A C27 1.443(13) . ? C23A C26 1.349(12) . ? C23A C25A 1.414(16) . ? C24A C25A 1.333(16) . ? C20B C21B 1.348(17) . ? C21B C22B 1.470(17) . ? C22B C24B 1.422(16) . ? C22B C27 1.513(14) . ? C23B C25B 1.361(15) . ? C23B C26 1.509(12) . ? C24B C25B 1.326(16) . ? C26 C27 1.428(7) . ? C28 C29 1.401(8) . ? C29 C30 1.347(8) . ? C30 C31 1.422(8) . ? C31 C32 1.408(7) . ? C31 C36 1.417(7) . ? C32 C33 1.357(7) . ? C33 C34 1.421(7) . ? C34 C35 1.360(6) . ? C35 C36 1.424(6) . ? C37 O5 1.287(3) 12_664 ? C37 O5 1.287(3) 6_566 ? 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 O5 Co1 N1 152.71(18) . . ? O5 Co1 O7 84.33(12) . . ? N1 Co1 O7 97.84(16) . . ? O5 Co1 N2 89.44(15) . . ? N1 Co1 N2 101.70(17) . . ? O7 Co1 N2 148.27(16) . . ? O5 Co1 O1 74.62(13) . . ? N1 Co1 O1 78.60(18) . . ? O7 Co1 O1 105.16(13) . . ? N2 Co1 O1 103.06(16) . . ? O5 Co1 O2 110.92(13) . . ? N1 Co1 O2 95.81(18) . . ? O7 Co1 O2 75.09(13) . . ? N2 Co1 O2 78.25(16) . . ? O1 Co1 O2 174.40(14) . . ? O8 Co2 N3 156.22(16) . . ? O8 Co2 O4 105.86(12) . . ? N3 Co2 O4 97.61(15) . . ? O8 Co2 O3 77.34(13) . . ? N3 Co2 O3 79.13(16) . . ? O4 Co2 O3 176.64(13) . . ? O8 Co2 N4 94.20(15) . . ? N3 Co2 N4 93.89(17) . . ? O4 Co2 N4 79.29(15) . . ? O3 Co2 N4 101.65(15) . . ? O8 Co2 O6 83.09(12) . 12_664 ? N3 Co2 O6 98.40(15) . 12_664 ? O4 Co2 O6 77.82(12) . 12_664 ? O3 Co2 O6 101.76(13) . 12_664 ? N4 Co2 O6 155.22(15) . 12_664 ? O4 Co3 O4 104.55(10) 6_566 . ? O4 Co3 O4 104.55(10) 6_566 12_664 ? O4 Co3 O4 104.55(10) . 12_664 ? O4 Co3 O6 77.48(12) 6_566 . ? O4 Co3 O6 85.37(12) . . ? O4 Co3 O6 168.76(12) 12_664 . ? O4 Co3 O6 168.76(12) 6_566 12_664 ? O4 Co3 O6 77.48(12) . 12_664 ? O4 Co3 O6 85.37(12) 12_664 12_664 ? O6 Co3 O6 91.77(12) . 12_664 ? O4 Co3 O6 85.37(12) 6_566 6_566 ? O4 Co3 O6 168.76(12) . 6_566 ? O4 Co3 O6 77.48(12) 12_664 6_566 ? O6 Co3 O6 91.77(12) . 6_566 ? O6 Co3 O6 91.77(12) 12_664 6_566 ? O1 Co4 O3 107.11(13) . . ? O1 Co4 O2 103.72(13) . 12_664 ? O3 Co4 O2 106.03(13) . 12_664 ? O1 Co4 O7 165.13(13) . 12_664 ? O3 Co4 O7 87.10(13) . 12_664 ? O2 Co4 O7 75.66(12) 12_664 12_664 ? O1 Co4 O5 74.86(13) . . ? O3 Co4 O5 165.32(13) . . ? O2 Co4 O5 87.25(13) 12_664 . ? O7 Co4 O5 90.28(12) 12_664 . ? O1 Co4 O8 86.25(12) . . ? O3 Co4 O8 75.64(13) . . ? O2 Co4 O8 168.60(13) 12_664 . ? O7 Co4 O8 93.28(12) 12_664 . ? O5 Co4 O8 90.11(12) . . ? C8 O1 Co4 127.5(3) . . ? C8 O1 Co1 112.7(4) . . ? Co4 O1 Co1 99.59(14) . . ? C17 O2 Co4 125.1(3) . 6_566 ? C17 O2 Co1 113.8(3) . . ? Co4 O2 Co1 96.64(13) 6_566 . ? C26 O3 Co4 131.3(4) . . ? C26 O3 Co2 113.7(3) . . ? Co4 O3 Co2 99.37(14) . . ? C35 O4 Co3 129.1(3) . . ? C35 O4 Co2 113.2(3) . . ? Co3 O4 Co2 98.15(13) . . ? C37 O5 Co1 121.19(19) . . ? C37 O5 Co4 129.4(3) . . ? Co1 O5 Co4 97.74(13) . . ? C38 O6 Co2 127.3(3) . 6_566 ? C38 O6 Co3 127.2(3) . . ? Co2 O6 Co3 94.03(12) 6_566 . ? C38 O7 Co1 126.3(3) . . ? C38 O7 Co4 125.3(3) . 6_566 ? Co1 O7 Co4 95.70(13) . 6_566 ? C38 O8 Co2 124.3(3) . . ? C38 O8 Co4 128.3(3) . . ? Co2 O8 Co4 95.51(13) . . ? C1 N1 C9 119.3(5) . . ? C1 N1 Co1 127.6(5) . . ? C9 N1 Co1 113.0(4) . . ? C10 N2 C18 118.9(5) . . ? C10 N2 Co1 127.7(4) . . ? C18 N2 Co1 113.4(4) . . ? C19 N3 C27 119.6(5) . . ? C19 N3 Co2 128.5(4) . . ? C27 N3 Co2 111.9(4) . . ? C28 N4 C36 119.2(5) . . ? C28 N4 Co2 128.6(4) . . ? C36 N4 Co2 112.2(3) . . ? N1 C1 C2 122.6(7) . . ? C1 C2 C3 118.9(7) . . ? C2 C3 C4 121.1(7) . . ? C3 C4 C5 126.3(8) . . ? C3 C4 C9 115.6(7) . . ? C5 C4 C9 118.1(7) . . ? C6 C5 C4 121.2(7) . . ? C5 C6 C7 120.7(7) . . ? C8 C7 C6 122.1(7) . . ? O1 C8 C7 125.0(6) . . ? O1 C8 C9 118.3(5) . . ? C7 C8 C9 116.7(6) . . ? N1 C9 C8 116.4(6) . . ? N1 C9 C4 122.5(6) . . ? C8 C9 C4 121.1(6) . . ? N2 C10 C11 122.4(6) . . ? C12 C11 C10 119.1(6) . . ? C11 C12 C13 120.9(6) . . ? C18 C13 C12 116.1(6) . . ? C18 C13 C14 118.6(6) . . ? C12 C13 C14 125.3(6) . . ? C15 C14 C13 119.8(6) . . ? C14 C15 C16 122.7(6) . . ? C17 C16 C15 120.7(6) . . ? O2 C17 C16 124.4(5) . . ? O2 C17 C18 118.1(5) . . ? C16 C17 C18 117.5(5) . . ? N2 C18 C13 122.7(6) . . ? N2 C18 C17 116.5(5) . . ? C13 C18 C17 120.7(6) . . ? N3 C19 C20A 121.3(8) . . ? N3 C19 C20B 124.2(8) . . ? C20A C19 C20B 24.2(7) . . ? C21A C20A C19 119.0(13) . . ? C20A C21A C22A 121.1(14) . . ? C21A C22A C24A 125.9(14) . . ? C21A C22A C27 117.5(12) . . ? C24A C22A C27 116.1(12) . . ? C26 C23A C25A 117.9(12) . . ? C25A C24A C22A 120.0(14) . . ? C24A C25A C23A 124.8(14) . . ? C21B C20B C19 115.2(13) . . ? C20B C21B C22B 124.0(14) . . ? C24B C22B C21B 129.5(13) . . ? C24B C22B C27 118.6(11) . . ? C21B C22B C27 109.4(11) . . ? C25B C23B C26 120.5(11) . . ? C25B C24B C22B 121.0(14) . . ? C24B C25B C23B 123.1(14) . . ? O3 C26 C23A 121.7(7) . . ? O3 C26 C27 117.5(5) . . ? C23A C26 C27 118.7(8) . . ? O3 C26 C23B 123.7(7) . . ? C23A C26 C23B 29.5(6) . . ? C27 C26 C23B 116.4(7) . . ? N3 C27 C26 117.3(5) . . ? N3 C27 C22A 119.4(7) . . ? C26 C27 C22A 121.5(7) . . ? N3 C27 C22B 120.0(7) . . ? C26 C27 C22B 117.8(7) . . ? C22A C27 C22B 35.0(6) . . ? N4 C28 C29 122.0(6) . . ? C30 C29 C28 120.5(6) . . ? C29 C30 C31 119.7(6) . . ? C32 C31 C36 119.3(5) . . ? C32 C31 C30 124.1(6) . . ? C36 C31 C30 116.6(6) . . ? C33 C32 C31 119.2(5) . . ? C32 C33 C34 120.9(5) . . ? C35 C34 C33 122.6(5) . . ? O4 C35 C34 124.9(5) . . ? O4 C35 C36 118.7(5) . . ? C34 C35 C36 116.5(5) . . ? N4 C36 C31 122.1(5) . . ? N4 C36 C35 116.4(5) . . ? C31 C36 C35 121.5(5) . . ? O5 C37 O5 119.998(5) . 12_664 ? O5 C37 O5 120.001(4) . 6_566 ? O5 C37 O5 119.997(4) 12_664 6_566 ? O6 C38 O7 121.7(5) . . ? O6 C38 O8 120.1(5) . . ? O7 C38 O8 118.2(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.701 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.091 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 703 206 '5 DMF' 2 0.500 0.000 0.500 703 208 '5 DMF' 3 0.184 0.184 0.184 13 1 ' ' 4 0.684 0.184 0.316 13 1 ' ' 5 1.000 0.500 0.500 703 208 '5 DMF' 6 0.500 0.500 1.000 703 207 '5 DMF' 7 0.184 0.315 0.684 13 1 ' ' 8 0.684 0.315 0.815 13 1 ' ' 9 0.316 0.684 0.184 13 1 ' ' 10 0.816 0.684 0.315 13 1 ' ' 11 0.316 0.815 0.684 13 1 ' ' 12 0.816 0.815 0.815 13 1 ' ' _platon_squeeze_details ; The unit cell contains 20 DMF slovent molecules which have been treated as a diffuse contribution to the overall scattering and removed by SQUEEZE/PLATON. The amount of these disordered solvent was determined by TGA, elemental analysis and SQUEEZE results. A. L. Spek, J. Appl. Crystallogr., 2003, 36, 7-13. A. L. Spek, Acta Crystallogr., 2009, D65, 148-155. ;