# 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_1 _database_code_depnum_ccdc_archive 'CCDC 918129' #TrackingRef '16631_web_deposit_cif_file_0_LeiHou_1357479426.1.cif' # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.250 1.125 177 12 ' ' 2 0.000 0.750 -0.125 177 12 ' ' 3 0.032 0.454 0.042 7 0 ' ' 4 0.032 0.954 0.958 7 0 ' ' 5 0.250 0.500 0.832 1234 386 ' ' 6 0.250 1.000 0.117 1237 386 ' ' 7 0.204 0.219 0.196 6 0 ' ' 8 0.204 0.719 0.804 7 0 ' ' 9 0.296 0.281 0.304 6 0 ' ' 10 0.296 0.781 0.696 6 0 ' ' 11 0.500 0.250 0.375 177 12 ' ' 12 0.500 0.750 0.625 177 12 ' ' 13 0.469 0.046 0.446 6 0 ' ' 14 0.469 0.546 0.554 7 0 ' ' 15 0.532 0.454 0.458 7 0 ' ' 16 0.532 0.954 0.542 7 0 ' ' 17 0.750 0.500 0.617 1237 386 ' ' 18 0.750 1.000 0.332 1234 386 ' ' 19 0.704 0.219 0.304 7 0 ' ' 20 0.704 0.719 0.696 6 0 ' ' 21 0.796 0.281 0.196 6 0 ' ' 22 0.796 0.781 0.804 6 0 ' ' 23 0.969 0.046 0.054 7 0 ' ' 24 0.969 0.546 0.946 6 0 ' ' _platon_squeeze_details ; ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H25 Co2 N4 O6' _chemical_formula_weight 667.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 43.939(10) _cell_length_b 43.939(10) _cell_length_c 8.5387(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16485(6) _cell_formula_units_Z 16 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9483 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 27.35 _exptl_crystal_description Prism _exptl_crystal_colour Purple _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.076 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5456 _exptl_absorpt_coefficient_mu 0.841 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8366 _exptl_absorpt_correction_T_max 0.9058 _exptl_absorpt_process_details sadabs _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 42861 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -54 _diffrn_reflns_limit_h_max 52 _diffrn_reflns_limit_k_min -54 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8089 _reflns_number_gt 6181 _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. ; _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^)+(0.0590P)^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 8089 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0977 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.002 _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 0.447831(6) 0.904596(6) 0.19294(3) 0.02414(9) Uani 1 1 d . . . Co2 Co 0.426100(6) 0.870156(6) 0.50572(3) 0.02473(9) Uani 1 1 d . . . C1 C 0.42267(6) 0.93445(6) 0.4871(3) 0.0432(6) Uani 1 1 d . . . C2 C 0.41590(6) 0.96527(5) 0.5546(3) 0.0484(7) Uani 1 1 d . . . C3 C 0.40453(8) 0.96818(6) 0.7047(4) 0.0653(9) Uani 1 1 d . . . H3 H 0.4008 0.9509 0.7642 0.078 Uiso 1 1 calc R . . C4 C 0.39870(9) 0.99663(6) 0.7673(4) 0.0721(10) Uani 1 1 d . . . H4 H 0.3910 0.9982 0.8684 0.087 Uiso 1 1 calc R . . C5 C 0.40425(7) 1.02301(6) 0.6801(4) 0.0593(8) Uani 1 1 d . . . C6 C 0.41527(7) 1.01992(6) 0.5287(4) 0.0640(9) Uani 1 1 d . . . H6 H 0.4189 1.0372 0.4683 0.077 Uiso 1 1 calc R . . C7 C 0.42101(7) 0.99108(6) 0.4661(4) 0.0597(8) Uani 1 1 d . . . H7 H 0.4283 0.9893 0.3643 0.072 Uiso 1 1 calc R . . C8 C 0.39837(7) 1.05379(6) 0.7486(4) 0.0565(8) Uani 1 1 d . . . C9 C 0.40302(7) 1.05901(6) 0.9077(4) 0.0635(8) Uani 1 1 d . . . H9 H 0.4103 1.0434 0.9707 0.076 Uiso 1 1 calc R . . C10 C 0.39684(7) 1.08718(6) 0.9731(3) 0.0538(7) Uani 1 1 d . . . H10 H 0.4001 1.0903 1.0795 0.065 Uiso 1 1 calc R . . C11 C 0.38590(6) 1.11072(5) 0.8809(3) 0.0412(6) Uani 1 1 d . . . C12 C 0.38179(7) 1.10599(6) 0.7219(3) 0.0553(7) Uani 1 1 d . . . H12 H 0.3750 1.1218 0.6587 0.066 Uiso 1 1 calc R . . C13 C 0.38785(8) 1.07758(6) 0.6564(4) 0.0641(9) Uani 1 1 d . . . H13 H 0.3848 1.0745 0.5497 0.077 Uiso 1 1 calc R . . C14 C 0.37868(5) 1.14096(5) 0.9544(3) 0.0357(5) Uani 1 1 d . . . C15 C 0.47170(6) 0.92009(6) -0.0978(3) 0.0451(7) Uani 1 1 d . . . C16 C 0.48274(6) 0.94333(6) -0.2149(3) 0.0448(6) Uani 1 1 d . . . C17 C 0.48310(10) 0.97394(7) -0.1747(3) 0.0811(12) Uani 1 1 d . . . H17 H 0.4785 0.9798 -0.0728 0.097 Uiso 1 1 calc R . . C18 C 0.49033(10) 0.99581(7) -0.2853(3) 0.0843(13) Uani 1 1 d . . . H18 H 0.4907 1.0162 -0.2560 0.101 Uiso 1 1 calc R . . C19 C 0.49710(7) 0.98800(6) -0.4390(3) 0.0475(7) Uani 1 1 d . . . C20 C 0.49787(6) 0.95717(6) -0.4760(3) 0.0463(6) Uani 1 1 d . . . H20 H 0.5032 0.9512 -0.5769 0.056 Uiso 1 1 calc R . . C21 C 0.49089(6) 0.93503(6) -0.3652(3) 0.0433(6) Uani 1 1 d . . . H21 H 0.4917 0.9145 -0.3924 0.052 Uiso 1 1 calc R . . C22 C 0.52633(6) 0.88967(7) 0.1648(3) 0.0584(8) Uani 1 1 d . . . H22A H 0.5135 0.9033 0.1071 0.088 Uiso 1 1 calc R . . H22B H 0.5355 0.8754 0.0940 0.088 Uiso 1 1 calc R . . H22C H 0.5420 0.9011 0.2168 0.088 Uiso 1 1 calc R . . C23 C 0.50769(5) 0.87290(5) 0.2839(2) 0.0314(5) Uani 1 1 d . . . C24 C 0.51712(5) 0.85117(5) 0.3938(2) 0.0306(5) Uani 1 1 d . . . C25 C 0.49088(5) 0.84354(5) 0.4772(3) 0.0329(5) Uani 1 1 d . . . C26 C 0.48754(6) 0.82052(7) 0.6074(4) 0.0664(10) Uani 1 1 d . . . H26A H 0.4668 0.8202 0.6427 0.100 Uiso 1 1 calc R . . H26B H 0.5006 0.8260 0.6929 0.100 Uiso 1 1 calc R . . H26C H 0.4931 0.8007 0.5694 0.100 Uiso 1 1 calc R . . C27 C 0.55465(7) 0.86730(8) 0.7010(3) 0.0696(10) Uani 1 1 d . . . H27A H 0.5704 0.8677 0.7790 0.104 Uiso 1 1 calc R . . H27B H 0.5363 0.8592 0.7460 0.104 Uiso 1 1 calc R . . H27C H 0.5510 0.8876 0.6639 0.104 Uiso 1 1 calc R . . C28 C 0.56447(5) 0.84756(5) 0.5668(3) 0.0349(5) Uani 1 1 d . . . C29 C 0.54853(5) 0.84072(5) 0.4292(3) 0.0322(5) Uani 1 1 d . . . C30 C 0.56781(5) 0.82263(6) 0.3404(3) 0.0355(5) Uani 1 1 d . . . C31 C 0.56319(6) 0.80757(8) 0.1845(3) 0.0595(8) Uani 1 1 d . . . H31A H 0.5813 0.7966 0.1562 0.089 Uiso 1 1 calc R . . H31B H 0.5590 0.8228 0.1067 0.089 Uiso 1 1 calc R . . H31C H 0.5464 0.7937 0.1910 0.089 Uiso 1 1 calc R . . N1 N 0.47772(4) 0.87778(4) 0.30046(19) 0.0266(4) Uani 1 1 d . . . N2 N 0.46718(4) 0.85975(4) 0.4224(2) 0.0279(4) Uani 1 1 d . . . N3 N 0.59212(4) 0.83412(4) 0.5640(2) 0.0314(4) Uani 1 1 d . . . N4 N 0.59347(4) 0.81931(4) 0.4236(2) 0.0332(4) Uani 1 1 d . . . H4A H 0.6090 0.8090 0.3922 0.040 Uiso 1 1 calc R . . O1 O 0.43123(4) 0.93352(4) 0.3466(2) 0.0508(5) Uani 1 1 d . . . O2 O 0.41974(4) 0.91166(4) 0.5766(2) 0.0481(4) Uani 1 1 d . . . O3 O 0.36619(4) 1.16075(3) 0.8695(2) 0.0412(4) Uani 1 1 d . . . O4 O 0.38570(4) 1.14423(4) 1.0969(2) 0.0434(4) Uani 1 1 d . . . O5 O 0.46469(5) 0.93122(4) 0.0371(2) 0.0568(5) Uani 1 1 d . . . O6 O 0.46998(5) 0.89280(4) -0.1312(2) 0.0596(5) 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 0.02485(16) 0.02177(15) 0.02578(16) 0.00368(11) -0.00322(12) -0.00110(12) Co2 0.02297(15) 0.02007(15) 0.03116(17) 0.00266(12) 0.00275(12) -0.00135(11) C1 0.0359(13) 0.0296(13) 0.0640(18) -0.0111(13) -0.0050(12) 0.0027(11) C2 0.0566(17) 0.0278(13) 0.0606(17) -0.0130(12) 0.0105(14) 0.0024(12) C3 0.096(2) 0.0292(14) 0.071(2) -0.0087(14) 0.0240(18) -0.0019(15) C4 0.109(3) 0.0364(16) 0.071(2) -0.0139(15) 0.037(2) 0.0021(17) C5 0.075(2) 0.0282(14) 0.075(2) -0.0155(14) 0.0204(17) 0.0056(14) C6 0.089(2) 0.0295(14) 0.074(2) -0.0074(14) 0.0209(18) 0.0055(15) C7 0.081(2) 0.0330(14) 0.0649(19) -0.0105(13) 0.0198(16) 0.0090(14) C8 0.068(2) 0.0323(14) 0.0687(19) -0.0141(13) 0.0146(16) 0.0039(14) C9 0.088(2) 0.0277(14) 0.074(2) -0.0083(14) 0.0027(18) 0.0139(15) C10 0.0688(19) 0.0318(14) 0.0607(17) -0.0127(13) -0.0038(15) 0.0083(13) C11 0.0416(14) 0.0242(12) 0.0578(16) -0.0114(11) 0.0051(12) 0.0017(10) C12 0.079(2) 0.0291(13) 0.0582(18) -0.0094(12) 0.0067(15) 0.0085(14) C13 0.096(2) 0.0373(15) 0.0593(19) -0.0182(14) 0.0079(17) 0.0104(16) C14 0.0292(12) 0.0269(12) 0.0511(15) -0.0092(11) 0.0071(11) -0.0026(10) C15 0.0408(14) 0.0481(16) 0.0465(16) 0.0267(13) -0.0101(12) -0.0138(12) C16 0.0537(16) 0.0377(14) 0.0431(15) 0.0167(11) -0.0097(12) -0.0223(12) C17 0.162(4) 0.0500(18) 0.0313(15) 0.0088(13) 0.0059(18) -0.042(2) C18 0.177(4) 0.0357(16) 0.0401(16) 0.0058(13) 0.005(2) -0.040(2) C19 0.0698(18) 0.0383(14) 0.0345(13) 0.0129(11) -0.0035(13) -0.0252(13) C20 0.0555(16) 0.0439(15) 0.0395(14) 0.0103(12) 0.0042(12) -0.0110(13) C21 0.0481(15) 0.0311(13) 0.0507(16) 0.0146(11) -0.0018(12) -0.0069(11) C22 0.0260(13) 0.088(2) 0.0610(18) 0.0366(16) 0.0077(12) 0.0021(14) C23 0.0238(11) 0.0404(13) 0.0300(12) 0.0084(10) -0.0016(9) 0.0017(10) C24 0.0228(11) 0.0398(13) 0.0292(11) 0.0060(10) -0.0012(9) 0.0054(10) C25 0.0271(11) 0.0370(13) 0.0345(12) 0.0115(10) 0.0014(9) 0.0070(10) C26 0.0425(16) 0.077(2) 0.080(2) 0.0527(18) 0.0172(15) 0.0254(15) C27 0.0537(18) 0.096(3) 0.0588(18) -0.0295(17) -0.0158(15) 0.0429(18) C28 0.0291(12) 0.0397(13) 0.0358(13) 0.0043(10) 0.0000(10) 0.0118(10) C29 0.0241(11) 0.0396(13) 0.0329(12) 0.0089(10) 0.0003(9) 0.0061(10) C30 0.0239(11) 0.0507(15) 0.0319(12) 0.0066(11) 0.0002(9) 0.0064(11) C31 0.0419(15) 0.096(2) 0.0407(15) -0.0150(15) -0.0046(12) 0.0062(16) N1 0.0218(9) 0.0316(10) 0.0265(9) 0.0090(8) -0.0001(7) 0.0001(7) N2 0.0219(9) 0.0318(10) 0.0300(10) 0.0102(8) 0.0035(7) 0.0007(8) N3 0.0271(10) 0.0373(10) 0.0298(10) 0.0035(8) -0.0001(8) 0.0123(8) N4 0.0239(9) 0.0449(11) 0.0307(10) -0.0005(9) 0.0040(8) 0.0101(8) O1 0.0635(12) 0.0356(10) 0.0534(11) -0.0174(8) -0.0001(9) 0.0121(9) O2 0.0560(11) 0.0252(9) 0.0632(12) -0.0105(8) 0.0018(9) 0.0039(8) O3 0.0510(10) 0.0267(8) 0.0460(10) -0.0080(7) 0.0060(8) 0.0048(8) O4 0.0471(10) 0.0314(9) 0.0518(11) -0.0146(8) -0.0061(8) 0.0068(8) O5 0.0681(13) 0.0508(11) 0.0516(12) 0.0281(9) 0.0021(10) -0.0112(10) O6 0.0647(13) 0.0407(11) 0.0736(13) 0.0261(10) -0.0120(10) -0.0240(10) _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 1.9207(17) . ? Co1 O1 1.9669(17) . ? Co1 O3 1.9705(16) 8_353 ? Co1 N1 1.9890(17) . ? Co2 O2 1.9419(16) . ? Co2 O4 1.9660(16) 8_353 ? Co2 N2 1.9933(17) . ? Co2 N3 2.0223(18) 12_767 ? C1 O1 1.258(3) . ? C1 O2 1.266(3) . ? C1 C2 1.501(3) . ? C2 C7 1.381(4) . ? C2 C3 1.382(4) . ? C3 C4 1.383(4) . ? C3 H3 0.9300 . ? C4 C5 1.399(4) . ? C4 H4 0.9300 . ? C5 C6 1.387(4) . ? C5 C8 1.497(3) . ? C6 C7 1.398(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C13 1.388(4) . ? C8 C9 1.392(4) . ? C9 C10 1.385(3) . ? C9 H9 0.9300 . ? C10 C11 1.386(4) . ? C10 H10 0.9300 . ? C11 C12 1.385(4) . ? C11 C14 1.503(3) . ? C12 C13 1.393(3) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 O3 1.258(3) . ? C14 O4 1.264(3) . ? C15 O6 1.235(3) . ? C15 O5 1.289(3) . ? C15 C16 1.509(3) . ? C16 C21 1.381(4) . ? C16 C17 1.388(4) . ? C17 C18 1.384(4) . ? C17 H17 0.9300 . ? C18 C19 1.389(4) . ? C18 H18 0.9300 . ? C19 C20 1.392(4) . ? C19 C19 1.504(4) 9_674 ? C20 C21 1.392(3) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.500(3) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 N1 1.342(3) . ? C23 C24 1.401(3) . ? C24 C25 1.396(3) . ? C24 C29 1.485(3) . ? C25 N2 1.346(3) . ? C25 C26 1.510(3) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.501(3) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 N3 1.351(3) . ? C28 C29 1.401(3) . ? C29 C30 1.387(3) . ? C30 N4 1.340(3) . ? C30 C31 1.500(3) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? N1 N2 1.387(2) . ? N3 N4 1.366(2) . ? N3 Co2 2.0223(17) 15_566 ? N4 H4A 0.8600 . ? O3 Co1 1.9705(16) 7 ? O4 Co2 1.9660(16) 7 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Co1 O1 102.22(9) . . ? O5 Co1 O3 112.38(8) . 8_353 ? O1 Co1 O3 101.85(8) . 8_353 ? O5 Co1 N1 115.22(8) . . ? O1 Co1 N1 108.65(8) . . ? O3 Co1 N1 114.72(7) 8_353 . ? O2 Co2 O4 103.62(7) . 8_353 ? O2 Co2 N2 117.19(8) . . ? O4 Co2 N2 111.64(7) 8_353 . ? O2 Co2 N3 107.63(8) . 12_767 ? O4 Co2 N3 106.67(7) 8_353 12_767 ? N2 Co2 N3 109.47(7) . 12_767 ? O1 C1 O2 125.5(2) . . ? O1 C1 C2 117.0(2) . . ? O2 C1 C2 117.5(2) . . ? C7 C2 C3 119.4(2) . . ? C7 C2 C1 119.9(3) . . ? C3 C2 C1 120.7(2) . . ? C2 C3 C4 120.6(3) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C5 120.7(3) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 118.4(2) . . ? C6 C5 C8 120.9(3) . . ? C4 C5 C8 120.7(3) . . ? C5 C6 C7 120.5(3) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C2 C7 C6 120.4(3) . . ? C2 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C13 C8 C9 118.6(2) . . ? C13 C8 C5 121.1(3) . . ? C9 C8 C5 120.3(3) . . ? C10 C9 C8 120.8(3) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C9 C10 C11 120.4(3) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 119.4(2) . . ? C12 C11 C14 120.9(2) . . ? C10 C11 C14 119.7(2) . . ? C11 C12 C13 120.2(3) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C8 C13 C12 120.7(3) . . ? C8 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? O3 C14 O4 125.6(2) . . ? O3 C14 C11 117.6(2) . . ? O4 C14 C11 116.8(2) . . ? O6 C15 O5 124.1(2) . . ? O6 C15 C16 121.6(3) . . ? O5 C15 C16 114.3(2) . . ? C21 C16 C17 118.9(2) . . ? C21 C16 C15 121.3(2) . . ? C17 C16 C15 119.7(3) . . ? C18 C17 C16 120.4(3) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 121.5(3) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C18 C19 C20 117.4(2) . . ? C18 C19 C19 121.2(3) . 9_674 ? C20 C19 C19 121.4(3) . 9_674 ? C19 C20 C21 121.4(2) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C16 C21 C20 120.3(2) . . ? C16 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N1 C23 C24 109.17(18) . . ? N1 C23 C22 121.93(19) . . ? C24 C23 C22 128.9(2) . . ? C25 C24 C23 105.12(18) . . ? C25 C24 C29 126.12(19) . . ? C23 C24 C29 128.42(19) . . ? N2 C25 C24 109.56(18) . . ? N2 C25 C26 122.4(2) . . ? C24 C25 C26 128.0(2) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C28 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 C29 109.93(19) . . ? N3 C28 C27 121.7(2) . . ? C29 C28 C27 128.4(2) . . ? C30 C29 C28 106.03(19) . . ? C30 C29 C24 129.3(2) . . ? C28 C29 C24 124.7(2) . . ? N4 C30 C29 106.6(2) . . ? N4 C30 C31 122.4(2) . . ? C29 C30 C31 130.9(2) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C23 N1 N2 108.39(16) . . ? C23 N1 Co1 133.95(14) . . ? N2 N1 Co1 117.65(12) . . ? C25 N2 N1 107.75(16) . . ? C25 N2 Co2 134.25(14) . . ? N1 N2 Co2 116.06(12) . . ? C28 N3 N4 105.26(17) . . ? C28 N3 Co2 129.15(15) . 15_566 ? N4 N3 Co2 122.41(13) . 15_566 ? C30 N4 N3 112.13(18) . . ? C30 N4 H4A 123.9 . . ? N3 N4 H4A 123.9 . . ? C1 O1 Co1 140.18(17) . . ? C1 O2 Co2 122.68(17) . . ? C14 O3 Co1 126.18(15) . 7 ? C14 O4 Co2 135.49(15) . 7 ? C15 O5 Co1 118.71(16) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.339 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.052