# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_'CoIMI4PIC' _database_code_depnum_ccdc_archive 'CCDC 889588' _audit_creation_method SHELXL97 _chemical_name_systematic ; poly-[[dekakis(mu-imidazolato-KN:KN')pentacobalt(II)]-water-4-methylpyridine (1/8/1) ; _chemical_formula_moiety 'C30 H30 Co5 N20, 8 (H2 O), C6 H7 N' _chemical_formula_structural 'C30 H30 Co5 N20, 8 (H2 O), C6 H7 N' _chemical_formula_sum 'C36 H53 Co5 N21 O8' _chemical_formula_weight 1202.64 _chemical_compound_source 'synthesis as described' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 24.3302(11) _cell_length_b 9.5623(5) _cell_length_c 24.6111(16) _cell_angle_alpha 90.00 _cell_angle_beta 91.542(5) _cell_angle_gamma 90.00 _cell_volume 5723.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21401 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 67.14 _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2460 _exptl_absorpt_coefficient_mu 11.624 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++) (compiled Jun 6 2003,13:53:32) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _exptl_absorpt_correction_T_min 0.273 _exptl_absorpt_correction_T_max 0.349 _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Xcalibur _diffrn_measurement_method \w _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21401 _diffrn_reflns_av_R_equivalents 0.1220 _diffrn_reflns_av_sigmaI/netI 0.1708 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 67.14 _reflns_number_total 10225 _reflns_number_gt 4296 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2003)' _computing_cell_refinement 'CrysAlis CCD (Oxford Diffraction, 2003)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2003)' _computing_structure_solution 'Sir92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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. ; # 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 -0.071 0.000 1148 259 ' ' 2 0.500 -0.015 0.500 1148 259 ' ' _platon_squeeze_details ; ; _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^)+(0.0534P)^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 10225 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1221 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1551 _refine_ls_wR_factor_gt 0.1361 _refine_ls_goodness_of_fit_ref 0.754 _refine_ls_restrained_S_all 0.754 _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 -0.21603(4) 0.04199(12) 0.81698(5) 0.0544(3) Uani 1 1 d . . . Co2 Co 0.01477(4) 0.23587(11) 0.77837(5) 0.0534(3) Uani 1 1 d . . . Co3 Co 0.23582(4) 0.44928(11) 0.81975(4) 0.0477(3) Uani 1 1 d . . . Co4 Co 0.34085(4) 0.81757(11) 0.98274(4) 0.0497(3) Uani 1 1 d . . . Co5 Co 0.53405(4) 0.76987(11) 1.13781(5) 0.0534(3) Uani 1 1 d . . . N11 N -0.2599(2) 0.1759(6) 0.7715(3) 0.0589(16) Uani 1 1 d . . . C12 C -0.2462(3) 0.2974(8) 0.7507(3) 0.064(2) Uani 1 1 d . . . H12 H -0.2119 0.3378 0.7568 0.077 Uiso 1 1 calc R . . N13 N -0.2850(2) 0.3572(6) 0.7205(2) 0.0604(16) Uani 1 1 d . . . C14 C -0.3285(3) 0.2713(9) 0.7232(4) 0.091(3) Uani 1 1 d . . . H14 H -0.3629 0.2860 0.7070 0.109 Uiso 1 1 calc R . . C15 C -0.3130(3) 0.1574(9) 0.7542(4) 0.102(4) Uani 1 1 d . . . H15 H -0.3350 0.0810 0.7620 0.122 Uiso 1 1 calc R . . N21 N -0.1382(2) 0.1043(6) 0.8297(3) 0.0646(17) Uani 1 1 d . . . C22 C -0.0996(3) 0.1280(8) 0.7940(3) 0.061(2) Uani 1 1 d . . . H22 H -0.1059 0.1185 0.7568 0.073 Uiso 1 1 calc R . . N23 N -0.0509(2) 0.1668(6) 0.8155(2) 0.0602(16) Uani 1 1 d . . . C24 C -0.0603(3) 0.1654(11) 0.8696(4) 0.106(4) Uani 1 1 d . . . H24 H -0.0347 0.1873 0.8970 0.127 Uiso 1 1 calc R . . C25 C -0.1121(4) 0.1276(12) 0.8769(4) 0.122(4) Uani 1 1 d . . . H25 H -0.1281 0.1187 0.9107 0.146 Uiso 1 1 calc R . . N31 N -0.0067(2) 0.4178(6) 0.7437(2) 0.0548(15) Uani 1 1 d . . . C32 C 0.0189(3) 0.4832(8) 0.7041(3) 0.0584(19) Uani 1 1 d . . . H32 H 0.0487 0.4446 0.6866 0.070 Uiso 1 1 calc R . . N33 N -0.0017(2) 0.6089(6) 0.6914(2) 0.0549(15) Uani 1 1 d . . . C34 C -0.0451(3) 0.6243(9) 0.7253(4) 0.081(3) Uani 1 1 d . . . H34 H -0.0682 0.7016 0.7269 0.097 Uiso 1 1 calc R . . C35 C -0.0485(3) 0.5062(8) 0.7565(3) 0.070(2) Uani 1 1 d . . . H35 H -0.0750 0.4890 0.7821 0.084 Uiso 1 1 calc R . . N41 N 0.0413(2) 0.1051(5) 0.7215(2) 0.0478(13) Uani 1 1 d . . . C42 C 0.0234(3) -0.0252(7) 0.7115(3) 0.0581(19) Uani 1 1 d . . . H42 H -0.0042 -0.0686 0.7308 0.070 Uiso 1 1 calc R . . N43 N 0.0498(2) -0.0861(6) 0.6706(2) 0.0537(15) Uani 1 1 d . . . C44 C 0.0871(3) 0.0136(7) 0.6544(3) 0.059(2) Uani 1 1 d . . . H44 H 0.1122 0.0018 0.6269 0.070 Uiso 1 1 calc R . . C45 C 0.0817(3) 0.1304(8) 0.6844(3) 0.0596(19) Uani 1 1 d . . . H45 H 0.1015 0.2129 0.6808 0.072 Uiso 1 1 calc R . . N51 N 0.0812(2) 0.2701(6) 0.8256(3) 0.0578(15) Uani 1 1 d . . . C52 C 0.1182(3) 0.3670(7) 0.8125(3) 0.0585(19) Uani 1 1 d . . . H52 H 0.1106 0.4388 0.7880 0.070 Uiso 1 1 calc R . . N53 N 0.1669(2) 0.3514(6) 0.8378(2) 0.0519(15) Uani 1 1 d . . . C54 C 0.1604(3) 0.2330(9) 0.8690(4) 0.082(3) Uani 1 1 d . . . H54 H 0.1873 0.1922 0.8914 0.099 Uiso 1 1 calc R . . C55 C 0.1076(3) 0.1858(9) 0.8615(3) 0.076(2) Uani 1 1 d . . . H55 H 0.0925 0.1083 0.8783 0.091 Uiso 1 1 calc R . . N61 N 0.2715(2) 0.3266(5) 0.7657(2) 0.0438(13) Uani 1 1 d . . . C62 C 0.2519(2) 0.2018(6) 0.7513(3) 0.0445(15) Uani 1 1 d . . . H62 H 0.2200 0.1641 0.7654 0.053 Uiso 1 1 calc R . . N63 N 0.2822(2) 0.1353(5) 0.7148(2) 0.0505(14) Uani 1 1 d . . . C64 C 0.3248(2) 0.2276(7) 0.7061(3) 0.0511(17) Uani 1 1 d . . . H64 H 0.3535 0.2122 0.6827 0.061 Uiso 1 1 calc R . . C65 C 0.3185(3) 0.3419(7) 0.7363(3) 0.0568(19) Uani 1 1 d . . . H65 H 0.3418 0.4190 0.7373 0.068 Uiso 1 1 calc R . . N71 N 0.27690(19) 0.4956(6) 0.8877(2) 0.0495(14) Uani 1 1 d . . . C72 C 0.2874(2) 0.6271(7) 0.9024(3) 0.0522(18) Uani 1 1 d . . . H72 H 0.2768 0.7037 0.8814 0.063 Uiso 1 1 calc R . . N73 N 0.31412(19) 0.6392(5) 0.9497(2) 0.0458(13) Uani 1 1 d . . . C74 C 0.3224(3) 0.5049(8) 0.9674(3) 0.0593(19) Uani 1 1 d . . . H74 H 0.3413 0.4789 0.9992 0.071 Uiso 1 1 calc R . . C75 C 0.2985(3) 0.4162(8) 0.9307(3) 0.062(2) Uani 1 1 d . . . H75 H 0.2968 0.3193 0.9338 0.074 Uiso 1 1 calc R . . N81 N 0.3521(2) 0.9570(6) 0.9231(2) 0.0550(15) Uani 1 1 d . . . C82 C 0.3974(3) 1.0342(7) 0.9228(3) 0.0532(18) Uani 1 1 d . . . H82 H 0.4255 1.0269 0.9490 0.064 Uiso 1 1 calc R . . N83 N 0.3986(2) 1.1234(6) 0.8810(2) 0.0543(15) Uani 1 1 d . . . C84 C 0.3500(3) 1.1009(7) 0.8527(3) 0.058(2) Uani 1 1 d . . . H84 H 0.3385 1.1479 0.8213 0.070 Uiso 1 1 calc R . . C85 C 0.3216(3) 0.9991(7) 0.8780(3) 0.0519(18) Uani 1 1 d . . . H85 H 0.2874 0.9640 0.8669 0.062 Uiso 1 1 calc R . . N91 N 0.2949(2) 0.9161(6) 1.0359(2) 0.0507(14) Uani 1 1 d . . . C92 C 0.2807(3) 0.8786(7) 1.0846(3) 0.0564(19) Uani 1 1 d . . . H92 H 0.2915 0.7943 1.1003 0.068 Uiso 1 1 calc R . . N93 N 0.2501(2) 0.9693(6) 1.1093(2) 0.0543(15) Uani 1 1 d . . . C94 C 0.2432(4) 1.0777(9) 1.0730(4) 0.103(4) Uani 1 1 d . . . H94 H 0.2237 1.1599 1.0788 0.124 Uiso 1 1 calc R . . C95 C 0.2701(4) 1.0426(10) 1.0270(4) 0.093(3) Uani 1 1 d . . . H95 H 0.2713 1.0953 0.9953 0.112 Uiso 1 1 calc R . . N101 N 0.4146(2) 0.7717(6) 1.0143(2) 0.0532(15) Uani 1 1 d . . . C102 C 0.4362(3) 0.8035(7) 1.0621(3) 0.0509(17) Uani 1 1 d . . . H102 H 0.4175 0.8559 1.0875 0.061 Uiso 1 1 calc R . . N103 N 0.4870(2) 0.7552(6) 1.0716(3) 0.0583(15) Uani 1 1 d . . . C104 C 0.4992(3) 0.6880(8) 1.0226(3) 0.070(2) Uani 1 1 d . . . H104 H 0.5322 0.6454 1.0140 0.084 Uiso 1 1 calc R . . C105 C 0.4541(3) 0.6975(8) 0.9908(3) 0.067(2) Uani 1 1 d . . . H105 H 0.4504 0.6574 0.9565 0.081 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 0.0365(6) 0.0593(7) 0.0678(8) -0.0004(6) 0.0068(5) -0.0026(5) Co2 0.0347(5) 0.0521(7) 0.0735(8) -0.0044(6) 0.0002(5) -0.0040(5) Co3 0.0360(5) 0.0465(6) 0.0599(7) -0.0004(6) -0.0111(5) -0.0036(5) Co4 0.0376(5) 0.0586(7) 0.0523(7) 0.0000(5) -0.0073(5) -0.0036(5) Co5 0.0411(6) 0.0530(7) 0.0652(7) 0.0069(6) -0.0172(5) -0.0022(5) N11 0.033(3) 0.062(4) 0.082(5) 0.004(3) 0.005(3) 0.001(3) C12 0.033(4) 0.073(6) 0.087(6) -0.009(4) 0.000(4) -0.013(3) N13 0.043(3) 0.064(4) 0.075(4) -0.002(3) 0.005(3) -0.003(3) C14 0.028(4) 0.086(7) 0.158(10) 0.010(6) -0.005(5) -0.006(4) C15 0.046(5) 0.073(6) 0.185(11) 0.037(7) -0.026(6) -0.006(4) N21 0.035(3) 0.076(4) 0.083(5) 0.002(4) 0.006(3) -0.012(3) C22 0.044(4) 0.078(6) 0.059(5) -0.008(4) 0.006(4) -0.007(4) N23 0.029(3) 0.083(5) 0.070(4) -0.001(3) 0.010(3) -0.008(3) C24 0.042(5) 0.206(11) 0.069(6) -0.024(7) -0.009(4) -0.034(6) C25 0.064(6) 0.254(14) 0.049(5) -0.009(7) 0.003(4) -0.044(7) N31 0.032(3) 0.049(4) 0.083(4) -0.007(3) -0.007(3) -0.003(2) C32 0.046(4) 0.063(5) 0.067(5) -0.006(4) 0.008(4) -0.004(4) N33 0.041(3) 0.051(4) 0.071(4) -0.009(3) -0.018(3) 0.003(3) C34 0.051(5) 0.076(6) 0.117(8) -0.002(5) 0.012(5) 0.006(4) C35 0.043(4) 0.057(5) 0.110(7) 0.015(5) 0.019(4) -0.001(3) N41 0.045(3) 0.044(3) 0.054(3) -0.008(3) 0.001(3) -0.004(2) C42 0.050(4) 0.053(5) 0.070(5) 0.005(4) -0.020(4) -0.008(4) N43 0.037(3) 0.052(4) 0.071(4) -0.005(3) -0.016(3) 0.000(3) C44 0.037(4) 0.060(5) 0.079(5) -0.004(4) -0.002(4) 0.002(3) C45 0.050(4) 0.057(5) 0.071(5) 0.009(4) 0.000(4) -0.002(3) N51 0.046(3) 0.049(4) 0.078(4) -0.002(3) -0.006(3) -0.002(3) C52 0.056(4) 0.052(5) 0.067(5) 0.009(4) -0.012(4) -0.010(4) N53 0.037(3) 0.051(4) 0.068(4) 0.002(3) -0.004(3) -0.011(3) C54 0.050(5) 0.091(7) 0.105(7) 0.027(6) -0.015(4) -0.010(4) C55 0.054(5) 0.087(6) 0.086(6) 0.022(5) -0.013(4) -0.012(4) N61 0.047(3) 0.041(3) 0.043(3) -0.003(3) -0.005(2) 0.002(2) C62 0.037(3) 0.048(4) 0.048(4) 0.002(3) -0.009(3) -0.007(3) N63 0.044(3) 0.050(4) 0.057(4) -0.004(3) -0.012(3) 0.008(3) C64 0.033(3) 0.063(5) 0.058(4) 0.003(4) 0.008(3) -0.005(3) C65 0.053(4) 0.044(4) 0.073(5) 0.009(4) -0.003(4) -0.005(3) N71 0.031(3) 0.060(4) 0.058(4) 0.004(3) -0.003(2) -0.006(2) C72 0.029(3) 0.059(5) 0.068(5) 0.010(4) -0.016(3) -0.013(3) N73 0.030(3) 0.050(4) 0.057(4) -0.001(3) -0.006(2) -0.005(2) C74 0.049(4) 0.071(5) 0.057(5) -0.007(4) -0.008(3) -0.011(4) C75 0.056(4) 0.056(5) 0.072(5) 0.006(4) -0.023(4) -0.003(3) N81 0.038(3) 0.065(4) 0.061(4) 0.010(3) -0.012(3) 0.004(3) C82 0.042(4) 0.059(5) 0.058(4) -0.006(4) -0.016(3) 0.001(3) N83 0.041(3) 0.057(4) 0.065(4) -0.001(3) -0.008(3) -0.002(3) C84 0.040(4) 0.076(5) 0.059(5) 0.007(4) -0.019(3) 0.011(3) C85 0.035(3) 0.047(4) 0.072(5) 0.002(4) -0.015(3) 0.002(3) N91 0.038(3) 0.064(4) 0.050(4) 0.004(3) 0.004(3) 0.000(3) C92 0.042(4) 0.050(4) 0.077(6) -0.004(4) -0.007(4) 0.000(3) N93 0.048(3) 0.067(4) 0.048(3) 0.009(3) 0.008(3) -0.002(3) C94 0.105(8) 0.073(7) 0.134(9) 0.031(6) 0.047(7) 0.045(5) C95 0.099(7) 0.096(7) 0.086(7) 0.038(6) 0.024(6) 0.038(6) N101 0.037(3) 0.057(4) 0.065(4) -0.006(3) -0.018(3) 0.002(3) C102 0.040(3) 0.052(4) 0.060(4) 0.002(3) -0.008(3) -0.002(3) N103 0.047(3) 0.052(4) 0.076(4) 0.000(3) -0.021(3) 0.001(3) C104 0.048(4) 0.072(5) 0.090(6) -0.015(5) -0.005(4) 0.014(4) C105 0.058(5) 0.077(6) 0.066(5) -0.007(4) -0.026(4) 0.004(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 Co1 N11 1.992(6) . ? Co1 N13 1.994(6) 2_446 ? Co1 N21 2.001(5) . ? Co1 N93 2.018(5) 3_567 ? Co2 N23 1.975(5) . ? Co2 N51 1.993(6) . ? Co2 N41 1.997(5) . ? Co2 N31 2.001(6) . ? Co3 N71 1.975(5) . ? Co3 N53 1.981(5) . ? Co3 N61 1.991(5) . ? Co3 N63 2.015(5) 2_556 ? Co4 N91 1.982(6) . ? Co4 N101 1.986(5) . ? Co4 N73 1.991(5) . ? Co4 N81 2.007(6) . ? Co5 N43 1.967(5) 4_666 ? Co5 N103 1.972(5) . ? Co5 N33 1.975(6) 4_676 ? Co5 N83 1.995(6) 3_677 ? N11 C12 1.315(8) . ? N11 C15 1.360(9) . ? C12 N13 1.316(9) . ? C12 H12 0.9300 . ? N13 C14 1.342(9) . ? N13 Co1 1.994(6) 2_456 ? C14 C15 1.376(11) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? N21 C22 1.323(9) . ? N21 C25 1.328(10) . ? C22 N23 1.337(8) . ? C22 H22 0.9300 . ? N23 C24 1.357(10) . ? C24 C25 1.330(11) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? N31 C32 1.328(9) . ? N31 C35 1.365(8) . ? C32 N33 1.336(8) . ? C32 H32 0.9300 . ? N33 C34 1.372(9) . ? N33 Co5 1.975(6) 4_575 ? C34 C35 1.369(10) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? N41 C42 1.340(8) . ? N41 C45 1.381(9) . ? C42 N43 1.342(9) . ? C42 H42 0.9300 . ? N43 C44 1.383(8) . ? N43 Co5 1.967(5) 4_565 ? C44 C45 1.348(9) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? N51 C52 1.337(8) . ? N51 C55 1.345(9) . ? C52 N53 1.331(8) . ? C52 H52 0.9300 . ? N53 C54 1.380(9) . ? C54 C55 1.369(10) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? N61 C62 1.329(7) . ? N61 C65 1.377(8) . ? C62 N63 1.338(8) . ? C62 H62 0.9300 . ? N63 C64 1.383(8) . ? N63 Co3 2.015(5) 2_546 ? C64 C65 1.333(9) . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? N71 C72 1.332(8) . ? N71 C75 1.394(8) . ? C72 N73 1.323(8) . ? C72 H72 0.9300 . ? N73 C74 1.370(8) . ? C74 C75 1.360(9) . ? C74 H74 0.9300 . ? C75 H75 0.9300 . ? N81 C82 1.327(8) . ? N81 C85 1.377(7) . ? C82 N83 1.336(8) . ? C82 H82 0.9300 . ? N83 C84 1.372(7) . ? N83 Co5 1.995(5) 3_677 ? C84 C85 1.356(9) . ? C84 H84 0.9300 . ? C85 H85 0.9300 . ? N91 C92 1.305(9) . ? N91 C95 1.367(9) . ? C92 N93 1.304(8) . ? C92 H92 0.9300 . ? N93 C94 1.376(9) . ? N93 Co1 2.018(5) 3_567 ? C94 C95 1.366(12) . ? C94 H94 0.9300 . ? C95 H95 0.9300 . ? N101 C102 1.310(8) . ? N101 C105 1.336(9) . ? C102 N103 1.333(8) . ? C102 H102 0.9300 . ? N103 C104 1.406(9) . ? C104 C105 1.334(9) . ? C104 H104 0.9300 . ? C105 H105 0.9300 . ? 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 N11 Co1 N13 108.9(3) . 2_446 ? N11 Co1 N21 112.8(2) . . ? N13 Co1 N21 108.2(2) 2_446 . ? N11 Co1 N93 108.2(2) . 3_567 ? N13 Co1 N93 112.3(2) 2_446 3_567 ? N21 Co1 N93 106.6(2) . 3_567 ? N23 Co2 N51 116.0(3) . . ? N23 Co2 N41 113.3(2) . . ? N51 Co2 N41 103.9(2) . . ? N23 Co2 N31 106.4(2) . . ? N51 Co2 N31 107.7(2) . . ? N41 Co2 N31 109.3(2) . . ? N71 Co3 N53 109.2(2) . . ? N71 Co3 N61 118.6(2) . . ? N53 Co3 N61 105.0(2) . . ? N71 Co3 N63 105.0(2) . 2_556 ? N53 Co3 N63 109.6(2) . 2_556 ? N61 Co3 N63 109.4(2) . 2_556 ? N91 Co4 N101 111.5(2) . . ? N91 Co4 N73 119.5(2) . . ? N101 Co4 N73 104.6(2) . . ? N91 Co4 N81 104.9(2) . . ? N101 Co4 N81 107.1(2) . . ? N73 Co4 N81 108.7(2) . . ? N43 Co5 N103 112.2(2) 4_666 . ? N43 Co5 N33 109.6(3) 4_666 4_676 ? N103 Co5 N33 109.7(2) . 4_676 ? N43 Co5 N83 113.6(2) 4_666 3_677 ? N103 Co5 N83 107.8(2) . 3_677 ? N33 Co5 N83 103.5(2) 4_676 3_677 ? C12 N11 C15 103.9(6) . . ? C12 N11 Co1 130.5(5) . . ? C15 N11 Co1 125.6(5) . . ? N11 C12 N13 114.7(6) . . ? N11 C12 H12 122.6 . . ? N13 C12 H12 122.6 . . ? C12 N13 C14 105.0(7) . . ? C12 N13 Co1 128.9(5) . 2_456 ? C14 N13 Co1 125.9(6) . 2_456 ? N13 C14 C15 107.9(7) . . ? N13 C14 H14 126.0 . . ? C15 C14 H14 126.0 . . ? N11 C15 C14 108.3(7) . . ? N11 C15 H15 125.9 . . ? C14 C15 H15 125.9 . . ? C22 N21 C25 102.7(6) . . ? C22 N21 Co1 129.3(5) . . ? C25 N21 Co1 128.0(6) . . ? N21 C22 N23 115.1(7) . . ? N21 C22 H22 122.5 . . ? N23 C22 H22 122.5 . . ? C22 N23 C24 102.4(6) . . ? C22 N23 Co2 129.0(5) . . ? C24 N23 Co2 128.1(5) . . ? C25 C24 N23 108.7(7) . . ? C25 C24 H24 125.6 . . ? N23 C24 H24 125.6 . . ? N21 C25 C24 111.1(8) . . ? N21 C25 H25 124.4 . . ? C24 C25 H25 124.4 . . ? C32 N31 C35 104.1(6) . . ? C32 N31 Co2 126.9(5) . . ? C35 N31 Co2 128.9(5) . . ? N31 C32 N33 114.6(7) . . ? N31 C32 H32 122.7 . . ? N33 C32 H32 122.7 . . ? C32 N33 C34 104.1(6) . . ? C32 N33 Co5 121.1(5) . 4_575 ? C34 N33 Co5 134.7(5) . 4_575 ? C35 C34 N33 108.2(7) . . ? C35 C34 H34 125.9 . . ? N33 C34 H34 125.9 . . ? N31 C35 C34 109.0(7) . . ? N31 C35 H35 125.5 . . ? C34 C35 H35 125.5 . . ? C42 N41 C45 106.0(6) . . ? C42 N41 Co2 127.0(5) . . ? C45 N41 Co2 127.1(5) . . ? N41 C42 N43 112.4(7) . . ? N41 C42 H42 123.8 . . ? N43 C42 H42 123.8 . . ? C42 N43 C44 104.4(6) . . ? C42 N43 Co5 127.2(5) . 4_565 ? C44 N43 Co5 128.3(5) . 4_565 ? C45 C44 N43 109.8(7) . . ? C45 C44 H44 125.1 . . ? N43 C44 H44 125.1 . . ? C44 C45 N41 107.4(6) . . ? C44 C45 H45 126.3 . . ? N41 C45 H45 126.3 . . ? C52 N51 C55 105.1(6) . . ? C52 N51 Co2 120.9(5) . . ? C55 N51 Co2 130.5(5) . . ? N53 C52 N51 114.0(6) . . ? N53 C52 H52 123.0 . . ? N51 C52 H52 123.0 . . ? C52 N53 C54 103.7(5) . . ? C52 N53 Co3 126.3(5) . . ? C54 N53 Co3 128.5(5) . . ? C55 C54 N53 108.4(7) . . ? C55 C54 H54 125.8 . . ? N53 C54 H54 125.8 . . ? N51 C55 C54 108.7(7) . . ? N51 C55 H55 125.6 . . ? C54 C55 H55 125.6 . . ? C62 N61 C65 104.6(5) . . ? C62 N61 Co3 123.1(5) . . ? C65 N61 Co3 132.2(5) . . ? N61 C62 N63 113.9(6) . . ? N61 C62 H62 123.1 . . ? N63 C62 H62 123.1 . . ? C62 N63 C64 103.3(5) . . ? C62 N63 Co3 125.9(5) . 2_546 ? C64 N63 Co3 130.8(5) . 2_546 ? C65 C64 N63 109.8(6) . . ? C65 C64 H64 125.1 . . ? N63 C64 H64 125.1 . . ? C64 C65 N61 108.4(6) . . ? C64 C65 H65 125.8 . . ? N61 C65 H65 125.8 . . ? C72 N71 C75 104.0(6) . . ? C72 N71 Co3 122.1(4) . . ? C75 N71 Co3 133.8(5) . . ? N73 C72 N71 114.1(6) . . ? N73 C72 H72 122.9 . . ? N71 C72 H72 122.9 . . ? C72 N73 C74 105.2(5) . . ? C72 N73 Co4 125.6(5) . . ? C74 N73 Co4 129.0(4) . . ? C75 C74 N73 108.5(6) . . ? C75 C74 H74 125.8 . . ? N73 C74 H74 125.8 . . ? C74 C75 N71 108.1(6) . . ? C74 C75 H75 126.0 . . ? N71 C75 H75 126.0 . . ? C82 N81 C85 105.2(6) . . ? C82 N81 Co4 120.2(4) . . ? C85 N81 Co4 134.6(5) . . ? N81 C82 N83 113.3(6) . . ? N81 C82 H82 123.4 . . ? N83 C82 H82 123.4 . . ? C82 N83 C84 104.7(6) . . ? C82 N83 Co5 122.7(4) . 3_677 ? C84 N83 Co5 131.6(5) . 3_677 ? C85 C84 N83 108.9(6) . . ? C85 C84 H84 125.6 . . ? N83 C84 H84 125.6 . . ? C84 C85 N81 108.0(5) . . ? C84 C85 H85 126.0 . . ? N81 C85 H85 126.0 . . ? C92 N91 C95 105.3(6) . . ? C92 N91 Co4 130.0(5) . . ? C95 N91 Co4 124.7(5) . . ? N93 C92 N91 114.5(7) . . ? N93 C92 H92 122.8 . . ? N91 C92 H92 122.8 . . ? C92 N93 C94 105.0(7) . . ? C92 N93 Co1 129.6(5) . 3_567 ? C94 N93 Co1 125.3(6) . 3_567 ? C95 C94 N93 107.5(7) . . ? C95 C94 H94 126.3 . . ? N93 C94 H94 126.3 . . ? C94 C95 N91 107.7(7) . . ? C94 C95 H95 126.2 . . ? N91 C95 H95 126.2 . . ? C102 N101 C105 103.7(5) . . ? C102 N101 Co4 129.5(5) . . ? C105 N101 Co4 126.9(5) . . ? N101 C102 N103 115.1(7) . . ? N101 C102 H102 122.5 . . ? N103 C102 H102 122.5 . . ? C102 N103 C104 103.0(6) . . ? C102 N103 Co5 129.4(5) . . ? C104 N103 Co5 127.6(5) . . ? C105 C104 N103 106.3(7) . . ? C105 C104 H104 126.8 . . ? N103 C104 H104 126.8 . . ? C104 C105 N101 111.9(7) . . ? C104 C105 H105 124.1 . . ? N101 C105 H105 124.1 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 67.14 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.515 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.082