# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers # This journal is © The Partner Organisations 2014 ####################################################################### # # 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_3 #TrackingRef '123.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H8 Co2 N6 O7' _chemical_formula_weight 394.04 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n 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 8.9980(9) _cell_length_b 7.7962(9) _cell_length_c 18.1677(18) _cell_angle_alpha 90.00 _cell_angle_beta 101.649(10) _cell_angle_gamma 90.00 _cell_volume 1248.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1808 _cell_measurement_theta_min 2.3581 _cell_measurement_theta_max 28.8893 _exptl_crystal_description Block _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.097 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 2.704 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.87502 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details CRYSALISPRO _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2116 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4496 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0749 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2178 _reflns_number_gt 1699 _reflns_threshold_expression >2sigma(I) _computing_data_collection CRYSALISPRO _computing_cell_refinement CRYSALISPRO _computing_data_reduction CRYSALISPRO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0504P)^2^+6.0835P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2178 _refine_ls_number_parameters 199 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0828 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1427 _refine_ls_wR_factor_gt 0.1335 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co -0.00385(10) 0.92065(12) 0.23742(5) 0.0126(3) Uani 1 1 d . . . Co2 Co 0.18500(10) 0.90150(12) 0.45367(5) 0.0149(3) Uani 1 1 d . . . O4 O -0.2210(5) 1.0301(7) 0.1898(3) 0.0220(12) Uani 1 1 d . . . N2 N -0.0212(6) 1.0254(8) 0.4041(3) 0.0167(13) Uani 1 1 d . . . N3 N -0.0663(6) 1.0379(7) 0.3298(3) 0.0147(13) Uani 1 1 d . . . O1 O -0.3776(6) 1.2064(7) 0.4760(3) 0.0262(13) Uani 1 1 d . . . N1 N -0.1273(6) 1.0892(8) 0.4372(3) 0.0171(13) Uani 1 1 d . . . O3 O -0.4030(6) 1.1966(7) 0.2157(3) 0.0222(12) Uani 1 1 d . . . O2 O -0.4835(5) 1.2856(7) 0.3621(3) 0.0211(12) Uani 1 1 d . . . C4 C -0.2830(7) 1.1169(9) 0.2344(4) 0.0131(15) Uani 1 1 d . . . C3 C -0.2049(8) 1.1099(8) 0.3153(4) 0.0140(15) Uani 1 1 d . . . C2 C -0.2446(8) 1.1439(9) 0.3828(4) 0.0138(15) Uani 1 1 d . . . C1 C -0.3794(8) 1.2188(9) 0.4073(4) 0.0177(16) Uani 1 1 d . . . N5 N 0.2043(6) 0.8173(8) 0.2870(3) 0.0182(14) Uani 1 1 d . . . N6 N 0.3977(7) 0.6360(8) 0.2984(3) 0.0205(14) Uani 1 1 d . . . N4 N 0.2738(6) 0.8114(8) 0.3614(3) 0.0174(14) Uani 1 1 d . . . C5 C 0.2809(8) 0.7106(10) 0.2520(4) 0.0218(18) Uani 1 1 d . . . H5 H 0.2562 0.6896 0.2006 0.026 Uiso 1 1 calc R . . C6 C 0.3882(8) 0.7038(10) 0.3653(4) 0.0209(17) Uani 1 1 d . . . H6 H 0.4554 0.6776 0.4098 0.025 Uiso 1 1 calc R . . O6 O 0.0634(6) 0.6620(8) 0.4344(3) 0.0263(13) Uani 1 1 d D . . O7 O -0.2189(7) 0.5940(7) 0.4631(3) 0.0375(15) Uani 1 1 d . . . O5 O 0.2977(6) 1.1351(7) 0.4612(3) 0.0362(15) Uani 1 1 d . . . H5A H 0.2584 1.2122 0.4888 0.054 Uiso 1 1 d R . . H5B H 0.3961 1.1235 0.4832 0.054 Uiso 1 1 d R . . H6A H -0.019(4) 0.656(9) 0.450(3) 0.009(18) Uiso 1 1 d D . . H6B H 0.056(12) 0.616(13) 0.391(3) 0.07(4) Uiso 1 1 d 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 0.0118(5) 0.0152(5) 0.0110(5) -0.0006(4) 0.0028(4) 0.0005(4) Co2 0.0133(5) 0.0216(6) 0.0092(5) -0.0007(4) 0.0014(4) 0.0044(4) O4 0.019(3) 0.028(3) 0.018(3) -0.001(2) 0.003(2) 0.006(2) N2 0.018(3) 0.024(3) 0.009(3) -0.001(3) 0.006(2) 0.001(3) N3 0.016(3) 0.019(3) 0.009(3) -0.003(2) 0.003(2) 0.001(3) O1 0.028(3) 0.043(4) 0.008(2) 0.007(2) 0.005(2) 0.017(3) N1 0.014(3) 0.024(4) 0.014(3) 0.000(3) 0.004(2) 0.001(3) O3 0.026(3) 0.026(3) 0.013(3) -0.004(2) -0.001(2) 0.013(3) O2 0.015(3) 0.029(3) 0.018(3) 0.005(2) 0.001(2) 0.005(2) C4 0.014(4) 0.011(4) 0.017(4) 0.001(3) 0.008(3) 0.002(3) C3 0.014(3) 0.010(4) 0.018(4) -0.004(3) 0.005(3) 0.002(3) C2 0.017(4) 0.015(4) 0.012(3) -0.001(3) 0.007(3) 0.005(3) C1 0.017(4) 0.017(4) 0.019(4) 0.002(3) 0.001(3) -0.001(3) N5 0.016(3) 0.026(4) 0.012(3) 0.003(3) 0.002(2) 0.004(3) N6 0.021(3) 0.024(4) 0.015(3) -0.002(3) -0.001(3) 0.008(3) N4 0.013(3) 0.025(4) 0.015(3) -0.002(3) 0.005(3) 0.005(3) C5 0.024(4) 0.028(5) 0.013(4) -0.005(3) 0.002(3) 0.008(4) C6 0.022(4) 0.034(5) 0.006(3) -0.002(3) 0.000(3) 0.008(4) O6 0.026(3) 0.026(3) 0.028(3) -0.003(3) 0.008(3) -0.005(3) O7 0.047(4) 0.029(3) 0.038(3) -0.007(3) 0.012(3) 0.001(3) O5 0.022(3) 0.035(3) 0.056(4) -0.017(3) 0.018(3) -0.005(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 N5 2.070(6) . ? Co1 O2 2.076(5) 2_445 ? Co1 N3 2.085(5) . ? Co1 N6 2.098(6) 2 ? Co1 O4 2.148(5) . ? Co1 O3 2.184(5) 2_445 ? Co2 O5 2.075(6) . ? Co2 O1 2.110(5) 3_576 ? Co2 N4 2.118(6) . ? Co2 N2 2.124(6) . ? Co2 N1 2.150(6) 3_576 ? Co2 O6 2.157(6) . ? O4 C4 1.267(8) . ? N2 N1 1.325(8) . ? N2 N3 1.332(7) . ? N3 C3 1.345(8) . ? O1 C1 1.249(8) . ? O1 Co2 2.110(5) 3_576 ? N1 C2 1.360(9) . ? N1 Co2 2.150(6) 3_576 ? O3 C4 1.232(8) . ? O3 Co1 2.183(5) 2_455 ? O2 C1 1.229(8) . ? O2 Co1 2.076(5) 2_455 ? C4 C3 1.496(9) . ? C3 C2 1.372(9) . ? C2 C1 1.492(10) . ? N5 C5 1.322(9) . ? N5 N4 1.370(8) . ? N6 C5 1.340(9) . ? N6 C6 1.345(9) . ? N6 Co1 2.098(6) 2_545 ? N4 C6 1.319(9) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? O6 H6A 0.85(2) . ? O6 H6B 0.85(2) . ? O5 H5A 0.8992 . ? O5 H5B 0.8997 . ? 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 N5 Co1 O2 93.9(2) . 2_445 ? N5 Co1 N3 100.8(2) . . ? O2 Co1 N3 161.3(2) 2_445 . ? N5 Co1 N6 91.0(2) . 2 ? O2 Co1 N6 94.8(2) 2_445 2 ? N3 Co1 N6 96.4(2) . 2 ? N5 Co1 O4 178.0(2) . . ? O2 Co1 O4 88.02(19) 2_445 . ? N3 Co1 O4 77.2(2) . . ? N6 Co1 O4 89.5(2) 2 . ? N5 Co1 O3 84.5(2) . 2_445 ? O2 Co1 O3 88.63(19) 2_445 2_445 ? N3 Co1 O3 81.4(2) . 2_445 ? N6 Co1 O3 174.5(2) 2 2_445 ? O4 Co1 O3 94.9(2) . 2_445 ? O5 Co2 O1 88.8(2) . 3_576 ? O5 Co2 N4 94.9(2) . . ? O1 Co2 N4 87.3(2) 3_576 . ? O5 Co2 N2 90.1(2) . . ? O1 Co2 N2 168.2(2) 3_576 . ? N4 Co2 N2 104.6(2) . . ? O5 Co2 N1 96.6(2) . 3_576 ? O1 Co2 N1 77.1(2) 3_576 3_576 ? N4 Co2 N1 160.3(2) . 3_576 ? N2 Co2 N1 91.3(2) . 3_576 ? O5 Co2 O6 174.6(2) . . ? O1 Co2 O6 94.6(2) 3_576 . ? N4 Co2 O6 81.1(2) . . ? N2 Co2 O6 87.3(2) . . ? N1 Co2 O6 88.3(2) 3_576 . ? C4 O4 Co1 115.9(4) . . ? N1 N2 N3 109.4(5) . . ? N1 N2 Co2 128.8(4) . . ? N3 N2 Co2 121.6(4) . . ? N2 N3 C3 108.1(5) . . ? N2 N3 Co1 135.0(5) . . ? C3 N3 Co1 114.5(4) . . ? C1 O1 Co2 118.6(5) . 3_576 ? N2 N1 C2 108.2(5) . . ? N2 N1 Co2 139.7(4) . 3_576 ? C2 N1 Co2 111.3(4) . 3_576 ? C4 O3 Co1 132.8(4) . 2_455 ? C1 O2 Co1 134.2(5) . 2_455 ? O3 C4 O4 124.6(6) . . ? O3 C4 C3 120.0(6) . . ? O4 C4 C3 115.3(6) . . ? N3 C3 C2 107.7(6) . . ? N3 C3 C4 116.2(6) . . ? C2 C3 C4 135.7(6) . . ? N1 C2 C3 106.6(6) . . ? N1 C2 C1 117.7(6) . . ? C3 C2 C1 135.7(6) . . ? O2 C1 O1 123.7(7) . . ? O2 C1 C2 121.5(6) . . ? O1 C1 C2 114.9(6) . . ? C5 N5 N4 105.9(5) . . ? C5 N5 Co1 123.3(5) . . ? N4 N5 Co1 129.4(4) . . ? C5 N6 C6 102.2(6) . . ? C5 N6 Co1 120.1(5) . 2_545 ? C6 N6 Co1 135.3(5) . 2_545 ? C6 N4 N5 105.7(6) . . ? C6 N4 Co2 125.7(5) . . ? N5 N4 Co2 126.9(4) . . ? N5 C5 N6 113.0(6) . . ? N5 C5 H5 123.5 . . ? N6 C5 H5 123.5 . . ? N4 C6 N6 113.2(6) . . ? N4 C6 H6 123.4 . . ? N6 C6 H6 123.4 . . ? Co2 O6 H6A 116(5) . . ? Co2 O6 H6B 117(8) . . ? H6A O6 H6B 112(9) . . ? Co2 O5 H5A 112.5 . . ? Co2 O5 H5B 111.4 . . ? H5A O5 H5B 106.4 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.352 _refine_diff_density_min -0.540 _refine_diff_density_rms 0.155 _database_code_depnum_ccdc_archive 'CCDC 909523' ####################################################################### # # 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_p121126c #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H37.5 Co3 N12 O14.75' _chemical_formula_weight 1075.08 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4527(14) _cell_length_b 11.6239(9) _cell_length_c 11.7754(10) _cell_angle_alpha 64.825(8) _cell_angle_beta 81.406(9) _cell_angle_gamma 72.316(9) _cell_volume 1351.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2125 _cell_measurement_theta_min 3.0830 _cell_measurement_theta_max 29.0692 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 535 _exptl_absorpt_coefficient_mu 0.977 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.64593 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details CRYSALISPRO _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2116 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8802 _diffrn_reflns_av_R_equivalents 0.0762 _diffrn_reflns_av_sigmaI/netI 0.1233 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4747 _reflns_number_gt 3237 _reflns_threshold_expression >2sigma(I) _computing_data_collection CRYSALISPRO _computing_cell_refinement CRYSALISPRO _computing_data_reduction CRYSALISPRO _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^)+(0.1487P)^2^+0.1365P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4747 _refine_ls_number_parameters 351 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1183 _refine_ls_R_factor_gt 0.0866 _refine_ls_wR_factor_ref 0.2751 _refine_ls_wR_factor_gt 0.2442 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.0000 0.5000 0.5000 0.0227(4) Uani 1 2 d S . . Co2 Co 0.0000 1.0000 0.0000 0.0228(4) Uani 1 2 d S . . Co3 Co 0.0000 1.0000 0.5000 0.0228(4) Uani 1 2 d S . . O2 O -0.0490(5) 1.1039(4) 0.1166(4) 0.0297(12) Uani 1 1 d . . . O3 O -0.0446(5) 0.6344(4) 0.5860(4) 0.0282(12) Uani 1 1 d . . . O4 O -0.0794(5) 0.8451(4) 0.5509(4) 0.0320(12) Uani 1 1 d . . . N3 N 0.0044(5) 0.6751(5) 0.3477(5) 0.0237(13) Uani 1 1 d . . . N2 N 0.0241(5) 0.7158(5) 0.2251(5) 0.0255(13) Uani 1 1 d . . . O1 O -0.0462(5) 1.0779(4) 0.3129(4) 0.0345(13) Uani 1 1 d . . . N1 N 0.0100(5) 0.8461(5) 0.1756(5) 0.0231(13) Uani 1 1 d . . . C1 C -0.0386(6) 1.0326(6) 0.2323(6) 0.0237(15) Uani 1 1 d . . . C2 C -0.0192(6) 0.8893(6) 0.2698(6) 0.0228(15) Uani 1 1 d . . . C4 C -0.0489(6) 0.7521(6) 0.5142(6) 0.0237(15) Uani 1 1 d . . . C3 C -0.0209(6) 0.7798(6) 0.3797(6) 0.0229(15) Uani 1 1 d . . . N4 N -0.1965(5) 0.5447(5) 0.4788(6) 0.0289(14) Uani 1 1 d . . . N5 N 0.1891(6) 0.9971(6) 0.0095(5) 0.0333(15) Uani 1 1 d . . . N6 N 0.1733(5) 0.8765(5) 0.4718(5) 0.0279(13) Uani 1 1 d . . . C12 C 0.4358(7) 0.9989(7) 0.0024(6) 0.0336(17) Uani 1 1 d . . . C5 C -0.2516(7) 0.6155(7) 0.3687(7) 0.0369(19) Uani 1 1 d . . . H5 H -0.2042 0.6266 0.2953 0.044 Uiso 1 1 calc R . . C14 C 0.2212(8) 1.1046(8) -0.0050(8) 0.043(2) Uani 1 1 d . . . H14 H 0.1589 1.1806 -0.0133 0.052 Uiso 1 1 calc R . . C15 C 0.2499(7) 0.9192(7) 0.3742(7) 0.0361(19) Uani 1 1 d . . . H15 H 0.2212 1.0008 0.3088 0.043 Uiso 1 1 calc R . . C6 C -0.3751(7) 0.6725(8) 0.3597(8) 0.042(2) Uani 1 1 d . . . H6 H -0.4094 0.7223 0.2808 0.051 Uiso 1 1 calc R . . C7 C -0.4511(7) 0.6571(7) 0.4676(7) 0.0319(17) Uani 1 1 d . . . C8 C -0.3930(7) 0.5803(7) 0.5792(7) 0.041(2) Uani 1 1 d . . . H8 H -0.4384 0.5649 0.6541 0.050 Uiso 1 1 calc R . . C10 C 0.2815(8) 0.8901(8) 0.0246(9) 0.050(2) Uani 1 1 d . . . H10 H 0.2626 0.8126 0.0388 0.060 Uiso 1 1 calc R . . C16 C 0.3690(7) 0.8472(8) 0.3671(7) 0.0372(19) Uani 1 1 d . . . H16 H 0.4176 0.8794 0.2965 0.045 Uiso 1 1 calc R . . C11 C 0.4014(8) 0.8866(8) 0.0207(10) 0.055(3) Uani 1 1 d . . . H11 H 0.4614 0.8086 0.0302 0.066 Uiso 1 1 calc R . . C17 C 0.4163(7) 0.7287(7) 0.4631(7) 0.0326(17) Uani 1 1 d . . . C18 C 0.3361(7) 0.6812(7) 0.5610(7) 0.0340(18) Uani 1 1 d . . . H18 H 0.3616 0.5981 0.6255 0.041 Uiso 1 1 calc R . . C19 C 0.2197(7) 0.7577(7) 0.5613(7) 0.0341(18) Uani 1 1 d . . . H19 H 0.1684 0.7247 0.6290 0.041 Uiso 1 1 calc R . . C9 C -0.2691(8) 0.5259(8) 0.5821(7) 0.046(2) Uani 1 1 d . . . H9 H -0.2331 0.4729 0.6598 0.056 Uiso 1 1 calc R . . C13 C 0.3360(7) 1.1093(7) -0.0083(8) 0.041(2) Uani 1 1 d . . . H13 H 0.3509 1.1873 -0.0180 0.049 Uiso 1 1 calc R . . O5 O 0.5000 1.0000 0.5000 0.069(11) Uani 0.25 2 d SPU . . O11 O 0.626(2) 0.5684(13) 0.1338(14) 0.223(14) Uani 0.82(2) 1 d P A 2 O8 O 0.6183(17) 1.073(3) 0.343(3) 0.170(10) Uani 0.50 1 d PU . . O6 O 0.818(6) 0.573(5) 0.079(5) 0.12(3) Uani 0.18(2) 1 d PU A 1 O10 O 0.952(3) 0.680(3) 0.834(2) 0.084(11) Uani 0.25 1 d P . . O9 O 0.607(3) 0.819(3) 0.689(3) 0.120(14) Uani 0.36(2) 1 d PU . 2 O7 O 0.474(3) 0.776(3) 0.787(3) 0.270(18) Uani 0.64(2) 1 d PU . 1 O12 O 0.486(4) 1.086(3) 0.396(3) 0.210(13) Uani 0.50 1 d PU . . 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 0.0280(8) 0.0144(6) 0.0259(7) -0.0090(5) 0.0003(6) -0.0050(5) Co2 0.0296(8) 0.0236(7) 0.0178(7) -0.0078(5) -0.0006(5) -0.0114(6) Co3 0.0300(8) 0.0182(7) 0.0237(7) -0.0129(6) -0.0020(5) -0.0041(5) O2 0.049(3) 0.020(2) 0.020(2) -0.004(2) -0.002(2) -0.014(2) O3 0.046(3) 0.018(2) 0.021(2) -0.008(2) 0.002(2) -0.010(2) O4 0.046(3) 0.026(2) 0.032(3) -0.020(2) 0.005(2) -0.012(2) N3 0.036(4) 0.014(3) 0.024(3) -0.008(2) 0.001(2) -0.010(2) N2 0.036(4) 0.019(3) 0.026(3) -0.013(2) 0.001(3) -0.009(2) O1 0.056(4) 0.021(2) 0.029(3) -0.016(2) -0.007(2) -0.004(2) N1 0.031(3) 0.017(3) 0.023(3) -0.008(2) -0.001(2) -0.008(2) C1 0.028(4) 0.023(3) 0.027(4) -0.015(3) 0.001(3) -0.009(3) C2 0.027(4) 0.020(3) 0.021(3) -0.007(3) -0.001(3) -0.007(3) C4 0.030(4) 0.026(4) 0.021(3) -0.012(3) -0.004(3) -0.011(3) C3 0.026(4) 0.019(3) 0.022(3) -0.008(3) 0.001(3) -0.005(3) N4 0.025(3) 0.025(3) 0.037(3) -0.014(3) -0.002(3) -0.005(2) N5 0.036(4) 0.037(3) 0.031(3) -0.013(3) -0.005(3) -0.014(3) N6 0.029(4) 0.027(3) 0.030(3) -0.015(3) 0.000(3) -0.007(3) C12 0.035(4) 0.043(4) 0.027(4) -0.015(3) -0.002(3) -0.014(3) C5 0.029(4) 0.046(4) 0.037(4) -0.024(4) -0.002(3) 0.000(3) C14 0.035(5) 0.039(4) 0.061(5) -0.027(4) 0.003(4) -0.008(4) C15 0.040(5) 0.025(4) 0.037(4) -0.011(3) -0.004(4) 0.000(3) C6 0.037(5) 0.051(5) 0.036(4) -0.017(4) -0.005(4) -0.009(4) C7 0.028(4) 0.031(4) 0.038(4) -0.019(3) 0.002(3) -0.004(3) C8 0.032(5) 0.042(4) 0.037(4) -0.010(4) 0.006(4) -0.004(4) C10 0.039(5) 0.040(5) 0.082(7) -0.035(5) -0.002(5) -0.010(4) C16 0.030(4) 0.051(5) 0.033(4) -0.020(4) 0.002(3) -0.009(4) C11 0.028(5) 0.044(5) 0.105(8) -0.045(5) -0.004(5) -0.003(4) C17 0.033(4) 0.031(4) 0.040(4) -0.022(4) -0.003(3) -0.004(3) C18 0.036(5) 0.024(4) 0.043(4) -0.011(3) -0.008(4) -0.008(3) C19 0.031(4) 0.033(4) 0.038(4) -0.015(4) 0.005(3) -0.010(3) C9 0.036(5) 0.055(5) 0.033(4) -0.007(4) -0.002(4) -0.006(4) C13 0.038(5) 0.033(4) 0.056(5) -0.018(4) -0.001(4) -0.016(3) O5 0.069(11) 0.069(11) 0.069(11) -0.028(5) -0.002(2) -0.019(4) O11 0.46(4) 0.096(11) 0.112(13) -0.047(9) 0.007(15) -0.070(14) O8 0.041(11) 0.31(3) 0.28(2) -0.25(2) 0.042(13) -0.040(14) O6 0.17(4) 0.10(3) 0.13(4) -0.07(3) 0.02(3) -0.06(3) O10 0.19(3) 0.069(18) 0.018(12) -0.002(12) -0.005(15) -0.09(2) O9 0.122(14) 0.121(14) 0.123(14) -0.054(7) -0.004(4) -0.032(5) O7 0.273(18) 0.270(18) 0.269(18) -0.113(8) -0.004(4) -0.073(6) O12 0.29(2) 0.189(18) 0.26(2) -0.140(16) -0.044(17) -0.121(16) _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 N3 2.071(5) 2_566 ? Co1 N3 2.071(5) . ? Co1 O3 2.106(4) 2_566 ? Co1 O3 2.106(4) . ? Co1 N4 2.178(6) . ? Co1 N4 2.178(6) 2_566 ? Co2 N1 2.070(5) 2_575 ? Co2 N1 2.070(5) . ? Co2 O2 2.105(5) . ? Co2 O2 2.105(5) 2_575 ? Co2 N5 2.174(6) 2_575 ? Co2 N5 2.174(6) . ? Co3 O1 2.077(5) 2_576 ? Co3 O1 2.077(5) . ? Co3 O4 2.084(5) . ? Co3 O4 2.084(5) 2_576 ? Co3 N6 2.142(6) 2_576 ? Co3 N6 2.142(6) . ? O2 C1 1.259(8) . ? O3 C4 1.256(8) . ? O4 C4 1.265(8) . ? N3 N2 1.322(7) . ? N3 C3 1.360(8) . ? N2 N1 1.338(7) . ? O1 C1 1.249(8) . ? N1 C2 1.363(8) . ? C1 C2 1.482(8) . ? C2 C3 1.380(9) . ? C4 C3 1.480(9) . ? N4 C5 1.333(9) . ? N4 C9 1.343(10) . ? N5 C10 1.329(10) . ? N5 C14 1.343(10) . ? N6 C19 1.336(9) . ? N6 C15 1.346(10) . ? C12 C11 1.398(11) . ? C12 C13 1.408(10) . ? C12 C12 1.471(15) 2_675 ? C5 C6 1.366(11) . ? C5 H5 0.9300 . ? C14 C13 1.326(11) . ? C14 H14 0.9300 . ? C15 C16 1.379(10) . ? C15 H15 0.9300 . ? C6 C7 1.406(11) . ? C6 H6 0.9300 . ? C7 C8 1.368(10) . ? C7 C17 1.489(10) 1_455 ? C8 C9 1.366(11) . ? C8 H8 0.9300 . ? C10 C11 1.356(12) . ? C10 H10 0.9300 . ? C16 C17 1.369(10) . ? C16 H16 0.9300 . ? C11 H11 0.9300 . ? C17 C18 1.389(10) . ? C17 C7 1.489(10) 1_655 ? C18 C19 1.359(10) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C9 H9 0.9300 . ? C13 H13 0.9300 . ? O5 O12 1.20(3) 2_676 ? O5 O12 1.20(3) . ? O8 O12 1.54(4) . ? O9 O12 1.42(4) 2_676 ? O12 O9 1.42(4) 2_676 ? 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 N3 Co1 N3 180.000(2) 2_566 . ? N3 Co1 O3 78.41(19) 2_566 2_566 ? N3 Co1 O3 101.59(19) . 2_566 ? N3 Co1 O3 101.59(19) 2_566 . ? N3 Co1 O3 78.41(19) . . ? O3 Co1 O3 180.0(3) 2_566 . ? N3 Co1 N4 90.0(2) 2_566 . ? N3 Co1 N4 90.0(2) . . ? O3 Co1 N4 93.7(2) 2_566 . ? O3 Co1 N4 86.3(2) . . ? N3 Co1 N4 90.0(2) 2_566 2_566 ? N3 Co1 N4 90.0(2) . 2_566 ? O3 Co1 N4 86.3(2) 2_566 2_566 ? O3 Co1 N4 93.7(2) . 2_566 ? N4 Co1 N4 179.999(2) . 2_566 ? N1 Co2 N1 179.998(1) 2_575 . ? N1 Co2 O2 100.95(18) 2_575 . ? N1 Co2 O2 79.05(18) . . ? N1 Co2 O2 79.05(18) 2_575 2_575 ? N1 Co2 O2 100.95(18) . 2_575 ? O2 Co2 O2 180.0 . 2_575 ? N1 Co2 N5 91.0(2) 2_575 2_575 ? N1 Co2 N5 89.0(2) . 2_575 ? O2 Co2 N5 92.1(2) . 2_575 ? O2 Co2 N5 87.9(2) 2_575 2_575 ? N1 Co2 N5 89.0(2) 2_575 . ? N1 Co2 N5 91.0(2) . . ? O2 Co2 N5 87.9(2) . . ? O2 Co2 N5 92.1(2) 2_575 . ? N5 Co2 N5 180.0 2_575 . ? O1 Co3 O1 179.999(1) 2_576 . ? O1 Co3 O4 86.53(19) 2_576 . ? O1 Co3 O4 93.47(19) . . ? O1 Co3 O4 93.47(19) 2_576 2_576 ? O1 Co3 O4 86.53(19) . 2_576 ? O4 Co3 O4 179.999(1) . 2_576 ? O1 Co3 N6 93.2(2) 2_576 2_576 ? O1 Co3 N6 86.8(2) . 2_576 ? O4 Co3 N6 90.0(2) . 2_576 ? O4 Co3 N6 90.0(2) 2_576 2_576 ? O1 Co3 N6 86.8(2) 2_576 . ? O1 Co3 N6 93.2(2) . . ? O4 Co3 N6 90.0(2) . . ? O4 Co3 N6 90.0(2) 2_576 . ? N6 Co3 N6 179.999(1) 2_576 . ? C1 O2 Co2 114.8(4) . . ? C4 O3 Co1 115.9(4) . . ? C4 O4 Co3 128.0(5) . . ? N2 N3 C3 109.1(5) . . ? N2 N3 Co1 137.8(4) . . ? C3 N3 Co1 113.1(4) . . ? N3 N2 N1 108.8(5) . . ? C1 O1 Co3 135.5(4) . . ? N2 N1 C2 108.6(5) . . ? N2 N1 Co2 138.6(4) . . ? C2 N1 Co2 112.3(4) . . ? O1 C1 O2 123.0(6) . . ? O1 C1 C2 120.7(6) . . ? O2 C1 C2 116.3(6) . . ? N1 C2 C3 106.6(5) . . ? N1 C2 C1 116.3(5) . . ? C3 C2 C1 137.1(6) . . ? O3 C4 O4 123.3(6) . . ? O3 C4 C3 116.4(6) . . ? O4 C4 C3 120.3(6) . . ? N3 C3 C2 106.8(6) . . ? N3 C3 C4 116.2(5) . . ? C2 C3 C4 136.9(6) . . ? C5 N4 C9 116.8(7) . . ? C5 N4 Co1 123.3(5) . . ? C9 N4 Co1 118.3(5) . . ? C10 N5 C14 115.4(7) . . ? C10 N5 Co2 122.2(5) . . ? C14 N5 Co2 122.4(5) . . ? C19 N6 C15 115.5(6) . . ? C19 N6 Co3 120.7(5) . . ? C15 N6 Co3 123.1(5) . . ? C11 C12 C13 113.8(7) . . ? C11 C12 C12 123.2(9) . 2_675 ? C13 C12 C12 123.0(9) . 2_675 ? N4 C5 C6 122.4(7) . . ? N4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C13 C14 N5 124.3(7) . . ? C13 C14 H14 117.9 . . ? N5 C14 H14 117.9 . . ? N6 C15 C16 122.8(7) . . ? N6 C15 H15 118.6 . . ? C16 C15 H15 118.6 . . ? C5 C6 C7 121.1(7) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C8 C7 C6 115.3(7) . . ? C8 C7 C17 121.4(7) . 1_455 ? C6 C7 C17 123.0(7) . 1_455 ? C9 C8 C7 120.8(7) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? N5 C10 C11 124.2(8) . . ? N5 C10 H10 117.9 . . ? C11 C10 H10 117.9 . . ? C17 C16 C15 120.6(7) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C10 C11 C12 120.7(8) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C16 C17 C18 116.8(7) . . ? C16 C17 C7 122.2(7) . 1_655 ? C18 C17 C7 120.9(7) . 1_655 ? C19 C18 C17 119.1(7) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? N6 C19 C18 125.1(7) . . ? N6 C19 H19 117.5 . . ? C18 C19 H19 117.5 . . ? N4 C9 C8 123.5(7) . . ? N4 C9 H9 118.3 . . ? C8 C9 H9 118.3 . . ? C14 C13 C12 121.5(7) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? O12 O5 O12 180(4) 2_676 . ? O5 O12 O9 142(4) . 2_676 ? O5 O12 O8 102(3) . . ? O9 O12 O8 116(3) 2_676 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.292 _refine_diff_density_min -0.780 _refine_diff_density_rms 0.191 # 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 -0.011 0.500 0.000 256 32 ' ' 2 0.311 0.036 0.685 32 4 ' ' 3 0.689 0.964 0.315 32 4 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 928525'