# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email zwang3@ustc.edu.cn _publ_contact_author_name 'Zhiyong Wang' loop_ _publ_author_name 'Zhiyong Wang' 'Shunshun Xiong' 'Shujuan Li' 'Sujing Wang' data_x0505 _database_code_depnum_ccdc_archive 'CCDC 786180' #TrackingRef 'compound 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H8 In N0 O8' _chemical_formula_weight 455.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' 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' In In 0.0822 5.0449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 17.379(5) _cell_length_b 9.906(5) _cell_length_c 22.043(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 3795(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rodlike _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.796 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 5.161 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2976 _exptl_absorpt_correction_T_max 0.5319 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _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 12091 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 62.80 _reflns_number_total 3165 _reflns_number_gt 2051 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.1100P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3165 _refine_ls_number_parameters 145 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.1812 _refine_ls_wR_factor_gt 0.1774 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 In1 In 0.41531(4) 0.2500 0.67182(2) 0.0660(3) Uani 1 2 d S . . O2 O 0.8984(4) 0.2500 0.7260(2) 0.0747(19) Uani 1 2 d S . . O6 O 0.5810(2) 0.5123(6) 0.31953(18) 0.0772(13) Uani 1 1 d U . . O4 O 0.5177(3) 0.2500 0.6017(2) 0.0785(19) Uani 1 2 d S . . O3 O 0.5361(3) 0.2500 0.6997(2) 0.0653(16) Uani 1 2 d S . . O1 O 0.7985(3) 0.2500 0.7847(3) 0.079(2) Uani 1 2 d S . . O5 O 0.6394(3) 0.6107(5) 0.39472(19) 0.0798(14) Uani 1 1 d . . . C10 C 0.6491(4) 0.3727(7) 0.3872(2) 0.0610(15) Uani 1 1 d U . . C2 C 0.6464(5) 0.2500 0.6368(3) 0.064(2) Uani 1 2 d S . . C4 C 0.7561(5) 0.2500 0.5691(4) 0.063(2) Uani 1 2 d S . . C7 C 0.7727(5) 0.2500 0.6786(4) 0.066(2) Uani 1 2 d S . . C9 C 0.6216(4) 0.5029(8) 0.3663(3) 0.0668(16) Uani 1 1 d U . . C1 C 0.5618(5) 0.2500 0.6462(4) 0.065(2) Uani 1 2 d S . . C11 C 0.6231(6) 0.2500 0.3652(4) 0.058(2) Uani 1 2 d S . . C3 C 0.6791(5) 0.2500 0.5780(4) 0.069(3) Uani 1 2 d S . . H3 H 0.6460 0.2500 0.5437 0.082 Uiso 1 2 calc SR . . C6 C 0.8265(5) 0.2500 0.7325(3) 0.069(3) Uani 1 2 d S . . C8 C 0.8045(6) 0.2500 0.6203(4) 0.069(3) Uani 1 2 d S . . H8 H 0.8588 0.2500 0.6153 0.083 Uiso 1 2 calc SR . . C5 C 0.6969(6) 0.2500 0.6868(4) 0.078(3) Uani 1 2 d S . . H5 H 0.6766 0.2500 0.7268 0.094 Uiso 1 2 calc SR . . C12 C 0.7058(4) 0.3714(6) 0.4335(2) 0.0600(16) Uani 1 1 d . . . H12 H 0.7253 0.4537 0.4494 0.072 Uiso 1 1 calc R . . C13 C 0.7321(5) 0.2500 0.4551(4) 0.061(2) Uani 1 2 d S . . C16 C 0.7924(6) 0.2500 0.5069(4) 0.081(3) Uani 1 2 d S . . H16A H 0.8255 0.1692 0.5028 0.097 Uiso 0.50 1 calc PR . . H16B H 0.8255 0.3308 0.5028 0.097 Uiso 0.50 1 calc PR . . H11 H 0.582(5) 0.2500 0.329(4) 0.07(3) Uiso 1 2 d S . . 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 In1 0.0583(4) 0.1064(6) 0.0332(3) 0.000 -0.0010(3) 0.000 O2 0.061(5) 0.125(6) 0.038(3) 0.000 -0.003(3) 0.000 O6 0.059(3) 0.125(4) 0.048(2) 0.008(2) -0.0014(17) 0.002(2) O4 0.055(4) 0.139(6) 0.041(3) 0.000 -0.002(3) 0.000 O3 0.053(4) 0.098(5) 0.044(3) 0.000 0.000(3) 0.000 O1 0.050(4) 0.145(6) 0.042(3) 0.000 -0.001(3) 0.000 O5 0.088(4) 0.100(4) 0.052(2) 0.000(3) 0.003(2) 0.005(3) C10 0.065(4) 0.077(4) 0.042(3) 0.001(3) 0.016(3) 0.000(3) C2 0.052(5) 0.100(7) 0.040(4) 0.000 -0.004(4) 0.000 C4 0.057(6) 0.086(7) 0.045(4) 0.000 0.002(4) 0.000 C7 0.055(6) 0.098(7) 0.044(5) 0.000 0.001(4) 0.000 C9 0.064(4) 0.093(4) 0.043(3) 0.007(3) 0.003(2) 0.011(4) C1 0.065(6) 0.079(7) 0.051(5) 0.000 0.000(5) 0.000 C11 0.068(6) 0.056(6) 0.049(5) 0.000 0.014(4) 0.000 C3 0.063(6) 0.105(8) 0.037(4) 0.000 -0.002(4) 0.000 C6 0.059(6) 0.116(8) 0.031(4) 0.000 -0.010(4) 0.000 C8 0.067(6) 0.099(8) 0.042(4) 0.000 -0.002(4) 0.000 C5 0.082(8) 0.121(9) 0.031(4) 0.000 0.000(4) 0.000 C12 0.072(4) 0.066(4) 0.043(3) -0.007(3) 0.007(3) -0.010(3) C13 0.072(6) 0.066(6) 0.046(4) 0.000 0.011(4) 0.000 C16 0.065(6) 0.139(9) 0.037(4) 0.000 -0.005(4) 0.000 _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 In1 O3 2.186(6) . ? In1 O5 2.227(5) 4_646 ? In1 O5 2.227(5) 5_666 ? In1 O1 2.245(6) 6_557 ? In1 O2 2.272(6) 6_557 ? In1 O6 2.364(6) 5_666 ? In1 O6 2.364(6) 4_646 ? In1 O4 2.358(6) . ? In1 C1 2.607(9) . ? In1 C6 2.614(8) 6_557 ? In1 C9 2.666(7) 4_646 ? In1 C9 2.666(7) 5_666 ? O2 C6 1.258(10) . ? O2 In1 2.272(5) 6_657 ? O6 C9 1.252(7) . ? O6 In1 2.364(6) 5_666 ? O4 C1 1.246(10) . ? O3 C1 1.260(10) . ? O1 C6 1.250(10) . ? O1 In1 2.245(6) 6_657 ? O5 C9 1.276(8) . ? O5 In1 2.227(5) 5_666 ? C10 C11 1.384(8) . ? C10 C12 1.420(8) . ? C10 C9 1.450(9) . ? C2 C5 1.408(12) . ? C2 C3 1.417(11) . ? C2 C1 1.485(13) . ? C4 C3 1.352(12) . ? C4 C8 1.409(12) . ? C4 C16 1.509(12) . ? C7 C5 1.329(14) . ? C7 C8 1.398(11) . ? C7 C6 1.511(11) . ? C9 In1 2.666(7) 5_666 ? C11 C10 1.384(8) 8_565 ? C6 In1 2.614(8) 6_657 ? C12 C13 1.372(7) . ? C13 C12 1.372(7) 8_565 ? C13 C16 1.549(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 In1 O5 126.49(16) . 4_646 ? O3 In1 O5 126.49(16) . 5_666 ? O5 In1 O5 76.6(3) 4_646 5_666 ? O3 In1 O1 138.4(2) . 6_557 ? O5 In1 O1 83.97(17) 4_646 6_557 ? O5 In1 O1 83.97(17) 5_666 6_557 ? O3 In1 O2 81.1(2) . 6_557 ? O5 In1 O2 126.71(16) 4_646 6_557 ? O5 In1 O2 126.71(16) 5_666 6_557 ? O1 In1 O2 57.3(2) 6_557 6_557 ? O3 In1 O6 87.20(10) . 5_666 ? O5 In1 O6 133.02(17) 4_646 5_666 ? O5 In1 O6 56.45(17) 5_666 5_666 ? O1 In1 O6 89.45(10) 6_557 5_666 ? O2 In1 O6 85.62(10) 6_557 5_666 ? O3 In1 O6 87.20(10) . 4_646 ? O5 In1 O6 56.45(17) 4_646 4_646 ? O5 In1 O6 133.02(17) 5_666 4_646 ? O1 In1 O6 89.45(10) 6_557 4_646 ? O2 In1 O6 85.62(10) 6_557 4_646 ? O6 In1 O6 170.23(19) 5_666 4_646 ? O3 In1 O4 57.29(19) . . ? O5 In1 O4 83.71(16) 4_646 . ? O5 In1 O4 83.71(16) 5_666 . ? O1 In1 O4 164.3(2) 6_557 . ? O2 In1 O4 138.4(2) 6_557 . ? O6 In1 O4 91.85(10) 5_666 . ? O6 In1 O4 91.85(10) 4_646 . ? O3 In1 C1 28.8(2) . . ? O5 In1 C1 105.9(2) 4_646 . ? O5 In1 C1 105.9(2) 5_666 . ? O1 In1 C1 167.2(2) 6_557 . ? O2 In1 C1 109.9(3) 6_557 . ? O6 In1 C1 89.47(10) 5_666 . ? O6 In1 C1 89.47(10) 4_646 . ? O4 In1 C1 28.5(2) . . ? O3 In1 C6 109.9(3) . 6_557 ? O5 In1 C6 106.2(2) 4_646 6_557 ? O5 In1 C6 106.2(2) 5_666 6_557 ? O1 In1 C6 28.6(2) 6_557 6_557 ? O2 In1 C6 28.8(2) 6_557 6_557 ? O6 In1 C6 87.20(10) 5_666 6_557 ? O6 In1 C6 87.20(10) 4_646 6_557 ? O4 In1 C6 167.2(2) . 6_557 ? C1 In1 C6 138.7(3) . 6_557 ? O3 In1 C9 108.61(16) . 4_646 ? O5 In1 C9 28.47(17) 4_646 4_646 ? O5 In1 C9 105.0(2) 5_666 4_646 ? O1 In1 C9 85.24(15) 6_557 4_646 ? O2 In1 C9 106.33(14) 6_557 4_646 ? O6 In1 C9 161.22(19) 5_666 4_646 ? O6 In1 C9 28.01(17) 4_646 4_646 ? O4 In1 C9 88.56(14) . 4_646 ? C1 In1 C9 99.59(16) . 4_646 ? C6 In1 C9 96.45(15) 6_557 4_646 ? O3 In1 C9 108.61(16) . 5_666 ? O5 In1 C9 105.0(2) 4_646 5_666 ? O5 In1 C9 28.47(17) 5_666 5_666 ? O1 In1 C9 85.24(15) 6_557 5_666 ? O2 In1 C9 106.33(14) 6_557 5_666 ? O6 In1 C9 28.01(17) 5_666 5_666 ? O6 In1 C9 161.22(19) 4_646 5_666 ? O4 In1 C9 88.56(14) . 5_666 ? C1 In1 C9 99.59(16) . 5_666 ? C6 In1 C9 96.45(15) 6_557 5_666 ? C9 In1 C9 133.3(3) 4_646 5_666 ? C6 O2 In1 90.9(5) . 6_657 ? C9 O6 In1 89.6(4) . 5_666 ? C1 O4 In1 86.9(5) . . ? C1 O3 In1 94.5(5) . . ? C6 O1 In1 92.3(5) . 6_657 ? C9 O5 In1 95.2(4) . 5_666 ? C11 C10 C12 118.1(7) . . ? C11 C10 C9 124.2(6) . . ? C12 C10 C9 117.7(6) . . ? C5 C2 C3 117.8(9) . . ? C5 C2 C1 120.6(8) . . ? C3 C2 C1 121.7(8) . . ? C3 C4 C8 118.3(8) . . ? C3 C4 C16 123.1(8) . . ? C8 C4 C16 118.6(8) . . ? C5 C7 C8 121.1(8) . . ? C5 C7 C6 120.4(8) . . ? C8 C7 C6 118.5(8) . . ? O6 C9 O5 118.6(6) . . ? O6 C9 C10 120.9(7) . . ? O5 C9 C10 120.5(6) . . ? O6 C9 In1 62.4(4) . 5_666 ? O5 C9 In1 56.3(3) . 5_666 ? C10 C9 In1 174.6(5) . 5_666 ? O4 C1 O3 121.3(8) . . ? O4 C1 C2 119.9(8) . . ? O3 C1 C2 118.8(8) . . ? O4 C1 In1 64.6(5) . . ? O3 C1 In1 56.7(4) . . ? C2 C1 In1 175.5(6) . . ? C10 C11 C10 122.8(9) . 8_565 ? C4 C3 C2 122.0(8) . . ? O1 C6 O2 119.5(8) . . ? O1 C6 C7 118.9(8) . . ? O2 C6 C7 121.7(7) . . ? O1 C6 In1 59.1(4) . 6_657 ? O2 C6 In1 60.4(4) . 6_657 ? C7 C6 In1 178.0(6) . 6_657 ? C7 C8 C4 120.0(9) . . ? C7 C5 C2 120.8(8) . . ? C13 C12 C10 119.3(6) . . ? C12 C13 C12 122.5(9) 8_565 . ? C12 C13 C16 118.7(4) 8_565 . ? C12 C13 C16 118.7(4) . . ? C4 C16 C13 112.7(8) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 62.80 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 2.922 _refine_diff_density_min -0.880 _refine_diff_density_rms 0.100 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 0.006 -0.017 -0.018 2604 779 ' ' _platon_squeeze_details ; ; # Attachment 'compound 3.cif' data_x0509 _database_code_depnum_ccdc_archive 'CCDC 786181' #TrackingRef 'compound 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H24 Co2 N4 O8' _chemical_formula_weight 770.46 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' 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' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 26.6496(5) _cell_length_b 11.4204(2) _cell_length_c 17.5511(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5341.66(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.958 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 5.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2568 _exptl_absorpt_correction_T_max 0.4235 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _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 15032 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 62.75 _reflns_number_total 7101 _reflns_number_gt 5036 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0230P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.406(5) _refine_ls_number_reflns 7101 _refine_ls_number_parameters 461 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0756 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 0.35677(3) 0.05918(5) 0.26425(4) 0.02378(17) Uani 1 1 d . . . Co2 Co 0.39322(3) -0.01807(5) 0.48374(4) 0.02457(17) Uani 1 1 d . . . O6 O -0.05158(12) 0.0297(3) 0.4047(2) 0.0343(8) Uani 1 1 d . . . O1 O 0.20092(15) 0.0558(3) 0.6718(2) 0.0406(10) Uani 1 1 d . . . O4 O 0.32025(11) -0.0181(2) 0.45539(18) 0.0328(8) Uani 1 1 d . . . O3 O 0.30247(13) 0.0657(2) 0.3439(2) 0.0339(9) Uani 1 1 d . . . O5 O -0.06995(11) -0.0573(2) 0.29475(18) 0.0324(8) Uani 1 1 d . . . N2 N 0.35703(14) 0.8699(3) 0.2636(3) 0.0332(8) Uani 1 1 d . . . O2 O 0.12192(13) 0.0723(3) 0.6432(2) 0.0381(9) Uani 1 1 d . . . N1 N 0.35815(14) 0.2481(3) 0.2670(3) 0.0335(9) Uani 1 1 d . . . O7 O 0.12790(13) -0.0069(3) 0.1051(2) 0.0418(9) Uani 1 1 d . . . C7 C 0.02255(16) -0.0028(4) 0.2335(3) 0.0321(12) Uani 1 1 d . . . H7 H 0.0005 -0.0475 0.2045 0.038 Uiso 1 1 calc R . . O8 O 0.04876(14) -0.0140(3) 0.0736(2) 0.0410(10) Uani 1 1 d . . . C2 C 0.00915(16) 0.0320(4) 0.3083(3) 0.0290(11) Uani 1 1 d . . . C12 C 0.24004(17) 0.0683(3) 0.4394(3) 0.0242(10) Uani 1 1 d U . . C4 C 0.08816(15) 0.1383(3) 0.3193(2) 0.0282(10) Uani 1 1 d . . . C13 C 0.22757(17) 0.0530(4) 0.5134(3) 0.0337(12) Uani 1 1 d U . . H13 H 0.2508 0.0193 0.5464 0.040 Uiso 1 1 calc R . . C30 C 0.3906(2) 0.5485(3) 0.4816(5) 0.0370(13) Uani 1 1 d . . . C35 C 0.39052(19) 0.4181(3) 0.4838(4) 0.0357(12) Uani 1 1 d . . . C16 C 0.29148(17) 0.0365(4) 0.4112(3) 0.0269(11) Uani 1 1 d . . . N4 N 0.39290(15) 0.1730(3) 0.4817(3) 0.0325(9) Uani 1 1 d . . . C17 C 0.1668(2) 0.0698(4) 0.6231(3) 0.0308(12) Uani 1 1 d . . . N3 N 0.39309(14) 0.7944(3) 0.4858(3) 0.0325(8) Uani 1 1 d . . . C3 C 0.04178(14) 0.1008(3) 0.3495(2) 0.0279(10) Uani 1 1 d . . . H3 H 0.0330 0.1232 0.3986 0.033 Uiso 1 1 calc R . . C5 C 0.10104(15) 0.0997(4) 0.2476(2) 0.0311(11) Uani 1 1 d . . . H5 H 0.1321 0.1204 0.2276 0.037 Uiso 1 1 calc R . . C9 C 0.12185(15) 0.2192(4) 0.3639(3) 0.0332(11) Uani 1 1 d . . . H9A H 0.1010 0.2706 0.3945 0.040 Uiso 1 1 calc R . . H9B H 0.1403 0.2679 0.3283 0.040 Uiso 1 1 calc R . . C1 C -0.04183(17) 0.0000(3) 0.3381(3) 0.0237(11) Uani 1 1 d . . . C25 C 0.35851(19) 0.6254(4) 0.2630(4) 0.0409(11) Uani 1 1 d . . . C29 C 0.4310(2) 0.6140(4) 0.4607(5) 0.078(3) Uani 1 1 d . . . H29 H 0.4598 0.5767 0.4430 0.093 Uiso 1 1 calc R . . C11 C 0.20628(14) 0.1220(4) 0.3917(3) 0.0297(10) Uani 1 1 d . . . H11 H 0.2153 0.1341 0.3411 0.036 Uiso 1 1 calc R . . C6 C 0.06852(17) 0.0299(4) 0.2038(3) 0.0320(12) Uani 1 1 d . . . C20 C 0.3580(2) 0.4933(3) 0.2672(4) 0.0338(14) Uani 1 1 d . . . C22 C 0.3962(2) 0.3071(4) 0.2439(4) 0.0500(17) Uani 1 1 d . . . H22 H 0.4247 0.2660 0.2289 0.060 Uiso 1 1 calc R . . C23 C 0.3923(2) 0.8114(4) 0.2280(4) 0.065(2) Uani 1 1 d . . . H23 H 0.4168 0.8528 0.2015 0.078 Uiso 1 1 calc R . . C8 C 0.0822(2) -0.0010(3) 0.1241(3) 0.0307(13) Uani 1 1 d . . . C15 C 0.14721(15) 0.1353(3) 0.4920(3) 0.0324(10) Uani 1 1 d . . . H15 H 0.1152 0.1536 0.5094 0.039 Uiso 1 1 calc R . . C26 C 0.3208(2) 0.6886(4) 0.2987(4) 0.059(2) Uani 1 1 d . . . H26 H 0.2954 0.6489 0.3243 0.070 Uiso 1 1 calc R . . C14 C 0.18035(17) 0.0867(4) 0.5417(3) 0.0278(11) Uani 1 1 d . . . C10 C 0.15912(14) 0.1589(3) 0.4159(2) 0.0252(10) Uani 1 1 d . . . C24 C 0.3944(3) 0.6862(5) 0.2283(4) 0.064(2) Uani 1 1 d . . . H24 H 0.4208 0.6475 0.2044 0.077 Uiso 1 1 calc R . . C36 C 0.4293(2) 0.3551(4) 0.4455(4) 0.0448(15) Uani 1 1 d . . . H36 H 0.4550 0.3937 0.4199 0.054 Uiso 1 1 calc R . . C21 C 0.3975(2) 0.4291(4) 0.2398(4) 0.067(2) Uani 1 1 d . . . H21 H 0.4251 0.4667 0.2186 0.080 Uiso 1 1 calc R . . C19 C 0.3203(2) 0.4325(4) 0.2951(4) 0.070(2) Uani 1 1 d . . . H19 H 0.2930 0.4719 0.3161 0.084 Uiso 1 1 calc R . . C18 C 0.3203(2) 0.3121(4) 0.2941(4) 0.0548(19) Uani 1 1 d . . . H18 H 0.2924 0.2731 0.3133 0.066 Uiso 1 1 calc R . . C27 C 0.32042(19) 0.8090(4) 0.2969(3) 0.0485(15) Uani 1 1 d . . . H27 H 0.2939 0.8490 0.3194 0.058 Uiso 1 1 calc R . . C34 C 0.3542(2) 0.3512(4) 0.5192(4) 0.0530(18) Uani 1 1 d . . . H34 H 0.3275 0.3872 0.5440 0.064 Uiso 1 1 calc R . . C31 C 0.3500(2) 0.6118(4) 0.5023(5) 0.078(3) Uani 1 1 d . . . H31 H 0.3201 0.5737 0.5137 0.093 Uiso 1 1 calc R . . C28 C 0.4301(2) 0.7326(4) 0.4653(4) 0.065(2) Uani 1 1 d . . . H28 H 0.4594 0.7720 0.4522 0.079 Uiso 1 1 calc R . . C32 C 0.3524(2) 0.7335(4) 0.5067(4) 0.068(2) Uani 1 1 d . . . H32 H 0.3246 0.7741 0.5249 0.082 Uiso 1 1 calc R . . C37 C 0.4272(2) 0.2357(4) 0.4481(3) 0.0472(16) Uani 1 1 d . . . H37 H 0.4527 0.1952 0.4234 0.057 Uiso 1 1 calc R . . C33 C 0.3577(2) 0.2339(4) 0.5176(3) 0.0438(15) Uani 1 1 d . . . H33 H 0.3333 0.1918 0.5439 0.053 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 0.0223(4) 0.0289(4) 0.0201(4) 0.0006(3) 0.0003(4) 0.0018(3) Co2 0.0231(4) 0.0283(4) 0.0223(4) 0.0000(4) 0.0007(4) 0.0016(3) O6 0.029(2) 0.0415(18) 0.032(2) 0.0021(15) 0.0038(17) -0.0024(14) O1 0.037(3) 0.058(2) 0.026(3) 0.0068(15) 0.002(2) 0.0018(15) O4 0.0230(18) 0.0368(18) 0.039(2) 0.0056(14) -0.0028(16) 0.0021(13) O3 0.032(2) 0.0413(19) 0.028(2) 0.0049(15) 0.0081(17) 0.0003(14) O5 0.0235(17) 0.0444(19) 0.029(2) 0.0032(15) -0.0022(16) -0.0108(14) N2 0.036(2) 0.035(2) 0.029(2) 0.003(2) -0.006(2) 0.000(2) O2 0.032(2) 0.058(2) 0.025(2) 0.0007(15) 0.0077(18) -0.0019(16) N1 0.033(2) 0.033(2) 0.034(2) 0.006(2) -0.005(2) 0.0002(19) O7 0.037(2) 0.059(2) 0.029(2) -0.0026(15) 0.0080(18) -0.0041(15) C7 0.024(3) 0.053(3) 0.019(3) -0.0038(19) 0.001(2) -0.011(2) O8 0.033(3) 0.066(3) 0.024(3) -0.0052(16) 0.000(2) -0.0013(16) C2 0.021(2) 0.042(3) 0.023(3) -0.006(2) 0.000(2) -0.006(2) C12 0.020(2) 0.029(2) 0.023(2) -0.0022(19) 0.002(2) -0.0027(19) C4 0.022(2) 0.027(2) 0.036(3) 0.009(2) -0.004(2) -0.0023(18) C13 0.035(3) 0.042(3) 0.024(2) -0.0003(19) 0.003(2) 0.005(2) C30 0.037(3) 0.026(3) 0.048(4) 0.000(3) 0.002(3) -0.001(2) C35 0.033(3) 0.027(2) 0.047(3) -0.001(3) 0.001(3) -0.007(2) C16 0.026(3) 0.031(3) 0.024(3) -0.001(2) -0.002(2) -0.0036(19) N4 0.038(2) 0.0251(19) 0.035(2) -0.003(2) 0.009(2) -0.0011(18) C17 0.036(3) 0.035(3) 0.021(3) -0.005(2) -0.002(3) 0.001(2) N3 0.033(2) 0.0223(18) 0.042(2) 0.001(2) 0.008(2) 0.0004(18) C3 0.024(2) 0.041(3) 0.018(2) -0.0029(18) 0.0066(19) 0.0018(19) C5 0.020(2) 0.053(3) 0.020(3) 0.0014(19) 0.003(2) -0.0060(19) C9 0.025(2) 0.040(3) 0.034(3) 0.008(2) 0.000(2) 0.0026(18) C1 0.027(3) 0.028(3) 0.016(3) 0.0046(18) 0.000(2) -0.0053(19) C25 0.047(3) 0.033(3) 0.043(3) 0.009(3) -0.003(3) -0.004(3) C29 0.049(4) 0.025(3) 0.159(8) 0.012(4) 0.034(4) 0.008(2) C11 0.021(2) 0.048(3) 0.020(2) -0.004(2) 0.0068(19) -0.0058(19) C6 0.027(3) 0.048(3) 0.021(3) 0.000(2) 0.004(2) 0.009(2) C20 0.038(4) 0.028(3) 0.036(4) -0.006(3) -0.002(4) 0.005(2) C22 0.042(4) 0.031(3) 0.077(5) -0.007(3) 0.011(4) 0.013(2) C23 0.065(4) 0.033(3) 0.096(6) 0.002(3) 0.026(4) 0.016(3) C8 0.032(3) 0.030(3) 0.030(3) -0.0001(19) 0.015(3) -0.002(2) C15 0.019(2) 0.041(3) 0.037(3) -0.006(2) 0.013(3) -0.0007(18) C26 0.061(4) 0.033(3) 0.082(5) 0.009(3) 0.042(4) -0.006(3) C14 0.020(3) 0.038(3) 0.025(3) 0.004(2) -0.002(2) -0.002(2) C10 0.021(2) 0.031(2) 0.024(3) -0.0048(19) -0.0013(19) 0.0001(17) C24 0.066(5) 0.038(3) 0.090(6) -0.003(3) 0.035(4) -0.003(3) C36 0.041(3) 0.031(3) 0.063(4) -0.004(2) 0.019(3) 0.000(2) C21 0.068(4) 0.030(3) 0.102(6) 0.003(3) 0.038(4) -0.001(3) C19 0.061(4) 0.033(3) 0.118(6) 0.004(3) 0.040(4) 0.009(3) C18 0.038(4) 0.036(3) 0.090(5) 0.006(3) 0.032(4) 0.003(2) C27 0.049(3) 0.027(3) 0.070(4) -0.004(3) 0.029(3) 0.004(2) C34 0.047(4) 0.030(3) 0.082(5) 0.010(3) 0.035(3) 0.017(2) C31 0.044(4) 0.029(3) 0.160(8) 0.020(4) 0.049(5) -0.002(2) C28 0.037(4) 0.032(3) 0.127(7) 0.017(3) 0.014(4) 0.001(2) C32 0.052(4) 0.039(3) 0.114(7) 0.006(3) 0.047(4) 0.003(3) C37 0.057(4) 0.038(3) 0.047(4) -0.004(3) 0.015(3) 0.010(3) C33 0.040(3) 0.028(3) 0.063(4) -0.006(2) 0.026(3) -0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 2.013(4) . ? Co1 O5 2.025(3) 4 ? Co1 N1 2.159(3) . ? Co1 N2 2.161(3) 1_545 ? Co1 O2 2.204(4) 3_554 ? Co1 O1 2.235(4) 3_554 ? Co2 O4 2.007(3) . ? Co2 O6 2.026(4) 4 ? Co2 N3 2.142(3) 1_545 ? Co2 N4 2.182(3) . ? Co2 O7 2.206(4) 3 ? Co2 O8 2.210(4) 3 ? O6 C1 1.245(6) . ? O6 Co2 2.026(4) 4_455 ? O1 C17 1.258(6) . ? O1 Co1 2.235(4) 3 ? O4 C16 1.257(5) . ? O3 C16 1.261(6) . ? O5 C1 1.252(5) . ? O5 Co1 2.025(3) 4_455 ? N2 C23 1.311(6) . ? N2 C27 1.333(6) . ? N2 Co1 2.161(3) 1_565 ? O2 C17 1.248(6) . ? O2 Co1 2.204(4) 3 ? N1 C22 1.284(6) . ? N1 C18 1.333(6) . ? O7 C8 1.266(6) . ? O7 Co2 2.206(4) 3_554 ? C7 C6 1.383(6) . ? C7 C2 1.417(6) . ? O8 C8 1.265(6) . ? O8 Co2 2.210(4) 3_554 ? C2 C3 1.377(6) . ? C2 C1 1.501(6) . ? C12 C13 1.352(6) . ? C12 C11 1.374(6) . ? C12 C16 1.502(6) . ? C4 C5 1.375(6) . ? C4 C3 1.411(5) . ? C4 C9 1.509(6) . ? C13 C14 1.407(6) . ? C30 C31 1.350(7) . ? C30 C29 1.361(7) . ? C30 C35 1.489(5) . ? C35 C34 1.381(7) . ? C35 C36 1.427(7) . ? N4 C37 1.302(6) . ? N4 C33 1.328(6) . ? C17 C14 1.486(7) . ? N3 C28 1.265(6) . ? N3 C32 1.339(6) . ? N3 Co2 2.142(3) 1_565 ? C5 C6 1.407(6) . ? C9 C10 1.515(6) . ? C25 C24 1.329(8) . ? C25 C26 1.388(8) . ? C25 C20 1.510(5) . ? C29 C28 1.357(6) . ? C11 C10 1.393(5) . ? C6 C8 1.487(7) . ? C20 C19 1.317(7) . ? C20 C21 1.369(8) . ? C22 C21 1.396(6) . ? C23 C24 1.432(6) . ? C15 C14 1.359(6) . ? C15 C10 1.399(6) . ? C26 C27 1.376(6) . ? C36 C37 1.365(6) . ? C19 C18 1.375(6) . ? C34 C33 1.343(6) . ? C31 C32 1.393(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Co1 O5 120.65(15) . 4 ? O3 Co1 N1 87.71(15) . . ? O5 Co1 N1 89.31(13) 4 . ? O3 Co1 N2 92.46(15) . 1_545 ? O5 Co1 N2 89.30(13) 4 1_545 ? N1 Co1 N2 178.47(18) . 1_545 ? O3 Co1 O2 148.43(14) . 3_554 ? O5 Co1 O2 90.39(13) 4 3_554 ? N1 Co1 O2 87.07(16) . 3_554 ? N2 Co1 O2 93.58(16) 1_545 3_554 ? O3 Co1 O1 90.60(12) . 3_554 ? O5 Co1 O1 148.75(14) 4 3_554 ? N1 Co1 O1 92.58(14) . 3_554 ? N2 Co1 O1 88.94(14) 1_545 3_554 ? O2 Co1 O1 58.60(13) 3_554 3_554 ? O4 Co2 O6 122.26(15) . 4 ? O4 Co2 N3 90.14(14) . 1_545 ? O6 Co2 N3 86.96(15) 4 1_545 ? O4 Co2 N4 89.54(14) . . ? O6 Co2 N4 93.27(15) 4 . ? N3 Co2 N4 179.68(16) 1_545 . ? O4 Co2 O7 89.54(13) . 3 ? O6 Co2 O7 148.18(14) 4 3 ? N3 Co2 O7 92.36(16) 1_545 3 ? N4 Co2 O7 87.56(16) . 3 ? O4 Co2 O8 148.74(14) . 3 ? O6 Co2 O8 88.97(12) 4 3 ? N3 Co2 O8 90.58(15) 1_545 3 ? N4 Co2 O8 89.64(15) . 3 ? O7 Co2 O8 59.21(13) 3 3 ? C1 O6 Co2 140.9(3) . 4_455 ? C17 O1 Co1 89.7(3) . 3 ? C16 O4 Co2 138.1(3) . . ? C16 O3 Co1 143.8(3) . . ? C1 O5 Co1 138.0(3) . 4_455 ? C23 N2 C27 117.9(4) . . ? C23 N2 Co1 120.9(4) . 1_565 ? C27 N2 Co1 121.2(3) . 1_565 ? C17 O2 Co1 91.4(3) . 3 ? C22 N1 C18 115.1(4) . . ? C22 N1 Co1 122.0(3) . . ? C18 N1 Co1 122.9(3) . . ? C8 O7 Co2 90.7(3) . 3_554 ? C6 C7 C2 119.8(4) . . ? C8 O8 Co2 90.6(3) . 3_554 ? C3 C2 C7 119.2(4) . . ? C3 C2 C1 121.9(4) . . ? C7 C2 C1 118.8(4) . . ? C13 C12 C11 118.9(4) . . ? C13 C12 C16 120.7(4) . . ? C11 C12 C16 120.2(4) . . ? C5 C4 C3 117.7(4) . . ? C5 C4 C9 121.5(4) . . ? C3 C4 C9 120.8(4) . . ? C12 C13 C14 121.6(5) . . ? C31 C30 C29 114.3(4) . . ? C31 C30 C35 121.9(4) . . ? C29 C30 C35 123.8(4) . . ? C34 C35 C36 116.1(4) . . ? C34 C35 C30 124.5(4) . . ? C36 C35 C30 119.4(4) . . ? O4 C16 O3 124.6(4) . . ? O4 C16 C12 118.2(4) . . ? O3 C16 C12 117.2(4) . . ? C37 N4 C33 115.0(4) . . ? C37 N4 Co2 123.7(4) . . ? C33 N4 Co2 121.3(3) . . ? O2 C17 O1 120.2(5) . . ? O2 C17 C14 120.1(5) . . ? O1 C17 C14 119.6(5) . . ? C28 N3 C32 114.8(4) . . ? C28 N3 Co2 123.5(3) . 1_565 ? C32 N3 Co2 121.7(3) . 1_565 ? C2 C3 C4 121.9(4) . . ? C4 C5 C6 121.8(4) . . ? C4 C9 C10 115.1(3) . . ? O6 C1 O5 126.0(4) . . ? O6 C1 C2 116.7(4) . . ? O5 C1 C2 117.2(4) . . ? C24 C25 C26 117.2(5) . . ? C24 C25 C20 123.4(5) . . ? C26 C25 C20 119.4(4) . . ? C28 C29 C30 121.2(5) . . ? C12 C11 C10 122.6(4) . . ? C7 C6 C5 119.5(4) . . ? C7 C6 C8 120.5(4) . . ? C5 C6 C8 119.9(4) . . ? C19 C20 C21 115.8(4) . . ? C19 C20 C25 123.5(5) . . ? C21 C20 C25 120.7(5) . . ? N1 C22 C21 123.9(5) . . ? N2 C23 C24 122.4(5) . . ? O8 C8 O7 119.1(5) . . ? O8 C8 C6 121.0(5) . . ? O7 C8 C6 119.8(5) . . ? C14 C15 C10 122.9(4) . . ? C27 C26 C25 121.0(5) . . ? C15 C14 C13 117.8(4) . . ? C15 C14 C17 120.8(4) . . ? C13 C14 C17 121.4(4) . . ? C11 C10 C15 116.0(4) . . ? C11 C10 C9 123.0(4) . . ? C15 C10 C9 121.0(4) . . ? C25 C24 C23 119.7(6) . . ? C37 C36 C35 117.2(5) . . ? C20 C21 C22 119.9(5) . . ? C20 C19 C18 121.4(5) . . ? N1 C18 C19 123.6(5) . . ? N2 C27 C26 121.8(4) . . ? C33 C34 C35 119.7(5) . . ? C30 C31 C32 120.9(5) . . ? N3 C28 C29 125.9(5) . . ? N3 C32 C31 122.6(5) . . ? N4 C37 C36 126.5(5) . . ? N4 C33 C34 125.5(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 62.75 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.199 _refine_diff_density_min -0.222 _refine_diff_density_rms 0.042 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 0.075 -0.278 0.519 2791 959 ' ' _platon_squeeze_details ; ; # Attachment 'compound 2.cif' data_x0530 _database_code_depnum_ccdc_archive 'CCDC 786182' #TrackingRef 'compound 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H28 N4 O8 Zn2' _chemical_formula_weight 835.41 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Aba2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/2, y+1, z+1/2' 'x+1/2, -y+1, z+1/2' _cell_length_a 14.687(5) _cell_length_b 18.524(5) _cell_length_c 16.622(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 4522(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description lamellar _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 1.110 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7463 _exptl_absorpt_correction_T_max 0.8601 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 5393 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 24.14 _reflns_number_total 2564 _reflns_number_gt 2159 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0752P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.69(3) _refine_ls_number_reflns 2564 _refine_ls_number_parameters 250 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1159 _refine_ls_wR_factor_gt 0.1106 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.039 _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 Zn1 Zn 0.60108(3) 0.82950(3) 0.87759(6) 0.0609(2) Uani 1 1 d . . . O2 O 0.6279(2) 0.9619(2) 0.8704(4) 0.0875(13) Uani 1 1 d . . . O3 O 0.8915(2) 1.2267(2) 0.8981(3) 0.0689(13) Uani 1 1 d . . . N2 N 0.4897(3) 0.8392(2) 0.9536(3) 0.0562(11) Uani 1 1 d . . . N1 N -0.0324(3) 0.8402(2) 1.2706(3) 0.0524(10) Uani 1 1 d . . . C17 C 0.1032(3) 0.8339(3) 1.1542(4) 0.0589(14) Uani 1 1 d . . . C5 C 1.0000 1.0000 1.0374(5) 0.0572(18) Uani 1 2 d S . . H5A H 0.9836 0.9588 1.0724 0.069 Uiso 0.50 1 calc PR . . H5B H 1.0164 1.0412 1.0724 0.069 Uiso 0.50 1 calc PR . . O1 O 0.7088(2) 0.8773(2) 0.9248(3) 0.0821(13) Uani 1 1 d . . . O4 O 0.7928(3) 1.1953(3) 0.8049(3) 0.0974(16) Uani 1 1 d . . . C6 C 0.9187(3) 1.0203(3) 0.9864(3) 0.0490(12) Uani 1 1 d . . . C4 C 0.8475(3) 0.9725(3) 0.9717(4) 0.0598(13) Uani 1 1 d . . . H4 H 0.8486 0.9257 0.9952 0.072 Uiso 1 1 calc R . . C8 C 0.8429(3) 1.1086(3) 0.8991(3) 0.0485(12) Uani 1 1 d . . . C15 C 0.2590(4) 0.8533(3) 1.1081(4) 0.0701(16) Uani 1 1 d . . . H15 H 0.2666 0.8832 1.1541 0.084 Uiso 1 1 calc R . . C16 C 0.1796(4) 0.8236(3) 1.0991(3) 0.0634(15) Uani 1 1 d . . . H16 H 0.1705 0.7933 1.0538 0.076 Uiso 1 1 calc R . . C21 C 0.0305(4) 0.7857(4) 1.1526(4) 0.0679(15) Uani 1 1 d . . . H21 H 0.0258 0.7506 1.1110 0.081 Uiso 1 1 calc R . . C19 C 0.0314(4) 0.8879(3) 1.2667(4) 0.0605(15) Uani 1 1 d . . . H19 H 0.0310 0.9255 1.3056 0.073 Uiso 1 1 calc R . . C18 C 0.1003(3) 0.8884(4) 1.2101(4) 0.0579(15) Uani 1 1 d . . . H18 H 0.1447 0.9257 1.2099 0.069 Uiso 1 1 calc R . . C9 C 0.8396(3) 1.1817(3) 0.8645(5) 0.0615(15) Uani 1 1 d . . . C2 C 0.7737(3) 0.9929(3) 0.9220(3) 0.0574(13) Uani 1 1 d . . . C11 C 0.3464(3) 0.7919(3) 0.9954(3) 0.0609(14) Uani 1 1 d . . . H11 H 0.3000 0.7567 0.9886 0.073 Uiso 1 1 calc R . . C12 C 0.3381(4) 0.8458(3) 1.0552(4) 0.0630(15) Uani 1 1 d . . . C1 C 0.6956(3) 0.9411(3) 0.9031(4) 0.0613(15) Uani 1 1 d . . . C3 C 0.7736(3) 1.0596(2) 0.8857(4) 0.0539(12) Uani 1 1 d . . . H3 H 0.7250 1.0722 0.8507 0.065 Uiso 1 1 calc R . . C20 C -0.0350(3) 0.7896(4) 1.2128(4) 0.0681(15) Uani 1 1 d . . . H20 H -0.0832 0.7554 1.2131 0.082 Uiso 1 1 calc R . . C7 C 0.9147(3) 1.0872(3) 0.9497(3) 0.0495(12) Uani 1 1 d . . . H7 H 0.9629 1.1204 0.9592 0.059 Uiso 1 1 calc R . . C13 C 0.4092(5) 0.8948(5) 1.0603(5) 0.089(3) Uani 1 1 d . . . H13 H 0.4077 0.9311 1.1006 0.107 Uiso 1 1 calc R . . C14 C 0.4814(4) 0.8920(4) 1.0083(5) 0.0757(19) Uani 1 1 d . . . H14 H 0.5268 0.9284 1.0111 0.091 Uiso 1 1 calc R . . C10 C 0.4209(4) 0.7911(3) 0.9483(4) 0.0626(14) Uani 1 1 d . . . H10 H 0.4254 0.7542 0.9088 0.075 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 Zn1 0.0513(3) 0.0591(3) 0.0723(4) 0.0042(4) -0.0053(4) -0.0055(2) O2 0.0530(19) 0.095(3) 0.115(4) 0.006(4) -0.019(3) -0.0269(19) O3 0.0597(18) 0.0525(19) 0.095(4) 0.008(2) -0.013(2) 0.0000(16) N2 0.048(2) 0.062(3) 0.059(3) 0.003(2) 0.001(2) -0.005(2) N1 0.048(2) 0.058(3) 0.051(2) 0.001(2) -0.001(2) 0.003(2) C17 0.053(3) 0.075(4) 0.048(3) 0.006(3) -0.003(2) 0.011(3) C5 0.061(4) 0.049(4) 0.061(5) 0.000 0.000 0.002(3) O1 0.0477(19) 0.074(3) 0.125(4) -0.014(3) 0.000(2) -0.0100(19) O4 0.089(3) 0.110(4) 0.092(3) 0.039(3) -0.040(3) -0.015(3) C6 0.027(2) 0.055(3) 0.065(3) -0.007(3) 0.005(2) 0.004(2) C4 0.047(3) 0.058(3) 0.075(3) -0.001(3) 0.014(3) 0.005(2) C8 0.039(2) 0.052(3) 0.055(3) -0.003(2) 0.003(2) 0.0063(19) C15 0.061(4) 0.085(4) 0.063(4) -0.005(3) 0.003(3) 0.002(3) C16 0.050(3) 0.089(4) 0.051(3) 0.005(3) 0.004(2) 0.001(3) C21 0.058(3) 0.087(4) 0.059(3) -0.004(3) -0.003(3) -0.002(3) C19 0.054(3) 0.061(4) 0.067(3) 0.001(3) 0.001(3) 0.006(3) C18 0.052(3) 0.065(4) 0.057(3) 0.007(3) 0.003(2) -0.003(3) C9 0.045(2) 0.069(3) 0.070(4) 0.002(3) 0.007(3) 0.004(2) C2 0.031(2) 0.071(3) 0.070(3) -0.012(3) 0.005(2) -0.008(2) C11 0.045(3) 0.070(4) 0.068(4) 0.003(3) 0.004(3) -0.007(2) C12 0.047(3) 0.077(4) 0.064(3) 0.011(3) 0.003(3) 0.002(3) C1 0.048(3) 0.058(3) 0.078(4) -0.006(3) 0.011(3) -0.008(2) C3 0.0321(17) 0.058(3) 0.072(3) -0.010(3) 0.004(3) 0.0009(17) C20 0.044(3) 0.082(4) 0.078(4) -0.001(4) 0.001(3) 0.001(3) C7 0.034(2) 0.054(3) 0.061(3) -0.012(3) 0.004(2) -0.0060(19) C13 0.072(4) 0.094(6) 0.102(6) -0.042(5) 0.016(4) -0.014(4) C14 0.064(4) 0.071(4) 0.092(5) -0.022(4) 0.021(3) -0.021(3) C10 0.055(3) 0.068(4) 0.065(3) -0.008(3) 0.005(3) -0.008(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 Zn1 O3 1.937(4) 3_645 ? Zn1 O1 1.975(4) . ? Zn1 N1 2.055(5) 7_544 ? Zn1 N2 2.074(4) . ? Zn1 O2 2.488(4) . ? Zn1 C1 2.526(5) . ? O2 C1 1.197(7) . ? O3 C9 1.261(7) . ? O3 Zn1 1.937(4) 3_655 ? N2 C14 1.341(8) . ? N2 C10 1.351(7) . ? N1 C19 1.290(7) . ? N1 C20 1.341(8) . ? N1 Zn1 2.055(5) 7_545 ? C17 C18 1.373(9) . ? C17 C21 1.393(8) . ? C17 C16 1.460(8) . ? C5 C6 1.512(6) . ? C5 C6 1.512(6) 2_775 ? O1 C1 1.250(7) . ? O4 C9 1.233(8) . ? C6 C7 1.383(7) . ? C6 C4 1.391(7) . ? C4 C2 1.414(7) . ? C8 C3 1.383(6) . ? C8 C7 1.406(7) . ? C8 C9 1.471(7) . ? C15 C16 1.298(9) . ? C15 C12 1.463(8) . ? C21 C20 1.391(8) . ? C19 C18 1.381(9) . ? C2 C3 1.374(7) . ? C2 C1 1.529(7) . ? C11 C10 1.346(8) . ? C11 C12 1.414(8) . ? C12 C13 1.385(9) . ? C13 C14 1.368(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O1 109.00(18) 3_645 . ? O3 Zn1 N1 105.95(18) 3_645 7_544 ? O1 Zn1 N1 133.9(2) . 7_544 ? O3 Zn1 N2 91.27(17) 3_645 . ? O1 Zn1 N2 110.5(2) . . ? N1 Zn1 N2 97.6(2) 7_544 . ? O3 Zn1 O2 165.64(17) 3_645 . ? O1 Zn1 O2 56.64(17) . . ? N1 Zn1 O2 86.64(19) 7_544 . ? N2 Zn1 O2 93.93(19) . . ? O3 Zn1 C1 138.04(18) 3_645 . ? O1 Zn1 C1 29.10(18) . . ? N1 Zn1 C1 109.68(19) 7_544 . ? N2 Zn1 C1 105.08(17) . . ? O2 Zn1 C1 27.62(16) . . ? C1 O2 Zn1 78.0(3) . . ? C9 O3 Zn1 127.3(4) . 3_655 ? C14 N2 C10 117.2(5) . . ? C14 N2 Zn1 123.3(4) . . ? C10 N2 Zn1 119.5(4) . . ? C19 N1 C20 117.6(5) . . ? C19 N1 Zn1 117.8(4) . 7_545 ? C20 N1 Zn1 122.6(4) . 7_545 ? C18 C17 C21 117.4(5) . . ? C18 C17 C16 123.0(5) . . ? C21 C17 C16 119.5(6) . . ? C6 C5 C6 111.8(6) . 2_775 ? C1 O1 Zn1 100.7(3) . . ? C7 C6 C4 117.5(5) . . ? C7 C6 C5 120.2(4) . . ? C4 C6 C5 122.2(4) . . ? C6 C4 C2 120.5(5) . . ? C3 C8 C7 117.6(5) . . ? C3 C8 C9 121.1(4) . . ? C7 C8 C9 121.2(4) . . ? C16 C15 C12 127.2(6) . . ? C15 C16 C17 124.2(6) . . ? C20 C21 C17 118.8(6) . . ? N1 C19 C18 124.8(6) . . ? C17 C18 C19 118.7(6) . . ? O4 C9 O3 123.9(6) . . ? O4 C9 C8 121.5(6) . . ? O3 C9 C8 114.5(5) . . ? C3 C2 C4 119.9(4) . . ? C3 C2 C1 118.2(5) . . ? C4 C2 C1 121.8(5) . . ? C10 C11 C12 119.2(5) . . ? C13 C12 C11 116.1(5) . . ? C13 C12 C15 120.0(6) . . ? C11 C12 C15 123.9(5) . . ? O2 C1 O1 124.4(5) . . ? O2 C1 C2 120.9(5) . . ? O1 C1 C2 114.7(5) . . ? O2 C1 Zn1 74.4(3) . . ? O1 C1 Zn1 50.2(3) . . ? C2 C1 Zn1 164.0(4) . . ? C2 C3 C8 121.2(5) . . ? N1 C20 C21 122.2(6) . . ? C6 C7 C8 123.2(4) . . ? C14 C13 C12 121.4(7) . . ? N2 C14 C13 121.8(6) . . ? C11 C10 N2 124.2(6) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 24.14 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.348 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.066 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 0.500 0.205 333 65 ' ' 2 0.000 0.000 0.705 333 65 ' ' 3 0.500 0.000 0.205 333 65 ' ' 4 0.500 0.500 0.705 333 65 ' ' _platon_squeeze_details ; ; # Attachment 'compound 4.cif' data_x0477-1 _database_code_depnum_ccdc_archive 'CCDC 802621' #TrackingRef 'compound 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H51 Co4 N7 O18' _chemical_formula_weight 1501.89 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 trigonal _symmetry_space_group_name_H-M P32 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' _cell_length_a 19.8876(4) _cell_length_b 19.8876(4) _cell_length_c 19.1704(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6566.4(3) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2298 _exptl_absorpt_coefficient_mu 0.804 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7608 _exptl_absorpt_correction_T_max 0.7831 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 19457 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0710 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 23.26 _reflns_number_total 11628 _reflns_number_gt 9029 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.1507P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(2) _refine_ls_number_reflns 11628 _refine_ls_number_parameters 859 _refine_ls_number_restraints 653 _refine_ls_R_factor_all 0.0883 _refine_ls_R_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.2179 _refine_ls_wR_factor_gt 0.2113 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.026 _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 Co2 Co 0.43357(6) 0.53459(7) 0.32995(6) 0.0315(3) Uani 1 1 d . . . Co4 Co -0.10240(6) 0.46324(6) 0.25528(7) 0.0322(3) Uani 1 1 d . . . Co3 Co 0.07897(6) 0.56193(6) 0.15883(6) 0.0319(3) Uani 1 1 d . . . Co1 Co 0.51805(6) 0.43846(6) 0.42488(6) 0.0310(3) Uani 1 1 d . . . O12 O 0.1010(3) 0.5229(4) 0.2507(4) 0.0459(17) Uani 1 1 d . . . O10 O 0.3206(3) 0.5046(4) 0.3564(4) 0.0454(17) Uani 1 1 d . . . O14 O 0.0200(3) 0.4558(4) 0.6340(4) 0.0477(18) Uani 1 1 d . . . O1 O 0.4166(3) 0.4292(3) 0.3767(3) 0.0324(14) Uani 1 1 d . . . O18 O -0.0128(3) 0.5698(3) 0.2116(3) 0.0356(15) Uani 1 1 d . . . O16 O -0.2944(4) 0.1157(4) 0.4865(4) 0.0491(18) Uani 1 1 d . . . O7 O 0.5922(4) 0.4782(4) 0.8260(4) 0.0423(16) Uani 1 1 d . . . O17 O -0.3214(3) 0.1860(3) 0.5599(3) 0.0414(16) Uani 1 1 d . . . O9 O 0.9103(4) 0.6144(4) 0.6598(4) 0.054(2) Uani 1 1 d . . . O5 O 0.6133(4) 0.9094(4) 0.5927(4) 0.055(2) Uani 1 1 d . . . O15 O -0.1023(3) 0.4202(3) 0.6678(3) 0.0395(16) Uani 1 1 d . . . O8 O 0.8525(4) 0.5311(4) 0.7473(4) 0.053(2) Uani 1 1 d . . . O11 O 0.2942(4) 0.4095(4) 0.4328(4) 0.0496(18) Uani 1 1 d . . . C11 C 0.0842(5) 0.4314(5) 0.3363(5) 0.033(2) Uani 1 1 d U . . C8 C 0.7285(5) 0.5612(5) 0.7475(5) 0.038(2) Uani 1 1 d U . . H8 H 0.7240 0.5211 0.7757 0.046 Uiso 1 1 calc R . . C9 C 0.1897(5) 0.4213(5) 0.3884(5) 0.032(2) Uani 1 1 d U . . O3 O 0.4753(4) 0.5910(3) 0.4243(4) 0.0439(17) Uani 1 1 d . . . C10 C 0.1629(5) 0.4566(5) 0.3441(5) 0.032(2) Uani 1 1 d U . . H10 H 0.1986 0.4991 0.3182 0.038 Uiso 1 1 calc R . . O4 O 0.5266(4) 0.8483(4) 0.5111(4) 0.052(2) Uani 1 1 d . . . C6 C 0.7997(5) 0.6621(5) 0.6656(5) 0.035(2) Uani 1 1 d U . . H6 H 0.8439 0.6894 0.6383 0.042 Uiso 1 1 calc R . . C17 C -0.1645(6) 0.2955(5) 0.5770(5) 0.040(2) Uani 1 1 d U . . H17 H -0.1989 0.3033 0.6038 0.048 Uiso 1 1 calc R . . C5 C 0.7436(5) 0.6826(5) 0.6631(5) 0.036(2) Uani 1 1 d U . . C16 C -0.0844(5) 0.3459(5) 0.5817(5) 0.031(2) Uani 1 1 d U . . C7 C 0.7933(5) 0.6017(5) 0.7076(6) 0.040(2) Uani 1 1 d U . . C15 C -0.0592(6) 0.2704(5) 0.5000(6) 0.043(3) Uani 1 1 d U . . C4 C 0.6606(6) 0.7986(5) 0.5875(5) 0.039(2) Uani 1 1 d U . . H4 H 0.6883 0.8426 0.6149 0.047 Uiso 1 1 calc R . . C2 C 0.5744(5) 0.6648(5) 0.5088(5) 0.037(2) Uani 1 1 d U . . C13 C 0.0574(5) 0.3288(5) 0.4202(5) 0.036(2) Uani 1 1 d U . . C12 C 0.0319(5) 0.3651(5) 0.3756(5) 0.039(2) Uani 1 1 d U . . H12 H -0.0212 0.3458 0.3709 0.047 Uiso 1 1 calc R . . C18 C -0.1920(5) 0.2312(5) 0.5291(5) 0.034(2) Uani 1 1 d U . . C14 C 0.1390(5) 0.3585(5) 0.4262(5) 0.034(2) Uani 1 1 d U . . H14 H 0.1575 0.3347 0.4561 0.041 Uiso 1 1 calc R . . O13 O -0.0195(3) 0.4352(4) 0.2862(4) 0.0485(18) Uani 1 1 d . . . C3 C 0.5988(5) 0.7897(5) 0.5501(5) 0.034(2) Uani 1 1 d U . . O6 O 0.5456(4) 0.5509(4) 0.7864(4) 0.055(2) Uani 1 1 d . . . N5 N 0.1733(5) 0.5635(5) 0.1032(4) 0.0432(19) Uani 1 1 d DU . . C041 C -0.0333(5) 0.3325(5) 0.5446(5) 0.036(2) Uani 1 1 d U . . H041 H 0.0198 0.3661 0.5497 0.044 Uiso 1 1 calc R . . C042 C 0.6693(5) 0.5783(5) 0.7470(5) 0.035(2) Uani 1 1 d U . . C043 C 0.5536(6) 0.7231(5) 0.5100(6) 0.047(3) Uani 1 1 d U . . H043 H 0.5111 0.7174 0.4849 0.057 Uiso 1 1 calc R . . C044 C 0.7525(6) 0.7526(6) 0.6241(6) 0.047(3) Uani 1 1 d U . . H04A H 0.7668 0.7944 0.6574 0.057 Uiso 1 1 calc R . . H04B H 0.7951 0.7693 0.5915 0.057 Uiso 1 1 calc R . . C045 C 0.6387(5) 0.6758(5) 0.5460(5) 0.033(2) Uani 1 1 d U . . H045 H 0.6524 0.6374 0.5446 0.040 Uiso 1 1 calc R . . C046 C 0.6833(6) 0.7414(6) 0.5851(5) 0.043(2) Uani 1 1 d U . . N4 N -0.1926(5) 0.3494(5) 0.2963(5) 0.053(2) Uani 1 1 d U . . O2 O 0.5474(4) 0.5419(4) 0.4685(4) 0.054(2) Uani 1 1 d . . . C049 C -0.1375(5) 0.2209(5) 0.4892(5) 0.039(2) Uani 1 1 d U . . H049 H -0.1545 0.1814 0.4563 0.047 Uiso 1 1 calc R . . N2 N 0.6056(6) 0.4323(6) 0.4857(5) 0.072(2) Uani 1 1 d DU . . C051 C 0.6788(5) 0.6394(5) 0.7052(5) 0.034(2) Uani 1 1 d U . . H051 H 0.6398 0.6522 0.7052 0.041 Uiso 1 1 calc R . . C052 C -0.2763(5) 0.1745(5) 0.5254(5) 0.034(2) Uani 1 1 d U . . C053 C 0.5774(5) 0.8543(5) 0.5516(5) 0.034(2) Uani 1 1 d U . . C054 C -0.0008(5) 0.2549(5) 0.4590(5) 0.038(2) Uani 1 1 d U . . H05A H 0.0267 0.2394 0.4910 0.045 Uiso 1 1 calc R . . H05B H -0.0286 0.2131 0.4258 0.045 Uiso 1 1 calc R . . C055 C 0.5300(5) 0.5954(6) 0.4641(6) 0.044(3) Uani 1 1 d U . . C056 C 0.0532(5) 0.4659(6) 0.2876(5) 0.038(2) Uani 1 1 d U . . C057 C 0.8581(5) 0.5807(6) 0.7044(6) 0.044(3) Uani 1 1 d U . . C058 C 0.2751(5) 0.4468(5) 0.3936(5) 0.034(2) Uani 1 1 d U . . C059 C 0.5948(6) 0.5307(5) 0.7916(5) 0.037(2) Uani 1 1 d U . . C060 C -0.0538(5) 0.4131(5) 0.6324(5) 0.034(2) Uani 1 1 d U . . N1 N 0.3915(5) 0.4800(5) 0.2299(5) 0.055(2) Uani 1 1 d U . . N3 N -0.0992(6) 0.5124(5) 0.3560(5) 0.062(3) Uani 1 1 d U . . C063 C 0.6709(8) 0.3662(9) 0.5141(7) 0.093(4) Uani 1 1 d DU . . H063 H 0.6808 0.3261 0.5040 0.112 Uiso 1 1 calc R . . C066 C 0.2289(10) 0.4907(10) 0.0541(7) 0.107(5) Uani 1 1 d DU . . H066 H 0.2282 0.4441 0.0469 0.128 Uiso 1 1 calc R . . C067 C 0.4251(7) 0.5125(7) 0.1734(7) 0.067(3) Uani 1 1 d U . . H067 H 0.4721 0.5586 0.1781 0.080 Uiso 1 1 calc R . . C068 C 0.4009(10) 0.4882(10) 0.1048(9) 0.104(5) Uani 1 1 d U . . H068 H 0.4267 0.5174 0.0657 0.125 Uiso 1 1 calc R . . C072 C 0.7096(10) 0.4160(9) 0.5656(9) 0.109(5) Uani 1 1 d DU . . H072 H 0.7463 0.4107 0.5914 0.131 Uiso 1 1 calc R . . C073 C -0.1092(8) 0.5733(9) 0.3635(8) 0.089(4) Uani 1 1 d U . . H073 H -0.1145 0.5974 0.3240 0.106 Uiso 1 1 calc R . . C074 C -0.1034(9) 0.5017(9) 0.4781(9) 0.094(4) Uani 1 1 d U . . H074 H -0.0991 0.4773 0.5178 0.113 Uiso 1 1 calc R . . C076 C -0.3029(9) 0.2618(9) 0.3584(8) 0.092(4) Uani 1 1 d U . . H076 H -0.3453 0.2538 0.3851 0.111 Uiso 1 1 calc R . . C077 C -0.1003(8) 0.4755(8) 0.4196(7) 0.074(4) Uani 1 1 d U . . H077 H -0.0986 0.4297 0.4177 0.089 Uiso 1 1 calc R . . C079 C -0.1847(8) 0.2881(7) 0.2842(7) 0.073(3) Uani 1 1 d U . . H079 H -0.1434 0.2956 0.2561 0.087 Uiso 1 1 calc R . . C082 C 0.6188(7) 0.3737(8) 0.4776(7) 0.073(4) Uani 1 1 d DU . . H082 H 0.5899 0.3359 0.4445 0.088 Uiso 1 1 calc R . . C083 C -0.2512(8) 0.3361(9) 0.3321(7) 0.082(4) Uani 1 1 d U . . H083 H -0.2604 0.3766 0.3414 0.099 Uiso 1 1 calc R . . C084 C 0.3252(8) 0.4090(9) 0.2263(8) 0.087(4) Uani 1 1 d U . . H084 H 0.3006 0.3849 0.2677 0.104 Uiso 1 1 calc R . . C085 C 0.2935(10) 0.3719(11) 0.1645(9) 0.107(5) Uani 1 1 d U . . H085 H 0.2496 0.3227 0.1632 0.128 Uiso 1 1 calc R . . C086 C 0.1687(10) 0.4924(10) 0.0891(6) 0.098(5) Uani 1 1 d DU . . H086 H 0.1254 0.4464 0.1032 0.118 Uiso 1 1 calc R . . C087 C 0.2371(7) 0.6295(8) 0.0857(6) 0.073(4) Uani 1 1 d DU . . H087 H 0.2400 0.6765 0.0962 0.087 Uiso 1 1 calc R . . C089 C -0.2316(9) 0.2154(10) 0.3092(8) 0.098(4) Uani 1 1 d U . . H089 H -0.2219 0.1749 0.3010 0.117 Uiso 1 1 calc R . . C090 C 0.6385(8) 0.4767(8) 0.5384(7) 0.085(2) Uani 1 1 d DU . . H090 H 0.6232 0.5126 0.5494 0.102 Uiso 1 1 calc R . . C091 C -0.1121(11) 0.6028(12) 0.4317(11) 0.131(6) Uani 1 1 d U . . H091 H -0.1136 0.6484 0.4377 0.157 Uiso 1 1 calc R . . C092 C -0.2915(10) 0.2061(10) 0.3457(8) 0.094(4) Uani 1 1 d U . . H092 H -0.3266 0.1570 0.3627 0.113 Uiso 1 1 calc R . . C094 C 0.6946(9) 0.4756(9) 0.5804(8) 0.096(3) Uani 1 1 d DU . . H094 H 0.7202 0.5118 0.6155 0.115 Uiso 1 1 calc R . . C095 C 0.3320(11) 0.4132(11) 0.1015(10) 0.120(6) Uani 1 1 d U . . H095 H 0.3119 0.3910 0.0582 0.143 Uiso 1 1 calc R . . C096 C -0.1123(11) 0.5601(11) 0.4853(11) 0.124(6) Uani 1 1 d U . . H096 H -0.1192 0.5739 0.5300 0.149 Uiso 1 1 calc R . . C23 C 0.0154(7) 0.6874(6) -0.0008(6) 0.111(5) Uani 1 1 d GDU . . H23 H 0.0074 0.7296 -0.0005 0.134 Uiso 1 1 calc R . . C24 C 0.0395(6) 0.6668(5) 0.0596(5) 0.107(5) Uani 1 1 d GDU . . H24 H 0.0475 0.6953 0.1003 0.129 Uiso 1 1 calc R . . N6 N 0.0514(5) 0.6037(6) 0.0592(4) 0.087(3) Uani 1 1 d GU . . C20 C 0.0394(6) 0.5611(5) -0.0017(6) 0.100(5) Uani 1 1 d GDU . . H20 H 0.0474 0.5189 -0.0020 0.120 Uiso 1 1 calc R . . C21 C 0.0153(7) 0.5816(7) -0.0621(4) 0.142(7) Uani 1 1 d GDU . . H21 H 0.0072 0.5531 -0.1028 0.171 Uiso 1 1 calc R . . C22 C 0.0033(7) 0.6448(8) -0.0617(5) 0.145(7) Uani 1 1 d GDU . . H22 H -0.0128 0.6585 -0.1021 0.174 Uiso 1 1 calc R . . C1 C 0.2999(8) 0.6300(8) 0.0518(7) 0.082(4) Uani 1 1 d DU . . H1 H 0.3463 0.6762 0.0450 0.099 Uiso 1 1 calc R . . C64 C 0.2915(10) 0.5617(10) 0.0294(8) 0.102(5) Uani 1 1 d DU . . H64 H 0.3268 0.5613 -0.0022 0.122 Uiso 1 1 calc R . . C30 C 0.4073(6) 0.7125(6) 0.2154(5) 0.118(6) Uani 1 1 d GU . . H30 H 0.3690 0.7139 0.1886 0.141 Uiso 1 1 calc R . . C32 C 0.4781(7) 0.7800(5) 0.2256(6) 0.151(7) Uani 1 1 d GU . . H32 H 0.4872 0.8264 0.2057 0.181 Uiso 1 1 calc R . . C31 C 0.5354(5) 0.7780(4) 0.2656(6) 0.122(6) Uani 1 1 d GU . . H31 H 0.5828 0.8231 0.2724 0.147 Uiso 1 1 calc R . . C33 C 0.5219(4) 0.7086(5) 0.2953(4) 0.076(4) Uani 1 1 d GU . . H33 H 0.5602 0.7073 0.3221 0.091 Uiso 1 1 calc R . . N8 N 0.4511(4) 0.6411(4) 0.2851(4) 0.052(2) Uani 1 1 d GU . . C35 C 0.3938(4) 0.6431(5) 0.2451(4) 0.080(4) Uani 1 1 d GU . . H35 H 0.3464 0.5980 0.2383 0.096 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 Co2 0.0213(6) 0.0298(7) 0.0462(8) 0.0008(6) 0.0027(5) 0.0147(5) Co4 0.0216(6) 0.0287(6) 0.0484(8) 0.0000(6) -0.0017(6) 0.0143(5) Co3 0.0206(6) 0.0191(6) 0.0496(8) -0.0037(5) 0.0013(6) 0.0052(5) Co1 0.0295(6) 0.0206(6) 0.0464(8) -0.0024(5) -0.0038(6) 0.0151(5) O12 0.019(3) 0.042(4) 0.071(5) 0.015(4) -0.001(3) 0.010(3) O10 0.023(3) 0.054(4) 0.066(5) 0.014(4) 0.005(3) 0.024(3) O14 0.021(3) 0.033(4) 0.075(5) -0.017(3) 0.001(3) 0.003(3) O1 0.024(3) 0.023(3) 0.052(4) 0.003(3) 0.003(3) 0.013(3) O18 0.023(3) 0.029(3) 0.053(4) -0.003(3) -0.001(3) 0.011(3) O16 0.031(4) 0.038(4) 0.061(5) -0.010(4) 0.010(3) 0.004(3) O7 0.036(4) 0.045(4) 0.058(4) 0.011(3) 0.013(3) 0.029(3) O17 0.019(3) 0.035(4) 0.050(4) 0.004(3) 0.021(3) -0.001(3) O9 0.040(4) 0.072(5) 0.071(5) 0.028(4) 0.025(4) 0.044(4) O5 0.065(5) 0.043(4) 0.073(5) -0.027(4) -0.032(4) 0.038(4) O15 0.020(3) 0.040(4) 0.052(4) -0.013(3) -0.003(3) 0.009(3) O8 0.048(4) 0.054(4) 0.079(5) 0.040(4) 0.027(4) 0.042(4) O11 0.036(4) 0.067(5) 0.059(5) 0.033(4) 0.008(3) 0.036(4) C11 0.018(4) 0.035(5) 0.055(6) 0.001(4) 0.002(4) 0.019(4) C8 0.037(5) 0.041(5) 0.048(6) 0.015(5) 0.008(5) 0.027(5) C9 0.024(4) 0.034(5) 0.042(5) 0.009(4) 0.010(4) 0.018(4) O3 0.042(4) 0.031(3) 0.063(5) -0.008(3) -0.016(3) 0.022(3) C10 0.028(5) 0.029(5) 0.041(5) 0.003(4) 0.005(4) 0.016(4) O4 0.049(4) 0.042(4) 0.083(5) -0.026(4) -0.040(4) 0.035(4) C6 0.029(5) 0.042(5) 0.039(5) 0.008(4) -0.002(4) 0.020(4) C17 0.042(5) 0.027(5) 0.052(6) 0.003(4) -0.001(5) 0.018(4) C5 0.028(5) 0.032(5) 0.047(6) 0.004(4) -0.005(4) 0.014(4) C16 0.021(4) 0.020(4) 0.039(5) 0.002(4) 0.000(4) 0.001(4) C7 0.012(4) 0.035(5) 0.073(7) 0.001(5) 0.004(4) 0.012(4) C15 0.033(5) 0.025(5) 0.066(7) 0.008(5) 0.013(5) 0.009(4) C4 0.054(6) 0.023(5) 0.041(6) -0.003(4) -0.005(5) 0.019(4) C2 0.036(5) 0.022(4) 0.064(6) -0.011(4) -0.013(5) 0.022(4) C13 0.032(5) 0.038(5) 0.042(6) -0.010(4) 0.007(4) 0.021(4) C12 0.018(4) 0.037(5) 0.062(7) 0.007(5) 0.011(4) 0.015(4) C18 0.044(5) 0.025(5) 0.030(5) -0.001(4) -0.001(4) 0.015(4) C14 0.032(5) 0.045(5) 0.034(5) -0.001(4) 0.001(4) 0.025(4) O13 0.019(3) 0.055(4) 0.066(5) 0.019(4) 0.001(3) 0.016(3) C3 0.044(5) 0.030(5) 0.042(5) -0.013(4) -0.021(4) 0.030(4) O6 0.034(4) 0.049(4) 0.092(6) 0.027(4) 0.023(4) 0.029(3) N5 0.043(2) 0.043(2) 0.044(2) -0.0008(10) 0.0006(10) 0.0217(13) C041 0.021(4) 0.030(5) 0.046(6) 0.002(4) -0.005(4) 0.003(4) C042 0.029(5) 0.040(5) 0.046(5) 0.008(4) 0.007(4) 0.025(4) C043 0.058(6) 0.041(6) 0.060(7) -0.010(5) -0.021(5) 0.037(5) C044 0.035(5) 0.037(5) 0.062(7) 0.018(5) -0.015(5) 0.012(4) C045 0.040(5) 0.028(5) 0.049(6) -0.006(4) -0.009(4) 0.030(4) C046 0.039(5) 0.037(5) 0.063(7) 0.015(5) -0.003(5) 0.027(5) N4 0.053(2) 0.053(2) 0.053(2) 0.0009(10) -0.0002(10) 0.0267(14) O2 0.067(5) 0.042(4) 0.076(5) -0.017(4) -0.027(4) 0.045(4) C049 0.028(5) 0.024(5) 0.058(6) 0.011(4) 0.012(4) 0.008(4) N2 0.072(2) 0.072(2) 0.075(2) 0.0023(10) 0.0008(10) 0.0377(14) C051 0.034(5) 0.031(5) 0.049(6) 0.007(4) -0.002(4) 0.026(4) C052 0.024(5) 0.022(5) 0.045(6) -0.007(4) -0.004(4) 0.005(4) C053 0.041(5) 0.023(5) 0.042(6) -0.006(4) -0.006(5) 0.020(4) C054 0.030(5) 0.038(5) 0.049(6) -0.005(5) 0.010(4) 0.020(4) C055 0.030(5) 0.043(6) 0.066(7) 0.000(5) -0.014(5) 0.024(5) C056 0.033(5) 0.043(6) 0.050(6) 0.009(5) 0.016(5) 0.028(5) C057 0.020(5) 0.050(6) 0.075(8) 0.011(6) 0.010(5) 0.026(5) C058 0.028(5) 0.033(5) 0.036(5) 0.002(4) 0.005(4) 0.012(4) C059 0.044(6) 0.032(5) 0.045(6) 0.005(5) 0.005(5) 0.027(5) C060 0.035(6) 0.021(4) 0.040(6) 0.004(4) -0.004(4) 0.010(4) N1 0.055(2) 0.056(2) 0.055(2) -0.0002(10) 0.0001(10) 0.0269(14) N3 0.062(3) 0.062(3) 0.062(3) 0.0003(10) -0.0005(10) 0.0311(15) C063 0.093(4) 0.093(4) 0.094(4) 0.0002(10) -0.0006(10) 0.047(2) C066 0.107(5) 0.107(5) 0.108(5) -0.0004(10) -0.0001(10) 0.054(3) C067 0.067(3) 0.067(3) 0.067(3) 0.0001(10) 0.0001(10) 0.0335(18) C068 0.104(5) 0.104(5) 0.104(5) -0.0001(10) 0.0005(10) 0.052(3) C072 0.110(5) 0.109(5) 0.110(5) -0.0002(10) -0.0005(10) 0.055(3) C073 0.089(4) 0.089(4) 0.088(4) -0.0004(10) -0.0001(10) 0.044(2) C074 0.094(4) 0.094(4) 0.094(4) 0.0001(10) -0.0001(10) 0.047(2) C076 0.092(4) 0.092(4) 0.092(4) 0.0001(10) 0.0003(10) 0.046(2) C077 0.074(4) 0.074(4) 0.074(4) 0.0000(10) 0.0000(10) 0.037(2) C079 0.073(4) 0.072(4) 0.073(4) 0.0001(10) 0.0001(10) 0.0358(19) C082 0.073(4) 0.073(4) 0.074(4) 0.0004(10) -0.0014(10) 0.037(2) C083 0.082(4) 0.082(4) 0.082(4) 0.0002(10) 0.0000(10) 0.041(2) C084 0.087(4) 0.087(4) 0.086(4) -0.0004(10) 0.0001(10) 0.043(2) C085 0.106(5) 0.107(5) 0.106(5) -0.0002(10) -0.0002(10) 0.053(3) C086 0.098(5) 0.098(5) 0.098(5) -0.0004(10) 0.0002(10) 0.049(2) C087 0.072(4) 0.073(4) 0.073(4) -0.0004(10) 0.0013(10) 0.0366(19) C089 0.098(5) 0.097(5) 0.098(5) 0.0007(10) -0.0001(10) 0.049(2) C090 0.086(2) 0.084(2) 0.083(2) -0.0041(10) 0.0000(10) 0.0412(14) C091 0.131(6) 0.131(6) 0.131(6) -0.0003(10) 0.0004(10) 0.066(3) C092 0.095(4) 0.094(4) 0.094(4) 0.0003(10) -0.0004(10) 0.047(2) C094 0.095(3) 0.097(3) 0.096(3) 0.0010(10) -0.0031(10) 0.0487(17) C095 0.120(6) 0.120(6) 0.119(6) -0.0006(10) 0.0002(10) 0.060(3) C096 0.124(6) 0.124(6) 0.124(6) 0.0000(10) -0.0002(10) 0.062(3) C23 0.111(5) 0.112(5) 0.112(5) 0.0003(10) -0.0001(10) 0.056(3) C24 0.107(5) 0.107(5) 0.107(5) 0.0004(10) 0.0002(10) 0.054(3) N6 0.087(3) 0.087(3) 0.087(3) 0.0002(10) 0.0004(10) 0.0439(19) C20 0.100(5) 0.100(5) 0.100(5) -0.0001(10) 0.0000(10) 0.050(3) C21 0.142(7) 0.142(7) 0.142(7) 0.0000(10) 0.0000(10) 0.071(3) C22 0.145(7) 0.145(7) 0.145(7) -0.0001(10) -0.0002(10) 0.072(4) C1 0.082(4) 0.082(4) 0.083(4) 0.0001(10) 0.0007(10) 0.041(2) C64 0.102(5) 0.102(5) 0.101(5) -0.0003(10) 0.0004(10) 0.051(3) C30 0.118(6) 0.118(6) 0.118(6) -0.0001(10) -0.0003(10) 0.059(3) C32 0.151(7) 0.151(7) 0.151(7) 0.0000(10) 0.0005(10) 0.076(4) C31 0.122(6) 0.122(6) 0.123(6) 0.0003(10) 0.0005(10) 0.061(3) C33 0.076(4) 0.076(4) 0.077(4) 0.0005(10) 0.0002(10) 0.039(2) N8 0.052(2) 0.052(2) 0.053(2) 0.0008(10) 0.0005(10) 0.0268(14) C35 0.080(4) 0.080(4) 0.080(4) 0.0007(10) 0.0002(10) 0.041(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co2 O14 2.052(6) 2_664 ? Co2 O3 2.070(7) . ? Co2 O10 2.079(6) . ? Co2 O1 2.145(5) . ? Co2 N8 2.148(6) . ? Co2 N1 2.157(9) . ? Co4 O13 2.074(6) . ? Co4 O17 2.093(6) 2_564 ? Co4 O7 2.097(6) 3_564 ? Co4 O18 2.143(6) . ? Co4 N3 2.151(10) . ? Co4 N4 2.214(9) . ? Co3 O6 2.037(6) 3_564 ? Co3 O4 2.057(6) 2_664 ? Co3 O12 2.058(7) . ? Co3 N5 2.145(8) . ? Co3 O18 2.160(6) . ? Co3 N6 2.257(8) . ? Co1 O2 2.018(6) . ? Co1 O8 2.036(6) 2_654 ? Co1 O15 2.040(6) 2_664 ? Co1 O1 2.141(6) . ? Co1 N2 2.149(11) . ? O12 C056 1.271(11) . ? O10 C058 1.269(11) . ? O14 C060 1.277(11) . ? O14 Co2 2.052(6) 3_565 ? O16 C052 1.277(11) . ? O7 C059 1.213(10) . ? O7 Co4 2.097(6) 2_665 ? O17 C052 1.225(11) . ? O17 Co4 2.093(6) 3_455 ? O9 C057 1.250(11) . ? O5 C053 1.245(11) . ? O15 C060 1.243(11) . ? O15 Co1 2.040(6) 3_565 ? O8 C057 1.247(12) . ? O8 Co1 2.036(6) 3_665 ? O11 C058 1.241(11) . ? C11 C10 1.392(12) . ? C11 C12 1.419(13) . ? C11 C056 1.465(13) . ? C8 C7 1.362(13) . ? C8 C042 1.378(12) . ? C9 C14 1.356(13) . ? C9 C10 1.368(12) . ? C9 C058 1.514(12) . ? O3 C055 1.295(11) . ? O4 C053 1.232(11) . ? O4 Co3 2.057(6) 3_565 ? C6 C5 1.366(13) . ? C6 C7 1.399(13) . ? C17 C16 1.398(13) . ? C17 C18 1.442(13) . ? C5 C051 1.394(13) . ? C5 C044 1.510(12) . ? C16 C041 1.370(13) . ? C16 C060 1.514(12) . ? C7 C057 1.542(12) . ? C15 C041 1.373(13) . ? C15 C049 1.380(14) . ? C15 C054 1.556(12) . ? C4 C3 1.354(13) . ? C4 C046 1.419(13) . ? C2 C045 1.383(12) . ? C2 C043 1.413(12) . ? C2 C055 1.484(13) . ? C13 C12 1.370(13) . ? C13 C14 1.428(13) . ? C13 C054 1.533(13) . ? C18 C049 1.421(13) . ? C18 C052 1.482(13) . ? O13 C056 1.258(11) . ? C3 C043 1.401(13) . ? C3 C053 1.543(12) . ? O6 C059 1.233(11) . ? O6 Co3 2.037(6) 2_665 ? N5 C087 1.334(14) . ? N5 C086 1.397(17) . ? C042 C051 1.387(12) . ? C042 C059 1.556(13) . ? C044 C046 1.483(13) . ? C045 C046 1.376(13) . ? N4 C083 1.260(15) . ? N4 C079 1.324(15) . ? O2 C055 1.275(11) . ? N2 C090 1.285(16) . ? N2 C082 1.327(16) . ? N1 C067 1.267(14) . ? N1 C084 1.369(16) . ? N3 C073 1.331(17) . ? N3 C077 1.416(15) . ? C063 C082 1.320(18) . ? C063 C072 1.34(2) . ? C066 C086 1.39(2) . ? C066 C64 1.42(2) . ? C067 C068 1.400(19) . ? C068 C095 1.44(2) . ? C072 C094 1.39(2) . ? C073 C091 1.44(2) . ? C074 C077 1.251(18) . ? C074 C096 1.27(2) . ? C076 C092 1.261(19) . ? C076 C083 1.41(2) . ? C079 C089 1.357(19) . ? C084 C085 1.372(19) . ? C085 C095 1.45(2) . ? C087 C1 1.404(18) . ? C089 C092 1.31(2) . ? C090 C094 1.385(19) . ? C091 C096 1.33(2) . ? C23 C24 1.3900 . ? C23 C22 1.3900 . ? C24 N6 1.3900 . ? N6 C20 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C1 C64 1.35(2) . ? C30 C32 1.3900 . ? C30 C35 1.3900 . ? C32 C31 1.3900 . ? C31 C33 1.3900 . ? C33 N8 1.3900 . ? N8 C35 1.3900 . ? 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 O14 Co2 O3 90.1(3) 2_664 . ? O14 Co2 O10 178.2(3) 2_664 . ? O3 Co2 O10 91.5(3) . . ? O14 Co2 O1 91.0(2) 2_664 . ? O3 Co2 O1 89.4(2) . . ? O10 Co2 O1 89.9(2) . . ? O14 Co2 N8 89.2(3) 2_664 . ? O3 Co2 N8 89.5(3) . . ? O10 Co2 N8 90.0(3) . . ? O1 Co2 N8 178.9(3) . . ? O14 Co2 N1 89.5(3) 2_664 . ? O3 Co2 N1 177.9(3) . . ? O10 Co2 N1 88.9(3) . . ? O1 Co2 N1 92.8(3) . . ? N8 Co2 N1 88.4(3) . . ? O13 Co4 O17 178.6(3) . 2_564 ? O13 Co4 O7 90.1(3) . 3_564 ? O17 Co4 O7 91.3(3) 2_564 3_564 ? O13 Co4 O18 89.9(2) . . ? O17 Co4 O18 90.3(2) 2_564 . ? O7 Co4 O18 89.7(2) 3_564 . ? O13 Co4 N3 91.1(3) . . ? O17 Co4 N3 87.5(3) 2_564 . ? O7 Co4 N3 175.5(3) 3_564 . ? O18 Co4 N3 94.6(3) . . ? O13 Co4 N4 88.3(3) . . ? O17 Co4 N4 91.6(3) 2_564 . ? O7 Co4 N4 87.3(3) 3_564 . ? O18 Co4 N4 176.6(3) . . ? N3 Co4 N4 88.3(4) . . ? O6 Co3 O4 168.0(3) 3_564 2_664 ? O6 Co3 O12 95.5(3) 3_564 . ? O4 Co3 O12 96.4(3) 2_664 . ? O6 Co3 N5 89.8(3) 3_564 . ? O4 Co3 N5 87.3(3) 2_664 . ? O12 Co3 N5 94.7(3) . . ? O6 Co3 O18 93.3(2) 3_564 . ? O4 Co3 O18 88.9(2) 2_664 . ? O12 Co3 O18 88.5(2) . . ? N5 Co3 O18 175.3(3) . . ? O6 Co3 N6 84.0(3) 3_564 . ? O4 Co3 N6 84.2(3) 2_664 . ? O12 Co3 N6 178.4(3) . . ? N5 Co3 N6 86.8(3) . . ? O18 Co3 N6 90.0(3) . . ? O2 Co1 O8 159.6(3) . 2_654 ? O2 Co1 O15 98.7(3) . 2_664 ? O8 Co1 O15 101.7(3) 2_654 2_664 ? O2 Co1 O1 92.6(2) . . ? O8 Co1 O1 88.0(2) 2_654 . ? O15 Co1 O1 91.7(2) 2_664 . ? O2 Co1 N2 90.2(3) . . ? O8 Co1 N2 86.0(3) 2_654 . ? O15 Co1 N2 97.6(3) 2_664 . ? O1 Co1 N2 169.8(3) . . ? C056 O12 Co3 127.5(6) . . ? C058 O10 Co2 125.1(6) . . ? C060 O14 Co2 138.1(6) . 3_565 ? Co1 O1 Co2 114.5(2) . . ? Co4 O18 Co3 115.2(3) . . ? C059 O7 Co4 128.4(6) . 2_665 ? C052 O17 Co4 126.1(6) . 3_455 ? C060 O15 Co1 125.6(6) . 3_565 ? C057 O8 Co1 129.0(6) . 3_665 ? C10 C11 C12 116.7(8) . . ? C10 C11 C056 124.0(8) . . ? C12 C11 C056 119.2(8) . . ? C7 C8 C042 121.5(9) . . ? C14 C9 C10 120.2(8) . . ? C14 C9 C058 117.8(8) . . ? C10 C9 C058 121.9(8) . . ? C055 O3 Co2 130.3(6) . . ? C9 C10 C11 122.4(8) . . ? C053 O4 Co3 131.1(6) . 3_565 ? C5 C6 C7 122.6(8) . . ? C16 C17 C18 117.9(9) . . ? C6 C5 C051 115.9(8) . . ? C6 C5 C044 123.8(9) . . ? C051 C5 C044 120.0(8) . . ? C041 C16 C17 121.2(8) . . ? C041 C16 C060 119.7(8) . . ? C17 C16 C060 118.9(8) . . ? C8 C7 C6 119.0(8) . . ? C8 C7 C057 122.3(9) . . ? C6 C7 C057 118.6(8) . . ? C041 C15 C049 121.1(9) . . ? C041 C15 C054 120.7(8) . . ? C049 C15 C054 118.2(9) . . ? C3 C4 C046 120.6(9) . . ? C045 C2 C043 119.2(8) . . ? C045 C2 C055 121.3(7) . . ? C043 C2 C055 119.4(8) . . ? C12 C13 C14 118.4(8) . . ? C12 C13 C054 120.5(8) . . ? C14 C13 C054 121.0(8) . . ? C13 C12 C11 121.8(8) . . ? C049 C18 C17 119.4(8) . . ? C049 C18 C052 121.2(8) . . ? C17 C18 C052 119.3(8) . . ? C9 C14 C13 120.4(8) . . ? C056 O13 Co4 138.7(6) . . ? C4 C3 C043 121.7(8) . . ? C4 C3 C053 119.4(8) . . ? C043 C3 C053 118.9(8) . . ? C059 O6 Co3 137.3(6) . 2_665 ? C087 N5 C086 119.7(11) . . ? C087 N5 Co3 122.3(8) . . ? C086 N5 Co3 117.8(9) . . ? C16 C041 C15 121.1(8) . . ? C8 C042 C051 117.4(8) . . ? C8 C042 C059 121.1(8) . . ? C051 C042 C059 121.5(7) . . ? C3 C043 C2 118.2(9) . . ? C046 C044 C5 116.1(8) . . ? C046 C045 C2 122.5(8) . . ? C045 C046 C4 117.8(8) . . ? C045 C046 C044 121.7(8) . . ? C4 C046 C044 120.5(9) . . ? C083 N4 C079 115.1(11) . . ? C083 N4 Co4 126.8(9) . . ? C079 N4 Co4 118.1(8) . . ? C055 O2 Co1 139.6(6) . . ? C15 C049 C18 119.1(9) . . ? C090 N2 C082 116.0(13) . . ? C090 N2 Co1 122.5(10) . . ? C082 N2 Co1 120.6(9) . . ? C042 C051 C5 123.6(8) . . ? O17 C052 O16 126.0(8) . . ? O17 C052 C18 119.2(8) . . ? O16 C052 C18 114.8(8) . . ? O4 C053 O5 124.4(8) . . ? O4 C053 C3 117.5(8) . . ? O5 C053 C3 118.1(8) . . ? C13 C054 C15 109.6(7) . . ? O2 C055 O3 123.6(9) . . ? O2 C055 C2 116.9(8) . . ? O3 C055 C2 119.5(8) . . ? O13 C056 O12 126.0(9) . . ? O13 C056 C11 116.0(8) . . ? O12 C056 C11 118.1(8) . . ? O8 C057 O9 126.6(8) . . ? O8 C057 C7 115.6(8) . . ? O9 C057 C7 117.8(9) . . ? O11 C058 O10 126.1(8) . . ? O11 C058 C9 117.8(8) . . ? O10 C058 C9 116.0(8) . . ? O7 C059 O6 128.7(9) . . ? O7 C059 C042 116.0(8) . . ? O6 C059 C042 115.2(8) . . ? O15 C060 O14 127.7(8) . . ? O15 C060 C16 117.4(8) . . ? O14 C060 C16 115.0(8) . . ? C067 N1 C084 118.3(11) . . ? C067 N1 Co2 122.1(8) . . ? C084 N1 Co2 119.6(9) . . ? C073 N3 C077 114.1(11) . . ? C073 N3 Co4 121.8(9) . . ? C077 N3 Co4 123.3(8) . . ? C082 C063 C072 120.1(16) . . ? C086 C066 C64 118.4(17) . . ? N1 C067 C068 128.6(14) . . ? C067 C068 C095 112.7(16) . . ? C063 C072 C094 119.6(18) . . ? N3 C073 C091 121.4(15) . . ? C077 C074 C096 122.6(19) . . ? C092 C076 C083 119.7(16) . . ? C074 C077 N3 123.2(14) . . ? N4 C079 C089 125.8(14) . . ? C063 C082 N2 123.3(14) . . ? N4 C083 C076 122.1(14) . . ? N1 C084 C085 123.0(15) . . ? C084 C085 C095 116.4(17) . . ? C066 C086 N5 119.8(15) . . ? N5 C087 C1 121.9(12) . . ? C092 C089 C079 115.4(16) . . ? N2 C090 C094 125.7(15) . . ? C096 C091 C073 115(2) . . ? C076 C092 C089 121.9(18) . . ? C090 C094 C072 114.4(16) . . ? C068 C095 C085 120.8(18) . . ? C074 C096 C091 123(2) . . ? C24 C23 C22 120.0 . . ? C23 C24 N6 120.0 . . ? C20 N6 C24 120.0 . . ? C20 N6 Co3 119.1(6) . . ? C24 N6 Co3 120.7(6) . . ? N6 C20 C21 120.0 . . ? C22 C21 C20 120.0 . . ? C21 C22 C23 120.0 . . ? C64 C1 C087 118.4(14) . . ? C1 C64 C066 120.1(16) . . ? C32 C30 C35 120.0 . . ? C30 C32 C31 120.0 . . ? C33 C31 C32 120.0 . . ? C31 C33 N8 120.0 . . ? C35 N8 C33 120.0 . . ? C35 N8 Co2 121.2(4) . . ? C33 N8 Co2 118.8(4) . . ? N8 C35 C30 120.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.910 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.134 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 -0.020 1995 250 ' ' _platon_squeeze_details ; ;