# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Miguel Julve' _publ_contact_author_email JULVE@UV.ES _publ_section_title ; Novel cobalt(II) coordination polymers based on 1,2,4,5-bezenetetracarboxylic acid and extended bidentate ligands ; loop_ _publ_author_name 'Miguel Julve' 'Laura Canadillas-Delgado' 'Fernando S Delgado' 'Oscar Fabelo' 'Francesc Lloret' ; J.Pasan ; 'Catalina Ruiz-Perez' 'Consuelo Yuste' # Attachment 'Compounds_1_to_4_new.cif' data_Compound-1 _database_code_depnum_ccdc_archive 'CCDC 728516' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H11 Co N2 O5' _chemical_formula_weight 358.19 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' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0891(12) _cell_length_b 9.4027(9) _cell_length_c 10.1213(11) _cell_angle_alpha 114.699(11) _cell_angle_beta 103.187(9) _cell_angle_gamma 101.465(9) _cell_volume 642.21(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Pink _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.852 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 364 _exptl_absorpt_coefficient_mu 1.367 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6296 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0778 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 6.42 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2857 _reflns_number_gt 2133 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_cell_refinement ? _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0166P)^2^+0.4801P] 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 2857 _refine_ls_number_parameters 216 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.0811 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _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 0.13295(6) 0.15190(6) 0.46433(5) 0.01587(14) Uani 1 1 d . . . C1 C -0.1171(4) 0.4870(4) 0.8655(3) 0.0145(7) Uani 1 1 d . . . C2 C -0.0318(4) 0.3695(4) 0.8521(3) 0.0153(7) Uani 1 1 d . . . C3 C 0.0816(4) 0.3851(4) 0.9866(3) 0.0166(7) Uani 1 1 d . . . C4 C -0.2544(4) 0.4791(4) 0.7313(4) 0.0178(7) Uani 1 1 d . . . C5 C -0.0413(4) 0.2309(4) 0.7019(3) 0.0180(7) Uani 1 1 d . . . C6 C -0.1029(5) 0.0476(5) 0.1382(4) 0.0269(8) Uani 1 1 d . . . C7 C -0.2227(5) 0.0417(5) 0.0143(4) 0.0290(9) Uani 1 1 d . . . C8 C -0.3057(4) 0.1610(4) 0.0381(4) 0.0186(7) Uani 1 1 d . . . C9 C -0.2635(5) 0.2783(5) 0.1915(4) 0.0303(9) Uani 1 1 d . . . C10 C -0.1439(5) 0.2743(5) 0.3101(4) 0.0303(9) Uani 1 1 d . . . C11 C -0.6246(5) 0.2739(4) -0.2044(4) 0.0267(8) Uani 1 1 d . . . C12 C -0.5076(5) 0.2829(4) -0.0765(4) 0.0266(8) Uani 1 1 d . . . C13 C -0.4330(4) 0.1585(4) -0.0953(4) 0.0191(8) Uani 1 1 d . . . C14 C -0.4848(5) 0.0305(4) -0.2455(4) 0.0240(8) Uani 1 1 d . . . C15 C -0.6058(4) 0.0287(5) -0.3661(4) 0.0235(8) Uani 1 1 d . . . N1 N -0.0609(3) 0.1610(4) 0.2859(3) 0.0191(6) Uani 1 1 d . . . N2 N -0.6779(4) 0.1486(3) -0.3480(3) 0.0194(6) Uani 1 1 d . . . O1 O -0.2879(3) 0.6106(3) 0.7543(3) 0.0339(6) Uani 1 1 d . . . O2 O -0.3281(3) 0.3434(3) 0.6100(2) 0.0264(6) Uani 1 1 d . . . O3 O 0.0201(3) 0.2708(3) 0.6139(2) 0.0229(5) Uani 1 1 d . . . O4 O -0.0946(3) 0.0861(3) 0.6812(2) 0.0230(5) Uani 1 1 d . . . O1W O 0.3356(4) 0.2966(3) 0.4549(3) 0.0330(7) Uani 1 1 d . . . H1WA H 0.328(5) 0.330(5) 0.399(4) 0.033(12) Uiso 1 1 d . . . H1WB H 0.445(6) 0.319(5) 0.506(4) 0.035(12) Uiso 1 1 d . . . H3 H 0.1371 0.3054 0.9772 0.020 Uiso 1 1 calc R . . H6 H -0.0471 -0.0328 0.1178 0.032 Uiso 1 1 calc R . . H7 H -0.2482 -0.0425 -0.0858 0.035 Uiso 1 1 calc R . . H9 H -0.3165 0.3607 0.2147 0.036 Uiso 1 1 calc R . . H10 H -0.1199 0.3542 0.4117 0.036 Uiso 1 1 calc R . . H11 H -0.6692 0.3612 -0.1893 0.032 Uiso 1 1 calc R . . H12 H -0.4790 0.3719 0.0217 0.032 Uiso 1 1 calc R . . H14 H -0.4370 -0.0553 -0.2649 0.029 Uiso 1 1 calc R . . H15 H -0.6392 -0.0602 -0.4653 0.028 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 0.0181(2) 0.0163(3) 0.0115(2) 0.00561(18) 0.00324(17) 0.00697(18) C1 0.0160(16) 0.0154(18) 0.0102(15) 0.0052(14) 0.0032(13) 0.0052(13) C2 0.0175(16) 0.0145(18) 0.0092(15) 0.0033(14) 0.0024(13) 0.0042(13) C3 0.0175(16) 0.0197(19) 0.0142(16) 0.0075(14) 0.0043(13) 0.0129(14) C4 0.0184(17) 0.026(2) 0.0128(16) 0.0115(16) 0.0068(14) 0.0092(15) C5 0.0170(16) 0.021(2) 0.0081(15) 0.0024(14) -0.0032(13) 0.0101(14) C6 0.031(2) 0.033(2) 0.0198(19) 0.0122(17) 0.0059(16) 0.0208(18) C7 0.034(2) 0.034(2) 0.0145(18) 0.0064(17) 0.0039(16) 0.0192(18) C8 0.0181(17) 0.021(2) 0.0156(17) 0.0105(16) 0.0021(14) 0.0063(15) C9 0.044(2) 0.025(2) 0.0175(18) 0.0052(17) 0.0042(17) 0.0232(19) C10 0.041(2) 0.029(2) 0.0151(18) 0.0070(17) 0.0005(16) 0.0186(19) C11 0.033(2) 0.019(2) 0.0214(19) 0.0063(17) 0.0003(16) 0.0126(16) C12 0.036(2) 0.019(2) 0.0132(17) 0.0020(15) -0.0021(15) 0.0127(17) C13 0.0153(17) 0.022(2) 0.0178(17) 0.0100(16) 0.0028(14) 0.0048(15) C14 0.0288(19) 0.027(2) 0.0202(18) 0.0113(17) 0.0064(16) 0.0195(17) C15 0.0240(19) 0.028(2) 0.0140(17) 0.0046(16) 0.0042(15) 0.0141(17) N1 0.0184(15) 0.0219(17) 0.0138(14) 0.0077(13) 0.0018(12) 0.0071(13) N2 0.0219(15) 0.0221(17) 0.0162(15) 0.0112(14) 0.0054(12) 0.0081(13) O1 0.0526(17) 0.0272(16) 0.0201(13) 0.0113(12) 0.0014(12) 0.0232(13) O2 0.0269(13) 0.0247(15) 0.0137(12) 0.0015(11) -0.0039(10) 0.0117(11) O3 0.0312(13) 0.0285(15) 0.0145(11) 0.0102(11) 0.0093(10) 0.0196(11) O4 0.0303(13) 0.0145(14) 0.0160(12) 0.0032(10) 0.0008(10) 0.0092(11) O1W 0.0204(15) 0.0453(19) 0.0383(16) 0.0329(15) -0.0003(13) 0.0045(12) _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 N1 2.149(3) . ? Co1 N2 2.166(3) 1_656 ? Co1 O1W 1.959(3) . ? Co1 O3 1.999(2) . ? Co1 O4 2.009(2) 2_556 ? C1 C3 1.390(4) 2_567 ? C1 C4 1.510(4) . ? C2 C1 1.391(4) . ? C2 C5 1.505(4) . ? C3 C1 1.390(4) 2_567 ? C3 C2 1.388(4) . ? C4 O1 1.257(4) . ? C4 O2 1.243(4) . ? C6 C7 1.372(4) . ? C7 C8 1.383(4) . ? C9 C8 1.386(4) . ? C10 C9 1.378(4) . ? C11 C12 1.377(4) . ? C12 C13 1.384(5) . ? C13 C8 1.488(4) . ? C14 C13 1.384(4) . ? C15 C14 1.371(4) . ? N1 C10 1.337(4) . ? N1 C6 1.334(4) . ? N2 C11 1.330(4) . ? N2 C15 1.335(4) . ? N2 Co1 2.166(3) 1_454 ? O3 C5 1.261(4) . ? O4 C5 1.253(4) . ? O4 Co1 2.009(2) 2_556 ? 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 C1 C2 C5 125.5(3) . . ? C2 C1 C4 124.3(3) . . ? C2 C3 C1 123.7(3) . 2_567 ? C3 C1 C2 117.8(3) 2_567 . ? C3 C1 C4 117.7(3) 2_567 . ? C3 C2 C1 118.4(3) . . ? C3 C2 C5 115.9(3) . . ? C5 O3 Co1 129.5(2) . . ? C5 O4 Co1 143.4(2) . 2_556 ? C6 C7 C8 120.0(3) . . ? C6 N1 C10 116.0(3) . . ? C6 N1 Co1 119.0(2) . . ? C7 C8 C13 120.7(3) . . ? C7 C8 C9 115.8(3) . . ? C9 C8 C13 123.5(3) . . ? C10 C9 C8 120.8(3) . . ? C10 N1 Co1 125.1(2) . . ? C11 C12 C13 119.5(3) . . ? C11 N2 C15 116.2(3) . . ? C11 N2 Co1 119.5(2) . 1_454 ? C12 C13 C8 122.1(3) . . ? C14 C13 C12 116.1(3) . . ? C14 C13 C8 121.8(3) . . ? C15 C14 C13 120.7(3) . . ? C15 N2 Co1 124.3(2) . 1_454 ? N1 C10 C9 123.0(3) . . ? N1 C6 C7 124.3(3) . . ? N1 Co1 N2 177.21(11) . 1_656 ? N2 C11 C12 124.3(3) . . ? N2 C15 C14 123.2(3) . . ? O1 C4 C1 116.5(3) . . ? O2 C4 C1 117.8(3) . . ? O2 C4 O1 125.7(3) . . ? O3 C5 C2 117.3(3) . . ? O3 Co1 N1 88.50(9) . . ? O3 Co1 N2 88.72(9) . 1_656 ? O3 Co1 O4 135.85(10) . 2_556 ? O4 C5 C2 117.2(3) . . ? O4 C5 O3 125.2(3) . . ? O4 Co1 N1 90.35(10) 2_556 . ? O4 Co1 N2 91.58(10) 2_556 1_656 ? O1W Co1 N1 92.93(11) . . ? O1W Co1 N2 88.32(12) . 1_656 ? O1W Co1 O3 114.74(11) . . ? O1W Co1 O4 109.40(11) . 2_556 ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.412 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.098 data_Compound-2 _database_code_depnum_ccdc_archive 'CCDC 728517' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H28 Co N4 O10' _chemical_formula_weight 711.54 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0734(4) _cell_length_b 9.5955(7) _cell_length_c 10.1366(7) _cell_angle_alpha 93.025(6) _cell_angle_beta 113.334(5) _cell_angle_gamma 106.250(4) _cell_volume 764.46(8) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prismatic _exptl_crystal_colour orange-pink _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 367 _exptl_absorpt_coefficient_mu 0.631 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6600 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 5.05 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3479 _reflns_number_gt 2686 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_cell_refinement ? _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0314P)^2^+0.3629P] 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 3479 _refine_ls_number_parameters 239 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.0891 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 0.0000 0.0000 0.01536(13) Uani 1 2 d S . . C1 C 0.4849(3) 0.3606(2) -0.0637(2) 0.0181(4) Uani 1 1 d . . . C2 C 0.3435(3) 0.3855(2) -0.0570(2) 0.0165(4) Uani 1 1 d . . . C3 C 0.3603(3) 0.5251(2) 0.0049(2) 0.0201(5) Uani 1 1 d . . . C4 C 0.4803(3) 0.2151(2) -0.1327(3) 0.0228(5) Uani 1 1 d . . . C5 C 0.1766(3) 0.2648(2) -0.0988(2) 0.0171(4) Uani 1 1 d . . . C6 C 0.0342(3) 0.1149(2) 0.3000(3) 0.0285(5) Uani 1 1 d . . . C7 C 0.0432(3) 0.2073(2) 0.4138(3) 0.0299(5) Uani 1 1 d . . . C8 C 0.0278(3) 0.3457(2) 0.3934(2) 0.0240(5) Uani 1 1 d . . . C9 C 0.0132(3) 0.3856(2) 0.2611(3) 0.0286(5) Uani 1 1 d . . . C10 C 0.0098(3) 0.2878(2) 0.1552(3) 0.0269(5) Uani 1 1 d . . . C11 C 0.0232(3) 0.4402(2) 0.5095(3) 0.0294(5) Uani 1 1 d . . . C12 C 0.6612(4) 0.1241(3) 0.4899(3) 0.0385(6) Uani 1 1 d . . . C13 C 0.6301(4) 0.2377(3) 0.5494(3) 0.0418(7) Uani 1 1 d . . . C14 C 0.5589(3) 0.3282(2) 0.4627(3) 0.0311(6) Uani 1 1 d . . . C15 C 0.5228(4) 0.2986(3) 0.3163(3) 0.0455(7) Uani 1 1 d . . . C16 C 0.5576(4) 0.1819(3) 0.2640(3) 0.0424(7) Uani 1 1 d . . . C17 C 0.5251(4) 0.4487(3) 0.5304(3) 0.0405(6) Uani 1 1 d . . . N1 N 0.0176(2) 0.15246(18) 0.1716(2) 0.0221(4) Uani 1 1 d . . . N2 N 0.6258(3) 0.0967(2) 0.3494(2) 0.0285(5) Uani 1 1 d . . . O1 O 0.6054(2) 0.1765(2) -0.0795(2) 0.0528(6) Uani 1 1 d . . . O2 O 0.3445(2) 0.14278(18) -0.24509(19) 0.0328(4) Uani 1 1 d . . . O3 O 0.18625(18) 0.15926(14) -0.03143(16) 0.0223(3) Uani 1 1 d . . . O4 O 0.0439(2) 0.28233(16) -0.18692(19) 0.0320(4) Uani 1 1 d . . . O1W O 0.1902(2) -0.06512(17) 0.15993(18) 0.0236(4) Uani 1 1 d . . . H1WA H 0.254(4) -0.088(3) 0.135(3) 0.035(8) Uiso 1 1 d . . . H1WB H 0.125(4) -0.141(3) 0.175(3) 0.058(9) Uiso 1 1 d . . . H2A H 0.355(6) 0.067(6) -0.278(6) 0.028(13) Uiso 0.50 1 d P . . H2B H 0.635(5) 0.023(6) 0.319(5) 0.013(11) Uiso 0.50 1 d P . . H3 H 0.2654 0.5426 0.0070 0.024 Uiso 1 1 calc R . . H6 H 0.0400 0.0211 0.3137 0.034 Uiso 1 1 calc R . . H7 H 0.0594 0.1776 0.5030 0.036 Uiso 1 1 calc R . . H9 H 0.0056 0.4782 0.2437 0.034 Uiso 1 1 calc R . . H10 H 0.0017 0.3174 0.0673 0.032 Uiso 1 1 calc R . . H11 H 0.0546 0.4148 0.6016 0.035 Uiso 1 1 calc R . . H12 H 0.7090 0.0638 0.5503 0.046 Uiso 1 1 calc R . . H13 H 0.6571 0.2537 0.6488 0.050 Uiso 1 1 calc R . . H15 H 0.4752 0.3571 0.2533 0.055 Uiso 1 1 calc R . . H16 H 0.5320 0.1627 0.1651 0.051 Uiso 1 1 calc R . . H17 H 0.5421 0.4504 0.6272 0.049 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 0.0199(2) 0.0111(2) 0.0177(2) 0.00164(15) 0.01047(19) 0.00549(16) C1 0.0241(11) 0.0142(10) 0.0207(11) 0.0037(8) 0.0125(10) 0.0088(8) C2 0.0205(11) 0.0147(10) 0.0174(11) 0.0048(8) 0.0105(9) 0.0066(8) C3 0.0216(11) 0.0189(10) 0.0265(12) 0.0046(9) 0.0150(10) 0.0093(8) C4 0.0262(12) 0.0150(10) 0.0320(14) 0.0017(9) 0.0177(11) 0.0066(9) C5 0.0228(11) 0.0133(9) 0.0191(11) 0.0022(8) 0.0129(10) 0.0060(8) C6 0.0436(15) 0.0202(11) 0.0304(14) 0.0060(10) 0.0203(12) 0.0164(10) C7 0.0479(15) 0.0282(12) 0.0233(13) 0.0089(10) 0.0202(12) 0.0186(11) C8 0.0310(13) 0.0216(11) 0.0211(12) -0.0003(9) 0.0128(10) 0.0096(9) C9 0.0471(15) 0.0186(11) 0.0282(13) 0.0050(9) 0.0206(12) 0.0158(10) C10 0.0422(14) 0.0222(11) 0.0219(12) 0.0037(9) 0.0167(11) 0.0145(10) C11 0.0433(15) 0.0271(12) 0.0223(12) 0.0008(10) 0.0176(12) 0.0134(11) C12 0.0544(17) 0.0355(14) 0.0308(15) 0.0045(11) 0.0154(13) 0.0267(12) C13 0.0637(19) 0.0431(15) 0.0301(15) 0.0055(12) 0.0218(14) 0.0319(14) C14 0.0339(14) 0.0242(12) 0.0337(14) -0.0020(10) 0.0126(12) 0.0117(10) C15 0.066(2) 0.0351(14) 0.0366(16) 0.0085(12) 0.0124(15) 0.0319(14) C16 0.0644(19) 0.0362(14) 0.0265(14) 0.0021(11) 0.0152(14) 0.0233(13) C17 0.0493(17) 0.0370(15) 0.0380(16) 0.0030(11) 0.0167(14) 0.0220(12) N1 0.0305(11) 0.0172(9) 0.0228(10) 0.0018(7) 0.0146(9) 0.0097(8) N2 0.0330(12) 0.0210(10) 0.0312(12) -0.0034(9) 0.0126(10) 0.0112(9) O1 0.0334(10) 0.0407(10) 0.0718(15) -0.0200(10) 0.0064(10) 0.0234(9) O2 0.0347(10) 0.0246(9) 0.0341(10) -0.0094(7) 0.0091(8) 0.0136(8) O3 0.0218(8) 0.0167(7) 0.0296(9) 0.0084(6) 0.0122(7) 0.0056(6) O4 0.0215(9) 0.0280(8) 0.0405(10) 0.0176(7) 0.0080(8) 0.0053(7) O1W 0.0227(9) 0.0231(8) 0.0291(9) 0.0067(7) 0.0133(8) 0.0099(7) _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 N1 2.1377(16) . ? Co1 N1 2.1377(16) 2 ? Co1 O1W 2.1195(16) . ? Co1 O1W 2.1195(16) 2 ? Co1 O3 2.0797(13) . ? Co1 O3 2.0797(13) 2 ? C1 C3 1.392(3) 2_665 ? C1 C4 1.510(3) . ? C2 C1 1.394(3) . ? C2 C5 1.507(3) . ? C3 C1 1.392(3) 2_665 ? C3 C2 1.391(3) . ? C4 O1 1.221(3) . ? C4 O2 1.275(3) . ? C5 O3 1.255(2) . ? C5 O4 1.247(3) . ? C6 C7 1.379(3) . ? C7 C8 1.391(3) . ? C8 C11 1.469(3) . ? C8 C9 1.380(3) . ? C10 C9 1.374(3) . ? C11 C11 1.326(4) 2_566 ? C12 C13 1.367(3) . ? C14 C13 1.375(4) . ? C14 C15 1.381(4) . ? C14 C17 1.477(3) . ? C15 C16 1.380(3) . ? C17 C17 1.285(5) 2_666 ? N1 C10 1.336(3) . ? N1 C6 1.331(3) . ? N2 C12 1.324(3) . ? N2 C16 1.317(3) . ? 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 C1 C2 C5 123.42(16) . . ? C2 C1 C4 123.58(18) . . ? C2 C3 C1 121.84(19) . 2_665 ? C3 C1 C2 119.18(17) 2_665 . ? C3 C1 C4 117.24(18) 2_665 . ? C3 C2 C1 118.97(18) . . ? C3 C2 C5 117.29(17) . . ? C5 O3 Co1 130.48(14) . . ? C6 C7 C8 119.1(2) . . ? C6 N1 C10 116.85(17) . . ? C6 N1 Co1 120.90(13) . . ? C7 C8 C11 119.5(2) . . ? C9 C8 C11 123.1(2) . . ? C9 C8 C7 117.36(19) . . ? C10 C9 C8 119.6(2) . . ? C10 N1 Co1 122.24(15) . . ? C11 C11 C8 123.8(3) 2_566 . ? C12 C13 C14 120.1(2) . . ? C13 C14 C15 116.9(2) . . ? C13 C14 C17 118.6(2) . . ? C15 C14 C17 124.5(2) . . ? C16 C15 C14 119.8(3) . . ? C16 N2 C12 118.7(2) . . ? C17 C17 C14 126.8(3) 2_666 . ? N1 C10 C9 123.5(2) . . ? N1 C6 C7 123.6(2) . . ? N1 Co1 N1 180.00(9) 2 . ? N2 C12 C13 122.4(3) . . ? N2 C16 C15 122.2(2) . . ? O1 C4 C1 118.61(19) . . ? O1 C4 O2 124.89(19) . . ? O2 C4 C1 116.5(2) . . ? O3 C5 C2 114.82(19) . . ? O3 Co1 N1 89.13(6) . 2 ? O3 Co1 N1 89.13(6) 2 . ? O3 Co1 N1 90.87(6) . . ? O3 Co1 N1 90.87(6) 2 2 ? O3 Co1 O1W 89.93(6) . 2 ? O3 Co1 O1W 89.93(6) 2 . ? O3 Co1 O1W 90.07(6) . . ? O3 Co1 O1W 90.07(6) 2 2 ? O3 Co1 O3 180.00(9) 2 . ? O4 C5 C2 118.58(18) . . ? O4 C5 O3 126.40(19) . . ? O1W Co1 N1 88.19(7) . . ? O1W Co1 N1 88.19(7) 2 2 ? O1W Co1 N1 91.81(7) . 2 ? O1W Co1 N1 91.81(7) 2 . ? O1W Co1 O1W 180.00(11) . 2 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.525 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.066 data_Compound-3 _database_code_depnum_ccdc_archive 'CCDC 728518' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H24 Co N8 O10' _chemical_formula_weight 715.50 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' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9901(14) _cell_length_b 9.5945(9) _cell_length_c 10.2763(12) _cell_angle_alpha 96.211(7) _cell_angle_beta 114.225(12) _cell_angle_gamma 105.727(12) _cell_volume 753.37(16) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour orange-pink _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 367 _exptl_absorpt_coefficient_mu 0.644 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13601 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 6.42 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3409 _reflns_number_gt 2883 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_cell_refinement ? _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0378P)^2^+0.6423P] 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 3409 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1035 _refine_ls_wR_factor_gt 0.0979 _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 0.0000 0.0000 0.0000 0.02000(13) Uani 1 2 d S . . C1 C 0.4781(3) 0.3548(2) -0.0621(2) 0.0238(5) Uani 1 1 d . . . C2 C 0.3394(3) 0.3848(2) -0.0523(2) 0.0231(4) Uani 1 1 d . . . C3 C 0.3629(3) 0.5303(2) 0.0085(3) 0.0254(5) Uani 1 1 d . . . C4 C 0.4675(3) 0.2037(2) -0.1295(3) 0.0279(5) Uani 1 1 d . . . C5 C 0.1694(3) 0.2644(2) -0.0897(2) 0.0239(4) Uani 1 1 d . . . C6 C 0.0517(4) 0.1327(3) 0.3067(3) 0.0340(6) Uani 1 1 d . . . C7 C 0.0613(4) 0.2286(3) 0.4226(3) 0.0349(6) Uani 1 1 d . . . C8 C 0.0339(3) 0.3609(3) 0.4003(3) 0.0292(5) Uani 1 1 d . . . C9 C 0.0076(3) 0.3962(3) 0.2683(3) 0.0312(5) Uani 1 1 d . . . C10 C 0.0056(3) 0.2951(3) 0.1610(3) 0.0305(5) Uani 1 1 d . . . C11 C 0.6645(4) 0.1433(3) 0.4970(3) 0.0487(7) Uani 1 1 d . . . C12 C 0.6255(5) 0.2561(4) 0.5545(3) 0.0532(8) Uani 1 1 d . . . C13 C 0.5603(4) 0.3442(3) 0.4670(3) 0.0411(6) Uani 1 1 d . . . C14 C 0.5366(4) 0.3172(3) 0.3240(3) 0.0481(7) Uani 1 1 d . . . C15 C 0.5773(4) 0.2007(3) 0.2749(3) 0.0443(7) Uani 1 1 d . . . H2 H 0.334(5) 0.023(5) -0.292(5) 0.089(13) Uiso 1 1 d . . . H3 H 0.2700 0.5513 0.0135 0.030 Uiso 1 1 calc R . . H6 H 0.0648 0.0415 0.3195 0.041 Uiso 1 1 calc R . . H7 H 0.0855 0.2049 0.5128 0.042 Uiso 1 1 calc R . . H9 H -0.0085 0.4856 0.2518 0.037 Uiso 1 1 calc R . . H10 H -0.0098 0.3195 0.0723 0.037 Uiso 1 1 calc R . . H11 H 0.7095 0.0840 0.5571 0.058 Uiso 1 1 calc R . . H12 H 0.6432 0.2723 0.6514 0.064 Uiso 1 1 calc R . . H14 H 0.4942 0.3763 0.2624 0.058 Uiso 1 1 calc R . . H15 H 0.5595 0.1811 0.1780 0.053 Uiso 1 1 calc R . . H1WA H 0.262(5) -0.076(4) 0.131(4) 0.057(11) Uiso 1 1 d . . . H1WB H 0.141(5) -0.133(4) 0.171(4) 0.061(11) Uiso 1 1 d . . . N1 N 0.0247(3) 0.1639(2) 0.1779(2) 0.0278(4) Uani 1 1 d . . . N2 N 0.0366(3) 0.4546(2) 0.5198(2) 0.0350(5) Uani 1 1 d . . . N3 N 0.6407(3) 0.1153(2) 0.3592(2) 0.0354(5) Uani 1 1 d . . . N4 N 0.5235(4) 0.4600(3) 0.5388(3) 0.0505(6) Uani 1 1 d . . . O1 O 0.5884(3) 0.1602(2) -0.0734(2) 0.0497(5) Uani 1 1 d . . . O2 O 0.3261(2) 0.12853(19) -0.2502(2) 0.0390(4) Uani 1 1 d . . . O3 O 0.1831(2) 0.15663(17) -0.03236(18) 0.0275(4) Uani 1 1 d . . . O4 O 0.0319(2) 0.2853(2) -0.1647(2) 0.0394(4) Uani 1 1 d . . . O1W O 0.1999(2) -0.05470(19) 0.1591(2) 0.0291(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0225(2) 0.0134(2) 0.0248(2) 0.00091(15) 0.01273(18) 0.00560(16) C1 0.0275(11) 0.0159(9) 0.0299(12) 0.0032(8) 0.0158(9) 0.0073(8) C2 0.0255(11) 0.0182(10) 0.0277(11) 0.0042(8) 0.0150(9) 0.0069(8) C3 0.0264(11) 0.0200(10) 0.0343(12) 0.0037(9) 0.0182(10) 0.0092(9) C4 0.0282(12) 0.0198(10) 0.0387(13) 0.0019(9) 0.0195(10) 0.0085(9) C5 0.0254(11) 0.0186(10) 0.0268(11) 0.0015(8) 0.0135(9) 0.0056(8) C6 0.0489(15) 0.0257(12) 0.0351(13) 0.0066(10) 0.0226(12) 0.0195(11) C7 0.0513(16) 0.0327(13) 0.0282(12) 0.0079(10) 0.0215(12) 0.0204(12) C8 0.0341(12) 0.0251(11) 0.0280(12) -0.0016(9) 0.0156(10) 0.0108(10) C9 0.0434(14) 0.0221(11) 0.0306(12) 0.0030(9) 0.0181(11) 0.0145(10) C10 0.0420(14) 0.0248(11) 0.0287(12) 0.0042(9) 0.0190(11) 0.0141(10) C11 0.067(2) 0.0423(16) 0.0394(16) 0.0065(12) 0.0196(14) 0.0319(15) C12 0.080(2) 0.0481(17) 0.0422(16) 0.0060(14) 0.0323(16) 0.0335(17) C13 0.0378(14) 0.0315(13) 0.0496(16) -0.0048(12) 0.0187(13) 0.0138(11) C14 0.0583(18) 0.0360(14) 0.0466(17) 0.0083(13) 0.0152(14) 0.0264(14) C15 0.0569(18) 0.0369(14) 0.0350(14) 0.0010(11) 0.0175(13) 0.0191(13) N1 0.0323(10) 0.0223(9) 0.0293(10) -0.0006(8) 0.0163(9) 0.0096(8) N2 0.0486(13) 0.0311(11) 0.0291(11) 0.0001(9) 0.0199(10) 0.0188(9) N3 0.0351(11) 0.0279(10) 0.0385(12) -0.0026(9) 0.0140(10) 0.0129(9) N4 0.0588(16) 0.0442(14) 0.0497(15) 0.0071(11) 0.0233(13) 0.0241(12) O1 0.0384(10) 0.0335(10) 0.0639(13) -0.0093(9) 0.0116(10) 0.0205(9) O2 0.0383(10) 0.0264(9) 0.0428(11) -0.0069(8) 0.0126(8) 0.0128(8) O3 0.0257(8) 0.0202(7) 0.0384(9) 0.0089(7) 0.0170(7) 0.0067(6) O4 0.0254(9) 0.0348(9) 0.0549(12) 0.0221(9) 0.0141(8) 0.0088(7) O1W 0.0261(9) 0.0258(9) 0.0363(10) 0.0052(7) 0.0152(8) 0.0098(7) _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 N1 2.1725(18) . ? Co1 N1 2.1725(18) 2 ? Co1 O1W 2.1128(17) . ? Co1 O1W 2.1128(17) 2 ? Co1 O3 2.0727(15) . ? Co1 O3 2.0727(15) 2 ? C1 C3 1.389(3) 2_665 ? C1 C4 1.498(3) . ? C2 C1 1.393(3) . ? C2 C5 1.512(3) . ? C3 C1 1.389(3) 2_665 ? C3 C2 1.388(3) . ? C4 O1 1.213(3) . ? C4 O2 1.300(3) . ? C5 O3 1.254(3) . ? C5 O4 1.244(3) . ? C6 C7 1.382(3) . ? C6 N1 1.328(3) . ? C7 C8 1.382(3) . ? C8 N2 1.429(3) . ? C9 C8 1.375(3) . ? C10 C9 1.378(3) . ? C10 N1 1.335(3) . ? C11 C12 1.371(4) . ? C11 N3 1.327(4) . ? C12 C13 1.366(4) . ? C13 N4 1.453(3) . ? C14 C13 1.380(4) . ? C15 C14 1.374(4) . ? C15 N3 1.323(4) . ? N2 N2 1.234(4) 2_566 ? N4 N4 1.198(5) 2_666 ? 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 C1 C2 C5 123.26(19) . . ? C2 C1 C4 123.91(19) . . ? C2 C3 C1 121.6(2) . 2_665 ? C3 C1 C2 119.54(19) 2_665 . ? C3 C1 C4 116.55(19) 2_665 . ? C3 C2 C1 118.9(2) . . ? C3 C2 C5 117.51(19) . . ? C5 O3 Co1 129.37(14) . . ? C6 C7 C8 117.9(2) . . ? C6 N1 C10 117.6(2) . . ? C6 N1 Co1 120.13(15) . . ? C7 C8 N2 116.7(2) . . ? C8 C9 C10 118.1(2) . . ? C9 C8 C7 119.6(2) . . ? C9 C8 N2 123.8(2) . . ? C10 N1 Co1 122.24(16) . . ? C12 C13 C14 118.9(2) . . ? C12 C13 N4 114.4(3) . . ? C13 C12 C11 118.9(3) . . ? C14 C13 N4 126.7(3) . . ? C15 C14 C13 118.3(3) . . ? C15 N3 C11 118.1(2) . . ? N1 C10 C9 123.4(2) . . ? N1 C6 C7 123.4(2) . . ? N1 Co1 N1 180.00(10) . 2 ? N2 N2 C8 112.7(3) 2_566 . ? N3 C11 C12 122.8(3) . . ? N3 C15 C14 123.0(3) . . ? N4 N4 C13 112.1(3) 2_666 . ? O1 C4 C1 120.0(2) . . ? O1 C4 O2 124.1(2) . . ? O2 C4 C1 115.8(2) . . ? O3 C5 C2 115.27(19) . . ? O3 Co1 N1 88.52(7) . 2 ? O3 Co1 N1 88.52(7) 2 . ? O3 Co1 N1 91.48(7) . . ? O3 Co1 N1 91.48(7) 2 2 ? O3 Co1 O1W 89.80(7) . 2 ? O3 Co1 O1W 89.80(7) 2 . ? O3 Co1 O1W 90.20(7) . . ? O3 Co1 O1W 90.20(7) 2 2 ? O3 Co1 O3 180.00(8) . 2 ? O4 C5 C2 118.00(19) . . ? O4 C5 O3 126.6(2) . . ? O1W Co1 N1 88.06(7) . . ? O1W Co1 N1 88.06(7) 2 2 ? O1W Co1 N1 91.94(7) . 2 ? O1W Co1 N1 91.94(7) 2 . ? O1W Co1 O1W 180.00(15) 2 . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.964 _refine_diff_density_min -0.262 _refine_diff_density_rms 0.062 data_Compound-4 _database_code_depnum_ccdc_archive 'CCDC 728519' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H25 Co N2 O10' _chemical_formula_weight 476.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.3490 0.9720 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 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' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3705(10) _cell_length_b 11.4792(13) _cell_length_c 11.6886(9) _cell_angle_alpha 60.996(8) _cell_angle_beta 66.612(8) _cell_angle_gamma 66.832(8) _cell_volume 977.13(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Pink _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 0.939 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.9120 _exptl_absorpt_correction_T_max 0.9634 _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 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19033 _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4468 _reflns_number_gt 3187 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_cell_refinement 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1377P)^2^+1.1229P] 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 SHELXL _refine_ls_extinction_coef 0.023(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4468 _refine_ls_number_parameters 275 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1019 _refine_ls_R_factor_gt 0.0723 _refine_ls_wR_factor_ref 0.2283 _refine_ls_wR_factor_gt 0.2005 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 1.0000 0.0000 1.0000 0.0314(3) Uani 1 2 d S . . Co2 Co 0.5000 0.5000 0.5000 0.0274(3) Uani 1 2 d S . . C1 C 0.5998(5) 0.3778(4) 0.9856(4) 0.0248(8) Uani 1 1 d . . . C2 C 0.5287(5) 0.4829(4) 0.8818(4) 0.0242(8) Uani 1 1 d . . . C3 C 0.4292(5) 0.6036(4) 0.8980(4) 0.0264(9) Uani 1 1 d . . . C4 C 0.6932(5) 0.2389(4) 0.9778(4) 0.0270(9) Uani 1 1 d . . . C5 C 0.5786(5) 0.4729(4) 0.7453(4) 0.0264(9) Uani 1 1 d . . . C6 C 1.2441(6) 0.0612(5) 0.7263(5) 0.0410(11) Uani 1 1 d . . . C7 C 1.3075(6) 0.1110(5) 0.5875(5) 0.0395(11) Uani 1 1 d . . . C8 C 1.2092(6) 0.1853(5) 0.5008(5) 0.0370(11) Uani 1 1 d . . . C9 C 1.0457(6) 0.2144(5) 0.5616(5) 0.0403(11) Uani 1 1 d . . . C10 C 0.9895(6) 0.1638(5) 0.7005(5) 0.0379(11) Uani 1 1 d . . . C11 C 1.2716(7) 0.2250(5) 0.3519(5) 0.0453(12) Uani 1 1 d . . . C12 C 1.2139(7) 0.1589(5) 0.2971(5) 0.0465(13) Uani 1 1 d . . . C13 C 1.2792(6) 0.0053(5) 0.3440(5) 0.0387(11) Uani 1 1 d . . . C14 C 1.2289(6) -0.0841(5) 0.4768(5) 0.0392(11) Uani 1 1 d . . . C15 C 1.2955(6) -0.2233(5) 0.5151(5) 0.0364(10) Uani 1 1 d . . . C16 C 1.4546(6) -0.1961(5) 0.3011(5) 0.0365(10) Uani 1 1 d . . . C17 C 1.3951(6) -0.0554(5) 0.2551(5) 0.0384(11) Uani 1 1 d . . . O1 O 0.8315(4) 0.1900(3) 0.9975(3) 0.0356(8) Uani 1 1 d . . . O2 O 0.6252(4) 0.1809(3) 0.9556(4) 0.0407(8) Uani 1 1 d . . . O3 O 0.4697(4) 0.4952(3) 0.6950(3) 0.0337(7) Uani 1 1 d . . . O4 O 0.7259(4) 0.4469(4) 0.6916(3) 0.0386(8) Uani 1 1 d . . . O1W O 1.1702(4) 0.0650(4) 1.0165(4) 0.0466(9) Uani 1 1 d . . . O2W O 0.7369(4) 0.5155(4) 0.4382(3) 0.0435(9) Uani 1 1 d . . . O3W O 0.9944(5) 0.4071(5) 0.7704(4) 0.0641(12) Uani 1 1 d . . . O4W O 0.9483(10) 0.2108(9) 1.1685(9) 0.140(3) Uani 1 1 d . . . O5W O 1.2795(15) 0.2872(14) 0.9540(11) 0.203(5) Uani 1 1 d . . . O6W O 0.9070(16) 0.4659(9) 1.1346(11) 0.198(5) Uani 1 1 d . . . N1 N 1.0861(4) 0.0857(4) 0.7834(4) 0.0348(9) Uani 1 1 d . . . N2 N 1.4063(5) -0.2813(4) 0.4297(4) 0.0341(9) Uani 1 1 d . . . H3 H 0.3811 0.6732 0.8295 0.032 Uiso 1 1 calc R . . H6 H 1.3141 0.0086 0.7820 0.049 Uiso 1 1 calc R . . H7 H 1.4183 0.0938 0.5524 0.047 Uiso 1 1 calc R . . H9 H 0.9734 0.2685 0.5080 0.048 Uiso 1 1 calc R . . H10 H 0.8793 0.1851 0.7382 0.045 Uiso 1 1 calc R . . H11A H 1.3881 0.1985 0.3294 0.054 Uiso 1 1 calc R . . H11B H 1.2381 0.3243 0.3074 0.054 Uiso 1 1 calc R . . H12A H 1.0975 0.1798 0.3254 0.056 Uiso 1 1 calc R . . H12B H 1.2456 0.1995 0.1990 0.056 Uiso 1 1 calc R . . H14 H 1.1500 -0.0495 0.5396 0.047 Uiso 1 1 calc R . . H15 H 1.2618 -0.2803 0.6050 0.044 Uiso 1 1 calc R . . H16 H 1.5320 -0.2340 0.2401 0.044 Uiso 1 1 calc R . . H17 H 1.4319 -0.0007 0.1649 0.046 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 0.0298(5) 0.0344(5) 0.0290(5) -0.0172(4) -0.0106(3) 0.0021(3) Co2 0.0309(5) 0.0361(5) 0.0205(4) -0.0157(3) -0.0089(3) -0.0052(3) C1 0.025(2) 0.032(2) 0.0206(19) -0.0145(16) -0.0048(15) -0.0055(16) C2 0.028(2) 0.031(2) 0.0196(18) -0.0133(16) -0.0095(15) -0.0048(16) C3 0.030(2) 0.031(2) 0.0179(18) -0.0110(16) -0.0089(15) -0.0023(16) C4 0.031(2) 0.031(2) 0.0190(18) -0.0124(16) -0.0093(16) -0.0018(17) C5 0.037(2) 0.026(2) 0.0191(18) -0.0124(16) -0.0113(17) -0.0018(17) C6 0.035(2) 0.047(3) 0.041(3) -0.018(2) -0.015(2) -0.004(2) C7 0.034(2) 0.047(3) 0.039(3) -0.021(2) -0.006(2) -0.010(2) C8 0.049(3) 0.034(2) 0.034(2) -0.0172(19) -0.009(2) -0.013(2) C9 0.049(3) 0.036(3) 0.036(2) -0.017(2) -0.022(2) 0.004(2) C10 0.031(2) 0.045(3) 0.037(2) -0.021(2) -0.0101(19) -0.001(2) C11 0.060(3) 0.038(3) 0.034(3) -0.012(2) -0.011(2) -0.012(2) C12 0.066(3) 0.036(3) 0.034(3) -0.012(2) -0.023(2) -0.002(2) C13 0.049(3) 0.043(3) 0.034(2) -0.017(2) -0.020(2) -0.009(2) C14 0.040(3) 0.047(3) 0.035(2) -0.023(2) -0.009(2) -0.006(2) C15 0.038(2) 0.040(3) 0.030(2) -0.0107(19) -0.0105(19) -0.011(2) C16 0.044(3) 0.040(3) 0.029(2) -0.0167(19) -0.0114(19) -0.007(2) C17 0.048(3) 0.043(3) 0.030(2) -0.016(2) -0.013(2) -0.013(2) N1 0.033(2) 0.039(2) 0.0314(19) -0.0170(16) -0.0106(15) -0.0006(16) N2 0.038(2) 0.039(2) 0.032(2) -0.0165(16) -0.0136(16) -0.0077(17) O1 0.0366(17) 0.0369(18) 0.0398(18) -0.0246(15) -0.0177(14) 0.0051(14) O2 0.0420(18) 0.0419(19) 0.052(2) -0.0288(16) -0.0190(16) -0.0036(15) O3 0.0375(17) 0.0470(19) 0.0271(15) -0.0235(14) -0.0121(13) -0.0051(14) O4 0.0352(18) 0.058(2) 0.0249(16) -0.0240(15) -0.0077(13) -0.0041(15) O1W 0.043(2) 0.045(2) 0.062(2) -0.0290(18) -0.0203(17) -0.0034(16) O2W 0.0404(19) 0.068(2) 0.0284(17) -0.0203(16) -0.0081(14) -0.0183(17) O3W 0.065(3) 0.087(3) 0.049(2) -0.025(2) -0.008(2) -0.036(2) O4W 0.141(6) 0.169(7) 0.151(7) -0.094(6) -0.063(6) -0.010(6) O5W 0.253(12) 0.281(14) 0.139(8) -0.096(9) 0.008(8) -0.167(12) O6W 0.356(15) 0.120(7) 0.223(10) -0.069(7) -0.191(11) -0.039(8) _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 O2W Co2 2.096(3) . ? O1W Co1 2.112(4) . ? Co2 O2W 2.096(3) 2_666 ? Co2 N2 2.142(4) 1_465 ? Co2 N2 2.142(4) 2_756 ? Co2 O3 2.158(3) . ? Co2 O3 2.158(3) 2_666 ? Co1 O1W 2.112(4) 2_757 ? Co1 O1 2.125(3) . ? Co1 O1 2.125(3) 2_757 ? Co1 N1 2.149(4) . ? Co1 N1 2.149(4) 2_757 ? O2 C4 1.245(5) . ? O1 C4 1.260(5) . ? O3 C5 1.256(5) . ? O4 C5 1.249(5) . ? N1 C10 1.333(6) . ? N1 C6 1.336(6) . ? C2 C3 1.387(6) . ? C2 C1 1.401(5) . ? C2 C5 1.523(5) . ? C4 C1 1.515(6) . ? N2 C15 1.340(6) . ? N2 C16 1.343(6) . ? N2 Co2 2.142(4) 1_645 ? C3 C1 1.383(5) 2_667 ? C1 C3 1.383(5) 2_667 ? C14 C15 1.373(7) . ? C14 C13 1.393(7) . ? C13 C17 1.398(7) . ? C13 C12 1.505(7) . ? C17 C16 1.377(7) . ? C9 C10 1.378(7) . ? C9 C8 1.388(7) . ? C6 C7 1.383(7) . ? C7 C8 1.374(7) . ? C8 C11 1.487(7) . ? C12 C11 1.533(8) . ? 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 C1 C2 C5 120.1(4) . . ? C1 C3 C2 121.1(4) 2_667 . ? C2 C1 C4 120.4(3) . . ? C3 C1 C2 119.6(4) 2_667 . ? C3 C1 C4 119.7(4) 2_667 . ? C3 C2 C1 119.3(4) . . ? C3 C2 C5 120.0(3) . . ? C4 O1 Co1 130.1(3) . . ? C5 O3 Co2 127.0(3) . . ? C6 N1 Co1 119.6(3) . . ? C7 C8 C11 122.7(5) . . ? C7 C8 C9 115.7(4) . . ? C8 C11 C12 113.4(4) . . ? C8 C7 C6 121.0(5) . . ? C9 C8 C11 121.5(5) . . ? C10 C9 C8 120.6(4) . . ? C10 N1 C6 117.1(4) . . ? C10 N1 Co1 123.4(3) . . ? C13 C12 C11 113.6(4) . . ? C14 C13 C12 122.5(5) . . ? C14 C13 C17 116.3(5) . . ? C15 C14 C13 120.1(5) . . ? C15 N2 C16 116.9(4) . . ? C15 N2 Co2 120.3(3) . 1_645 ? C16 C17 C13 120.0(5) . . ? C16 N2 Co2 122.8(3) . 1_645 ? C17 C13 C12 121.2(5) . . ? N1 C10 C9 122.9(4) . . ? N1 C6 C7 122.5(4) . . ? N1 Co1 N1 180.0 . 2_757 ? N2 C15 C14 123.5(4) . . ? N2 C16 C17 123.1(4) . . ? N2 Co2 N2 180.000(1) 1_465 2_756 ? N2 Co2 O3 89.11(13) 1_465 . ? N2 Co2 O3 89.11(13) 2_756 2_666 ? N2 Co2 O3 90.89(13) 1_465 2_666 ? N2 Co2 O3 90.89(13) 2_756 . ? O1 C4 C1 117.5(4) . . ? O1 Co1 N1 88.93(13) . 2_757 ? O1 Co1 N1 88.93(13) 2_757 . ? O1 Co1 N1 91.07(13) . . ? O1 Co1 N1 91.07(13) 2_757 2_757 ? O1 Co1 O1 180.0(2) . 2_757 ? O2 C4 C1 117.2(4) . . ? O2 C4 O1 125.3(4) . . ? O3 C5 C2 118.0(4) . . ? O3 Co2 O3 180.00(18) . 2_666 ? O4 C5 C2 116.2(4) . . ? O4 C5 O3 125.8(4) . . ? O1W Co1 N1 89.72(15) . . ? O1W Co1 N1 89.72(15) 2_757 2_757 ? O1W Co1 N1 90.28(15) . 2_757 ? O1W Co1 N1 90.28(15) 2_757 . ? O1W Co1 O1 89.20(13) . . ? O1W Co1 O1 89.20(13) 2_757 2_757 ? O1W Co1 O1 90.80(13) . 2_757 ? O1W Co1 O1 90.80(13) 2_757 . ? O1W Co1 O1W 180.00(17) 2_757 . ? O2W Co2 N2 87.46(15) . 2_756 ? O2W Co2 N2 87.46(15) 2_666 1_465 ? O2W Co2 N2 92.54(15) . 1_465 ? O2W Co2 N2 92.54(15) 2_666 2_756 ? O2W Co2 O2W 180.0(2) . 2_666 ? O2W Co2 O3 89.38(12) . 2_666 ? O2W Co2 O3 89.38(12) 2_666 . ? O2W Co2 O3 90.62(12) . . ? O2W Co2 O3 90.62(12) 2_666 2_666 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.999 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.162