Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Xiao-Ming Chen' _publ_contact_author_address ; School of Chemistry Sun Yat-Sen University State Key Lab of Optoelectronic Mat Guangzhou 510275 CHINA ; _publ_contact_author_email CXM@MAIL.SYSU.EDU.CN _publ_section_title ; A Robust Microporous 3D Cobalt(II) Coordination Polymer with New Magnetically Frustrated 2D Lattices: Single-Crystal Transformation and Guest Modulation of Cooperative Magnetic Properties ; loop_ _publ_author_name _publ_author_address 'Ming-Hua Zeng' ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; 'Xiao-Long Feng' ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; 'Wei-Xiong Zhang' ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; 'Xiao-Ming Chen' ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; #===============================END data_1.2H2O'@293k _database_code_depnum_ccdc_archive 'CCDC 257660' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H7 Co2 N O7, 2(H2 O)' _chemical_formula_sum 'C10 H11 Co2 N O9' _chemical_formula_weight 407.06 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 Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.617(16) _cell_length_b 10.096(6) _cell_length_c 14.994(12) _cell_angle_alpha 90.00 _cell_angle_beta 128.707(19) _cell_angle_gamma 90.00 _cell_volume 2790(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 789 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 26.36 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.938 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 2.424 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5938 _exptl_absorpt_correction_T_max 0.7596 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6842 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2685 _reflns_number_gt 2149 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1113P)^2^+2.9668P] 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 2685 _refine_ls_number_parameters 225 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1909 _refine_ls_wR_factor_gt 0.1723 _refine_ls_goodness_of_fit_ref 1.227 _refine_ls_restrained_S_all 1.242 _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 0.24378(4) 0.72201(7) 0.10283(6) 0.0222(3) Uani 1 1 d . . . Co2 Co 0.28476(4) 1.03236(7) 0.23654(6) 0.0289(3) Uani 1 1 d . . . C1 C 0.3949(3) 0.8410(6) 0.2780(5) 0.0317(13) Uani 1 1 d . . . C2 C 0.4769(3) 0.8233(6) 0.3498(5) 0.0314(13) Uani 1 1 d . . . C3 C 0.5086(3) 0.7000(6) 0.3761(6) 0.0437(17) Uani 1 1 d . . . H3A H 0.4797 0.6244 0.3485 0.052 Uiso 1 1 d R . . C4 C 0.5825(3) 0.6898(6) 0.4426(6) 0.0425(16) Uani 1 1 d . . . H4A H 0.6029 0.6056 0.4604 0.051 Uiso 1 1 d R . . C5 C 0.5956(3) 0.9131(6) 0.4553(6) 0.0454(17) Uani 1 1 d . . . H5A H 0.6253 0.9874 0.4810 0.054 Uiso 1 1 d R . . C6 C 0.5218(3) 0.9310(6) 0.3911(6) 0.0469(18) Uani 1 1 d . . . H6A H 0.5027 1.0162 0.3758 0.056 Uiso 1 1 d R . . C7 C 0.2055(3) 0.8274(6) 0.2501(5) 0.0307(12) Uani 1 1 d D . . C8 C 0.2031(8) 0.9482(9) 0.3090(12) 0.033(3) Uani 0.69(2) 1 d P A 1 H8A H 0.1580 0.9846 0.2441 0.040 Uiso 0.69(2) 1 d PR A 1 C9 C 0.2271(6) 0.8992(9) 0.4222(9) 0.041(3) Uani 0.69(2) 1 d P A 1 H9A H 0.2766 0.8675 0.4651 0.050 Uiso 0.69(2) 1 calc PR A 1 H9B H 0.1972 0.8235 0.4082 0.050 Uiso 0.69(2) 1 calc PR A 1 C8' C 0.2365(14) 0.924(2) 0.3549(19) 0.029(5) Uani 0.31(2) 1 d PDU A 2 H8'A H 0.2817 0.8884 0.4240 0.035 Uiso 0.31(2) 1 calc PR A 2 C9' C 0.1791(11) 0.9439(19) 0.3747(15) 0.029(6) Uani 0.31(2) 1 d P A 2 H9'A H 0.1423 1.0076 0.3211 0.034 Uiso 0.31(2) 1 calc PR A 2 H9'B H 0.1558 0.8608 0.3669 0.034 Uiso 0.31(2) 1 calc PR A 2 C10 C 0.2248(3) 0.9961(6) 0.4979(5) 0.0371(14) Uani 1 1 d . . . N1 N 0.6268(3) 0.7936(5) 0.4830(4) 0.0304(11) Uani 1 1 d . . . O1 O 0.3568(2) 0.7450(4) 0.2225(4) 0.0334(9) Uani 1 1 d . . . O2 O 0.3755(2) 0.9557(4) 0.2815(4) 0.0433(11) Uani 1 1 d . . . O3 O 0.2358(2) 0.8444(4) 0.2063(3) 0.0317(9) Uani 1 1 d . A . O4 O 0.1747(2) 0.7228(4) 0.2417(4) 0.0393(10) Uani 1 1 d . . . O5 O 0.2502(2) 1.0499(3) 0.3245(3) 0.0286(9) Uani 1 1 d . . . O6 O 0.24014(19) 1.1190(4) 0.5030(3) 0.0264(8) Uani 1 1 d . . . O7 O 0.2196(3) 0.9394(4) 0.5666(4) 0.0433(11) Uani 1 1 d . . . O1W O 0.6070(11) 0.259(2) 0.506(2) 0.272(9) Uani 1 1 d DU . . H1A H 0.5614(14) 0.273(3) 0.453(2) 0.326 Uiso 1 1 d D . . H1B H 0.6460 0.3030 0.5350 0.326 Uiso 1 1 d RD . . O2W O 0.4660(9) 0.2871(19) 0.3117(15) 0.273(10) Uani 1 1 d DU . . H2A H 0.4717(9) 0.219(2) 0.2864(17) 0.327 Uiso 1 1 d D . . H2B H 0.4305 0.2728 0.3161 0.327 Uiso 1 1 d RD . . 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 0.0177(4) 0.0236(4) 0.0243(4) -0.0008(3) 0.0127(3) -0.0013(3) Co2 0.0272(5) 0.0257(4) 0.0386(5) -0.0043(3) 0.0228(4) -0.0012(3) C1 0.023(3) 0.035(3) 0.032(3) -0.002(2) 0.015(2) 0.001(2) C2 0.018(3) 0.035(3) 0.031(3) -0.004(2) 0.011(2) 0.000(2) C3 0.019(3) 0.034(3) 0.061(4) -0.006(3) 0.016(3) -0.004(2) C4 0.024(3) 0.033(3) 0.058(4) -0.004(3) 0.020(3) 0.003(2) C5 0.020(3) 0.034(3) 0.058(4) 0.002(3) 0.012(3) -0.001(2) C6 0.018(3) 0.034(3) 0.062(4) -0.002(3) 0.012(3) 0.001(2) C7 0.031(3) 0.028(3) 0.039(3) -0.001(2) 0.026(3) 0.002(2) C8 0.039(7) 0.024(5) 0.046(6) -0.001(4) 0.032(6) 0.001(4) C9 0.041(7) 0.031(5) 0.049(6) -0.002(4) 0.026(6) -0.004(5) C8' 0.019(8) 0.028(8) 0.042(9) 0.017(7) 0.020(7) 0.005(6) C9' 0.022(12) 0.031(10) 0.024(9) -0.003(7) 0.010(8) -0.007(8) C10 0.034(3) 0.035(3) 0.038(3) -0.003(3) 0.020(3) -0.003(3) N1 0.020(2) 0.036(3) 0.030(2) 0.002(2) 0.0132(19) 0.0013(19) O1 0.0198(19) 0.032(2) 0.038(2) -0.0047(18) 0.0130(17) -0.0010(16) O2 0.022(2) 0.033(2) 0.066(3) -0.009(2) 0.023(2) -0.0022(17) O3 0.034(2) 0.0286(19) 0.041(2) -0.0082(17) 0.0278(19) -0.0034(17) O4 0.044(3) 0.030(2) 0.061(3) 0.0007(19) 0.041(2) 0.0013(19) O5 0.026(2) 0.0230(18) 0.046(2) -0.0030(16) 0.0268(18) -0.0031(15) O6 0.0253(19) 0.0274(18) 0.0262(18) 0.0008(15) 0.0159(16) 0.0020(15) O7 0.051(3) 0.037(2) 0.038(2) -0.0025(19) 0.026(2) -0.010(2) O1W 0.245(12) 0.265(12) 0.300(13) 0.031(9) 0.167(9) -0.025(8) O2W 0.254(13) 0.271(13) 0.296(13) 0.034(9) 0.174(9) 0.014(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 Co1 O5 2.009(4) 4_545 ? Co1 O3 2.082(4) . ? Co1 O1 2.100(4) . ? Co1 O6 2.121(4) 4_545 ? Co1 O6 2.159(4) 6_575 ? Co1 N1 2.163(5) 8_465 ? Co2 O5 1.944(4) . ? Co2 O2 1.958(5) . ? Co2 O7 2.010(5) 6_575 ? Co2 O4 2.080(4) 4 ? Co2 O3 2.118(4) . ? C1 O1 1.226(7) . ? C1 O2 1.258(7) . ? C1 C2 1.529(8) . ? C2 C3 1.376(9) . ? C2 C6 1.367(9) . ? C3 C4 1.370(9) . ? C3 H3A 0.9300 . ? C4 N1 1.329(8) . ? C4 H4A 0.9300 . ? C5 N1 1.337(8) . ? C5 C6 1.378(8) . ? C5 H5A 0.9300 . ? C6 H6A 0.9301 . ? C7 O3 1.250(7) . ? C7 O4 1.244(7) . ? C7 C8 1.527(10) . ? C7 C8' 1.587(16) . ? C8 O5 1.423(11) . ? C8 C9 1.497(17) . ? C8 H8A 0.9600 . ? C9 C10 1.526(12) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C8' O5 1.45(2) . ? C8' C9' 1.57(3) . ? C8' H8'A 0.9800 . ? C9' C10 1.538(18) . ? C9' H9'A 0.9700 . ? C9' H9'B 0.9700 . ? C10 O7 1.249(8) . ? C10 O6 1.281(7) . ? N1 Co1 2.163(5) 8_566 ? O4 Co2 2.080(4) 4_545 ? O5 Co1 2.009(4) 4 ? O6 Co1 2.121(4) 4 ? O6 Co1 2.159(4) 6_576 ? O7 Co2 2.010(5) 6_576 ? O1W H1A 0.862(11) . ? O1W H1B 0.8604 . ? O2W H2A 0.839(11) . ? O2W H2B 0.8939 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Co1 O3 96.74(17) 4_545 . ? O5 Co1 O1 90.67(17) 4_545 . ? O3 Co1 O1 87.49(17) . . ? O5 Co1 O6 89.84(16) 4_545 4_545 ? O3 Co1 O6 172.12(15) . 4_545 ? O1 Co1 O6 88.11(16) . 4_545 ? O5 Co1 O6 167.95(15) 4_545 6_575 ? O3 Co1 O6 95.30(16) . 6_575 ? O1 Co1 O6 89.33(16) . 6_575 ? O6 Co1 O6 78.12(16) 4_545 6_575 ? O5 Co1 N1 90.43(17) 4_545 8_465 ? O3 Co1 N1 89.95(18) . 8_465 ? O1 Co1 N1 177.31(17) . 8_465 ? O6 Co1 N1 94.34(17) 4_545 8_465 ? O6 Co1 N1 90.11(17) 6_575 8_465 ? O5 Co2 O2 129.4(2) . . ? O5 Co2 O7 122.2(2) . 6_575 ? O2 Co2 O7 107.4(2) . 6_575 ? O5 Co2 O4 99.01(16) . 4 ? O2 Co2 O4 90.83(18) . 4 ? O7 Co2 O4 88.88(19) 6_575 4 ? O5 Co2 O3 79.79(15) . . ? O2 Co2 O3 92.99(17) . . ? O7 Co2 O3 88.44(18) 6_575 . ? O4 Co2 O3 175.85(17) 4 . ? O1 C1 O2 128.6(5) . . ? O1 C1 C2 116.9(5) . . ? O2 C1 C2 114.4(5) . . ? C3 C2 C6 117.5(6) . . ? C3 C2 C1 122.0(5) . . ? C6 C2 C1 120.5(5) . . ? C2 C3 C4 119.5(6) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.5 . . ? N1 C4 C3 123.6(6) . . ? N1 C4 H4A 118.1 . . ? C3 C4 H4A 118.2 . . ? N1 C5 C6 123.2(6) . . ? N1 C5 H5A 118.2 . . ? C6 C5 H5A 118.7 . . ? C5 C6 C2 119.6(6) . . ? C5 C6 H6A 120.0 . . ? C2 C6 H6A 120.3 . . ? O3 C7 O4 123.6(5) . . ? O3 C7 C8 115.8(6) . . ? O4 C7 C8 120.4(6) . . ? O3 C7 C8' 112.0(9) . . ? O4 C7 C8' 120.1(9) . . ? C8 C7 C8' 25.5(7) . . ? O5 C8 C9 110.5(10) . . ? O5 C8 C7 111.2(7) . . ? C9 C8 C7 105.5(9) . . ? O5 C8 H8A 98.6 . . ? C9 C8 H8A 131.9 . . ? C7 C8 H8A 98.0 . . ? C8 C9 C10 117.8(8) . . ? C8 C9 H9A 107.8 . . ? C10 C9 H9A 107.8 . . ? C8 C9 H9B 107.8 . . ? C10 C9 H9B 107.8 . . ? H9A C9 H9B 107.2 . . ? O5 C8' C9' 109.7(17) . . ? O5 C8' C7 106.4(13) . . ? C9' C8' C7 110.3(15) . . ? O5 C8' H8'A 110.1 . . ? C9' C8' H8'A 110.1 . . ? C7 C8' H8'A 110.1 . . ? C10 C9' C8' 103.4(15) . . ? C10 C9' H9'A 111.1 . . ? C8' C9' H9'A 111.1 . . ? C10 C9' H9'B 111.1 . . ? C8' C9' H9'B 111.1 . . ? H9'A C9' H9'B 109.1 . . ? O7 C10 O6 124.4(6) . . ? O7 C10 C9 112.8(6) . . ? O6 C10 C9 121.6(6) . . ? O7 C10 C9' 118.5(8) . . ? O6 C10 C9' 111.3(8) . . ? C9 C10 C9' 37.8(8) . . ? C5 N1 C4 116.5(5) . . ? C5 N1 Co1 119.6(4) . 8_566 ? C4 N1 Co1 123.6(4) . 8_566 ? C1 O1 Co1 131.9(4) . . ? C1 O2 Co2 134.3(4) . . ? C7 O3 Co1 131.2(4) . . ? C7 O3 Co2 115.2(4) . . ? Co1 O3 Co2 113.57(18) . . ? C7 O4 Co2 125.9(4) . 4_545 ? C8 O5 C8' 27.7(7) . . ? C8 O5 Co2 116.2(4) . . ? C8' O5 Co2 113.8(8) . . ? C8 O5 Co1 119.7(4) . 4 ? C8' O5 Co1 122.6(7) . 4 ? Co2 O5 Co1 122.00(19) . 4 ? C10 O6 Co1 127.4(4) . 4 ? C10 O6 Co1 130.4(4) . 6_576 ? Co1 O6 Co1 101.88(16) 4 6_576 ? C10 O7 Co2 126.0(4) . 6_576 ? H1A O1W H1B 134.6 . . ? H2A O2W H2B 108.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -16.6(9) . . . . ? O2 C1 C2 C3 165.5(6) . . . . ? O1 C1 C2 C6 163.9(6) . . . . ? O2 C1 C2 C6 -14.0(9) . . . . ? C6 C2 C3 C4 0.8(11) . . . . ? C1 C2 C3 C4 -178.7(6) . . . . ? C2 C3 C4 N1 -1.1(12) . . . . ? N1 C5 C6 C2 -2.1(13) . . . . ? C3 C2 C6 C5 0.7(11) . . . . ? C1 C2 C6 C5 -179.8(7) . . . . ? O3 C7 C8 O5 -12.9(13) . . . . ? O4 C7 C8 O5 171.3(7) . . . . ? C8' C7 C8 O5 74(2) . . . . ? O3 C7 C8 C9 -132.8(8) . . . . ? O4 C7 C8 C9 51.5(12) . . . . ? C8' C7 C8 C9 -45(2) . . . . ? O5 C8 C9 C10 64.3(13) . . . . ? C7 C8 C9 C10 -175.4(7) . . . . ? O3 C7 C8' O5 37.6(18) . . . . ? O4 C7 C8' O5 -164.7(10) . . . . ? C8 C7 C8' O5 -66(2) . . . . ? O3 C7 C8' C9' 156.5(14) . . . . ? O4 C7 C8' C9' -46(2) . . . . ? C8 C7 C8' C9' 52(2) . . . . ? O5 C8' C9' C10 -82.0(18) . . . . ? C7 C8' C9' C10 161.1(12) . . . . ? C8 C9 C10 O7 155.5(9) . . . . ? C8 C9 C10 O6 -36.5(13) . . . . ? C8 C9 C10 C9' 47.9(14) . . . . ? C8' C9' C10 O7 -128.2(12) . . . . ? C8' C9' C10 O6 77.6(16) . . . . ? C8' C9' C10 C9 -37.0(13) . . . . ? C6 C5 N1 C4 1.7(11) . . . . ? C6 C5 N1 Co1 -171.7(6) . . . 8_566 ? C3 C4 N1 C5 -0.1(11) . . . . ? C3 C4 N1 Co1 173.0(6) . . . 8_566 ? O2 C1 O1 Co1 3.2(10) . . . . ? C2 C1 O1 Co1 -174.4(4) . . . . ? O5 Co1 O1 C1 -136.0(6) 4_545 . . . ? O3 Co1 O1 C1 -39.2(6) . . . . ? O6 Co1 O1 C1 134.2(6) 4_545 . . . ? O6 Co1 O1 C1 56.1(6) 6_575 . . . ? N1 Co1 O1 C1 -22(4) 8_465 . . . ? O1 C1 O2 Co2 16.5(11) . . . . ? C2 C1 O2 Co2 -165.9(5) . . . . ? O5 Co2 O2 C1 88.8(6) . . . . ? O7 Co2 O2 C1 -79.8(6) 6_575 . . . ? O4 Co2 O2 C1 -168.8(6) 4 . . . ? O3 Co2 O2 C1 9.5(6) . . . . ? O4 C7 O3 Co1 3.2(9) . . . . ? C8 C7 O3 Co1 -172.4(7) . . . . ? C8' C7 O3 Co1 160.0(11) . . . . ? O4 C7 O3 Co2 -179.4(5) . . . . ? C8 C7 O3 Co2 5.0(9) . . . . ? C8' C7 O3 Co2 -22.6(12) . . . . ? O5 Co1 O3 C7 -35.0(5) 4_545 . . . ? O1 Co1 O3 C7 -125.4(5) . . . . ? O6 Co1 O3 C7 178.5(9) 4_545 . . . ? O6 Co1 O3 C7 145.6(5) 6_575 . . . ? N1 Co1 O3 C7 55.5(5) 8_465 . . . ? O5 Co1 O3 Co2 147.56(19) 4_545 . . . ? O1 Co1 O3 Co2 57.2(2) . . . . ? O6 Co1 O3 Co2 1.1(13) 4_545 . . . ? O6 Co1 O3 Co2 -31.9(2) 6_575 . . . ? N1 Co1 O3 Co2 -122.0(2) 8_465 . . . ? O5 Co2 O3 C7 2.5(4) . . . . ? O2 Co2 O3 C7 132.0(4) . . . . ? O7 Co2 O3 C7 -120.6(4) 6_575 . . . ? O4 Co2 O3 C7 -71(2) 4 . . . ? O5 Co2 O3 Co1 -179.6(2) . . . . ? O2 Co2 O3 Co1 -50.1(2) . . . . ? O7 Co2 O3 Co1 57.3(2) 6_575 . . . ? O4 Co2 O3 Co1 107(2) 4 . . . ? O3 C7 O4 Co2 45.3(8) . . . 4_545 ? C8 C7 O4 Co2 -139.4(7) . . . 4_545 ? C8' C7 O4 Co2 -109.8(12) . . . 4_545 ? C9 C8 O5 C8' 40(2) . . . . ? C7 C8 O5 C8' -76.8(18) . . . . ? C9 C8 O5 Co2 131.9(7) . . . . ? C7 C8 O5 Co2 15.1(12) . . . . ? C9 C8 O5 Co1 -64.5(11) . . . 4 ? C7 C8 O5 Co1 178.7(6) . . . 4 ? C9' C8' O5 C8 -54(2) . . . . ? C7 C8' O5 C8 65.6(16) . . . . ? C9' C8' O5 Co2 -155.1(11) . . . . ? C7 C8' O5 Co2 -35.7(18) . . . . ? C9' C8' O5 Co1 39(2) . . . 4 ? C7 C8' O5 Co1 158.1(7) . . . 4 ? O2 Co2 O5 C8 -95.5(7) . . . . ? O7 Co2 O5 C8 71.5(7) 6_575 . . . ? O4 Co2 O5 C8 165.9(7) 4 . . . ? O3 Co2 O5 C8 -10.1(7) . . . . ? O2 Co2 O5 C8' -65.0(11) . . . . ? O7 Co2 O5 C8' 102.1(11) 6_575 . . . ? O4 Co2 O5 C8' -163.6(11) 4 . . . ? O3 Co2 O5 C8' 20.5(11) . . . . ? O2 Co2 O5 Co1 101.3(3) . . . 4 ? O7 Co2 O5 Co1 -91.7(3) 6_575 . . 4 ? O4 Co2 O5 Co1 2.7(3) 4 . . 4 ? O3 Co2 O5 Co1 -173.3(3) . . . 4 ? O7 C10 O6 Co1 176.2(5) . . . 4 ? C9 C10 O6 Co1 9.6(9) . . . 4 ? C9' C10 O6 Co1 -31.4(11) . . . 4 ? O7 C10 O6 Co1 -12.1(9) . . . 6_576 ? C9 C10 O6 Co1 -178.7(6) . . . 6_576 ? C9' C10 O6 Co1 140.4(10) . . . 6_576 ? O6 C10 O7 Co2 -40.4(9) . . . 6_576 ? C9 C10 O7 Co2 127.2(6) . . . 6_576 ? C9' C10 O7 Co2 168.9(10) . . . 6_576 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2W H2A O2W 0.839(11) 2.740(9) 3.116(10) 109.1(11) 2_655 O2W H2B O4 0.89 2.12 2.963(13) 157.5 4_545 O1W H1B O7 0.86 2.03 2.87(2) 164.7 3_545 O1W H1A O2W 0.862(11) 1.90(2) 2.74(3) 165(5) . _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.316 _refine_diff_density_min -1.040 _refine_diff_density_rms 0.412 #====================================== data_1.2H2O@293k _database_code_depnum_ccdc_archive 'CCDC 600566' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H7 Co2 N O7, 2(H2 O)' _chemical_formula_sum 'C10 H11 Co2 N O9' _chemical_formula_weight 407.06 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 Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.550(2) _cell_length_b 10.0816(10) _cell_length_c 14.9781(15) _cell_angle_alpha 90.00 _cell_angle_beta 128.4650(10) _cell_angle_gamma 90.00 _cell_volume 2784.4(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.942 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 2.429 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6801 _exptl_absorpt_correction_T_max 0.8294 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7164 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2666 _reflns_number_gt 2332 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+5.5586P] 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 2666 _refine_ls_number_parameters 223 _refine_ls_number_restraints 79 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1124 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.213 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.002 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 0.24408(3) 0.72253(5) 0.10297(4) 0.01928(18) Uani 1 1 d . . . Co2 Co 0.28465(3) 1.03287(6) 0.23628(5) 0.02657(19) Uani 1 1 d . . . O2 O 0.37596(18) 0.9547(3) 0.2825(3) 0.0432(9) Uani 1 1 d . . . O1 O 0.35655(16) 0.7443(3) 0.2210(3) 0.0309(7) Uani 1 1 d . . . O3 O 0.23570(16) 0.8451(3) 0.2062(2) 0.0291(7) Uani 1 1 d . A . O4 O 0.17436(19) 0.7229(3) 0.2416(3) 0.0375(8) Uani 1 1 d . . . O5 O 0.24980(16) 1.0500(3) 0.3238(3) 0.0262(6) Uani 1 1 d D . . O6 O 0.23972(14) 1.1188(3) 0.5030(2) 0.0234(6) Uani 1 1 d . . . O7 O 0.2197(2) 0.9390(3) 0.5669(3) 0.0393(8) Uani 1 1 d . . . N1 N 0.62727(19) 0.7931(4) 0.4843(3) 0.0284(8) Uani 1 1 d . . . C1 C 0.3956(2) 0.8410(4) 0.2786(4) 0.0287(9) Uani 1 1 d . . . C2 C 0.4768(2) 0.8224(5) 0.3502(3) 0.0285(9) Uani 1 1 d . . . C3 C 0.5082(3) 0.6986(5) 0.3772(5) 0.0411(12) Uani 1 1 d . . . H3A H 0.4794 0.6230 0.3496 0.049 Uiso 1 1 d R . . C4 C 0.5826(3) 0.6895(5) 0.4439(4) 0.0403(12) Uani 1 1 d . . . H4A H 0.6030 0.6053 0.4616 0.048 Uiso 1 1 d R . . C5 C 0.5955(2) 0.9125(5) 0.4547(4) 0.0415(12) Uani 1 1 d . . . H5A H 0.6252 0.9868 0.4805 0.050 Uiso 1 1 d R . . C6 C 0.5218(3) 0.9306(5) 0.3907(5) 0.0443(13) Uani 1 1 d . . . H6A H 0.5027 1.0157 0.3754 0.053 Uiso 1 1 d R . . C7 C 0.2052(2) 0.8270(4) 0.2500(4) 0.0281(9) Uani 1 1 d D . . C8 C 0.2017(5) 0.9491(7) 0.3067(7) 0.031(2) Uani 0.672(14) 1 d PDU A 1 H8A H 0.1519 0.9831 0.2610 0.037 Uiso 0.672(14) 1 calc PR A 1 C9 C 0.2255(5) 0.8992(7) 0.4203(6) 0.036(2) Uani 0.672(14) 1 d PDU A 1 H9A H 0.2744 0.8650 0.4620 0.044 Uiso 0.672(14) 1 calc PR A 1 H9B H 0.1946 0.8250 0.4058 0.044 Uiso 0.672(14) 1 calc PR A 1 C8' C 0.2308(10) 0.9280(13) 0.3472(14) 0.030(4) Uani 0.328(14) 1 d PDU A 2 H8'A H 0.2761 0.8921 0.4156 0.036 Uiso 0.328(14) 1 calc PR A 2 C9' C 0.1797(9) 0.9387(18) 0.3761(12) 0.039(4) Uani 0.328(14) 1 d PDU A 2 H9'A H 0.1606 0.8521 0.3732 0.047 Uiso 0.328(14) 1 calc PR A 2 H9'B H 0.1394 0.9970 0.3227 0.047 Uiso 0.328(14) 1 calc PR A 2 C10 C 0.2251(3) 0.9962(5) 0.4984(4) 0.0342(10) Uani 1 1 d D . . O1W O 0.6089(10) 0.2641(16) 0.5019(15) 0.330(9) Uani 1 1 d DU . . H1A H 0.5681 0.2535 0.5008 0.397 Uiso 1 1 d RD . . H1B H 0.6468 0.2968 0.5781 0.397 Uiso 1 1 d RD . . O2W O 0.4683(8) 0.2915(15) 0.3178(16) 0.292(8) Uani 1 1 d DU . . H2A H 0.4932(7) 0.232(2) 0.3155(12) 0.350 Uiso 1 1 d D . . H2B H 0.4301 0.2587 0.3078 0.350 Uiso 1 1 d RD . . 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 0.0180(3) 0.0192(3) 0.0189(3) -0.0011(2) 0.0106(2) -0.0016(2) Co2 0.0272(3) 0.0216(3) 0.0336(3) -0.0046(2) 0.0203(3) -0.0012(2) O2 0.0256(17) 0.0297(17) 0.066(2) -0.0140(16) 0.0244(17) -0.0011(13) O1 0.0194(15) 0.0292(16) 0.0330(16) -0.0042(13) 0.0108(13) -0.0017(12) O3 0.0333(17) 0.0237(15) 0.0335(16) -0.0060(13) 0.0224(14) -0.0028(13) O4 0.045(2) 0.0286(17) 0.056(2) 0.0014(15) 0.0396(18) 0.0029(15) O5 0.0335(17) 0.0163(14) 0.0382(16) -0.0043(12) 0.0269(15) -0.0047(12) O6 0.0254(15) 0.0217(15) 0.0233(14) -0.0007(11) 0.0152(12) -0.0002(12) O7 0.053(2) 0.0298(17) 0.0299(16) -0.0010(14) 0.0228(16) -0.0118(15) N1 0.0185(17) 0.032(2) 0.0270(18) 0.0017(15) 0.0102(15) 0.0026(15) C1 0.022(2) 0.031(2) 0.030(2) -0.0010(18) 0.0142(18) -0.0013(18) C2 0.019(2) 0.033(2) 0.025(2) -0.0018(18) 0.0092(18) 0.0000(17) C3 0.026(2) 0.027(2) 0.058(3) -0.008(2) 0.020(2) -0.0048(19) C4 0.028(2) 0.028(2) 0.050(3) 0.000(2) 0.017(2) 0.0057(19) C5 0.021(2) 0.027(2) 0.052(3) 0.001(2) 0.010(2) -0.0023(19) C6 0.024(2) 0.025(2) 0.057(3) 0.000(2) 0.012(2) 0.0033(19) C7 0.030(2) 0.025(2) 0.031(2) 0.0006(18) 0.020(2) 0.0009(18) C8 0.030(5) 0.027(4) 0.032(4) 0.001(3) 0.018(4) 0.007(3) C9 0.045(5) 0.027(4) 0.036(4) -0.002(3) 0.024(4) 0.001(3) C8' 0.025(7) 0.025(7) 0.045(8) 0.011(6) 0.024(6) -0.003(5) C9' 0.034(9) 0.045(9) 0.045(9) -0.008(7) 0.029(8) -0.009(7) C10 0.034(3) 0.032(3) 0.026(2) -0.0058(19) 0.013(2) 0.000(2) O1W 0.302(13) 0.311(12) 0.364(13) 0.041(9) 0.200(10) -0.042(8) O2W 0.259(11) 0.293(12) 0.320(12) 0.045(8) 0.179(9) 0.013(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 Co1 O5 2.013(3) 4_545 ? Co1 O3 2.082(3) . ? Co1 O1 2.089(3) . ? Co1 O6 2.124(3) 4_545 ? Co1 O6 2.150(3) 6_575 ? Co1 N1 2.161(3) 8_465 ? Co2 O5 1.939(3) . ? Co2 O2 1.968(3) . ? Co2 O7 2.008(3) 6_575 ? Co2 O4 2.077(3) 4 ? Co2 O3 2.114(3) . ? O2 C1 1.252(5) . ? O1 C1 1.246(5) . ? O3 C7 1.251(5) . ? O4 C7 1.238(5) . ? O4 Co2 2.077(3) 4_545 ? O5 C8 1.423(8) . ? O5 C8' 1.426(13) . ? O5 Co1 2.013(3) 4 ? O6 C10 1.273(6) . ? O6 Co1 2.124(3) 4 ? O6 Co1 2.150(3) 6_576 ? O7 C10 1.252(6) . ? O7 Co2 2.008(3) 6_576 ? N1 C5 1.339(6) . ? N1 C4 1.331(6) . ? N1 Co1 2.161(3) 8_566 ? C1 C2 1.513(6) . ? C2 C3 1.378(7) . ? C2 C6 1.372(6) . ? C3 C4 1.379(7) . ? C3 H3A 0.9292 . ? C4 H4A 0.9288 . ? C5 C6 1.376(7) . ? C5 H5A 0.9291 . ? C6 H6A 0.9289 . ? C7 C8 1.527(8) . ? C7 C8' 1.559(13) . ? C8 C9 1.508(9) . ? C8 H8A 0.9800 . ? C9 C10 1.528(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C8' C9' 1.514(14) . ? C8' H8'A 0.9800 . ? C9' C10 1.548(12) . ? C9' H9'A 0.9700 . ? C9' H9'B 0.9700 . ? O1W H1A 0.9567 . ? O1W H1B 0.9691 . ? O2W H2A 0.856(11) . ? O2W H2B 0.8784 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Co1 O3 96.65(12) 4_545 . ? O5 Co1 O1 90.37(12) 4_545 . ? O3 Co1 O1 88.02(12) . . ? O5 Co1 O6 89.79(11) 4_545 4_545 ? O3 Co1 O6 172.33(11) . 4_545 ? O1 Co1 O6 87.78(11) . 4_545 ? O5 Co1 O6 168.17(11) 4_545 6_575 ? O3 Co1 O6 95.17(11) . 6_575 ? O1 Co1 O6 89.83(11) . 6_575 ? O6 Co1 O6 78.40(11) 4_545 6_575 ? O5 Co1 N1 90.47(13) 4_545 8_465 ? O3 Co1 N1 89.67(13) . 8_465 ? O1 Co1 N1 177.62(13) . 8_465 ? O6 Co1 N1 94.45(12) 4_545 8_465 ? O6 Co1 N1 89.80(12) 6_575 8_465 ? O5 Co2 O2 128.86(15) . . ? O5 Co2 O7 122.10(14) . 6_575 ? O2 Co2 O7 107.95(15) . 6_575 ? O5 Co2 O4 99.19(12) . 4 ? O2 Co2 O4 90.88(13) . 4 ? O7 Co2 O4 89.11(14) 6_575 4 ? O5 Co2 O3 79.65(11) . . ? O2 Co2 O3 92.76(13) . . ? O7 Co2 O3 88.36(13) 6_575 . ? O4 Co2 O3 176.07(13) 4 . ? C1 O2 Co2 134.8(3) . . ? C1 O1 Co1 132.0(3) . . ? C7 O3 Co1 130.8(3) . . ? C7 O3 Co2 115.7(3) . . ? Co1 O3 Co2 113.51(14) . . ? C7 O4 Co2 125.5(3) . 4_545 ? C8 O5 C8' 24.5(6) . . ? C8 O5 Co2 116.1(3) . . ? C8' O5 Co2 114.8(5) . . ? C8 O5 Co1 119.7(3) . 4 ? C8' O5 Co1 122.6(5) . 4 ? Co2 O5 Co1 121.91(14) . 4 ? C10 O6 Co1 127.3(3) . 4 ? C10 O6 Co1 130.9(3) . 6_576 ? Co1 O6 Co1 101.60(11) 4 6_576 ? C10 O7 Co2 125.8(3) . 6_576 ? C5 N1 C4 115.7(4) . . ? C5 N1 Co1 120.1(3) . 8_566 ? C4 N1 Co1 123.9(3) . 8_566 ? O1 C1 O2 127.9(4) . . ? O1 C1 C2 117.2(4) . . ? O2 C1 C2 114.9(4) . . ? C3 C2 C6 117.6(4) . . ? C3 C2 C1 122.1(4) . . ? C6 C2 C1 120.2(4) . . ? C4 C3 C2 118.8(4) . . ? C4 C3 H3A 121.1 . . ? C2 C3 H3A 120.1 . . ? N1 C4 C3 124.5(4) . . ? N1 C4 H4A 117.8 . . ? C3 C4 H4A 117.7 . . ? N1 C5 C6 123.6(4) . . ? N1 C5 H5A 117.8 . . ? C6 C5 H5A 118.7 . . ? C5 C6 C2 119.7(4) . . ? C5 C6 H6A 120.1 . . ? C2 C6 H6A 120.2 . . ? O4 C7 O3 124.2(4) . . ? O4 C7 C8 120.6(5) . . ? O3 C7 C8 114.9(4) . . ? O4 C7 C8' 120.7(6) . . ? O3 C7 C8' 112.4(6) . . ? C8 C7 C8' 22.6(6) . . ? O5 C8 C9 109.9(7) . . ? O5 C8 C7 111.3(5) . . ? C9 C8 C7 104.3(6) . . ? O5 C8 H8A 110.4 . . ? C9 C8 H8A 110.4 . . ? C7 C8 H8A 110.4 . . ? C8 C9 C10 118.3(6) . . ? C8 C9 H9A 107.7 . . ? C10 C9 H9A 107.7 . . ? C8 C9 H9B 107.7 . . ? C10 C9 H9B 107.7 . . ? H9A C9 H9B 107.1 . . ? O5 C8' C9' 115.9(12) . . ? O5 C8' C7 109.3(9) . . ? C9' C8' C7 113.6(10) . . ? O5 C8' H8'A 105.7 . . ? C9' C8' H8'A 105.7 . . ? C7 C8' H8'A 105.7 . . ? C8' C9' C10 106.1(11) . . ? C8' C9' H9'A 110.5 . . ? C10 C9' H9'A 110.5 . . ? C8' C9' H9'B 110.5 . . ? C10 C9' H9'B 110.5 . . ? H9'A C9' H9'B 108.7 . . ? O7 C10 O6 124.4(4) . . ? O7 C10 C9 112.6(4) . . ? O6 C10 C9 122.2(5) . . ? O7 C10 C9' 116.7(7) . . ? O6 C10 C9' 113.1(8) . . ? C9 C10 C9' 35.3(6) . . ? H1A O1W H1B 103.8 . . ? H2A O2W H2B 112.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Co2 O2 C1 89.5(5) . . . . ? O7 Co2 O2 C1 -78.6(5) 6_575 . . . ? O4 Co2 O2 C1 -167.9(5) 4 . . . ? O3 Co2 O2 C1 10.6(5) . . . . ? O5 Co1 O1 C1 -134.7(4) 4_545 . . . ? O3 Co1 O1 C1 -38.0(4) . . . . ? O6 Co1 O1 C1 135.6(4) 4_545 . . . ? O6 Co1 O1 C1 57.2(4) 6_575 . . . ? N1 Co1 O1 C1 -24(3) 8_465 . . . ? O5 Co1 O3 C7 -34.8(4) 4_545 . . . ? O1 Co1 O3 C7 -125.0(4) . . . . ? O6 Co1 O3 C7 178.2(7) 4_545 . . . ? O6 Co1 O3 C7 145.4(4) 6_575 . . . ? N1 Co1 O3 C7 55.6(4) 8_465 . . . ? O5 Co1 O3 Co2 147.30(14) 4_545 . . . ? O1 Co1 O3 Co2 57.16(15) . . . . ? O6 Co1 O3 Co2 0.4(9) 4_545 . . . ? O6 Co1 O3 Co2 -32.49(15) 6_575 . . . ? N1 Co1 O3 Co2 -122.26(16) 8_465 . . . ? O5 Co2 O3 C7 2.3(3) . . . . ? O2 Co2 O3 C7 131.3(3) . . . . ? O7 Co2 O3 C7 -120.8(3) 6_575 . . . ? O4 Co2 O3 C7 -70.9(18) 4 . . . ? O5 Co2 O3 Co1 -179.49(17) . . . . ? O2 Co2 O3 Co1 -50.45(17) . . . . ? O7 Co2 O3 Co1 57.44(16) 6_575 . . . ? O4 Co2 O3 Co1 107.3(18) 4 . . . ? O2 Co2 O5 C8 -96.2(5) . . . . ? O7 Co2 O5 C8 70.4(5) 6_575 . . . ? O4 Co2 O5 C8 165.2(5) 4 . . . ? O3 Co2 O5 C8 -11.0(4) . . . . ? O2 Co2 O5 C8' -69.0(9) . . . . ? O7 Co2 O5 C8' 97.6(9) 6_575 . . . ? O4 Co2 O5 C8' -167.7(9) 4 . . . ? O3 Co2 O5 C8' 16.1(9) . . . . ? O2 Co2 O5 Co1 101.4(2) . . . 4 ? O7 Co2 O5 Co1 -92.0(2) 6_575 . . 4 ? O4 Co2 O5 Co1 2.7(2) 4 . . 4 ? O3 Co2 O5 Co1 -173.46(19) . . . 4 ? Co1 O1 C1 O2 2.2(7) . . . . ? Co1 O1 C1 C2 -175.6(3) . . . . ? Co2 O2 C1 O1 16.0(8) . . . . ? Co2 O2 C1 C2 -166.1(3) . . . . ? O1 C1 C2 C3 -17.6(7) . . . . ? O2 C1 C2 C3 164.3(5) . . . . ? O1 C1 C2 C6 162.4(5) . . . . ? O2 C1 C2 C6 -15.7(7) . . . . ? C6 C2 C3 C4 0.6(8) . . . . ? C1 C2 C3 C4 -179.4(5) . . . . ? C5 N1 C4 C3 -1.1(8) . . . . ? Co1 N1 C4 C3 173.2(4) 8_566 . . . ? C2 C3 C4 N1 -0.5(9) . . . . ? C4 N1 C5 C6 2.5(8) . . . . ? Co1 N1 C5 C6 -172.0(5) 8_566 . . . ? N1 C5 C6 C2 -2.5(9) . . . . ? C3 C2 C6 C5 0.8(8) . . . . ? C1 C2 C6 C5 -179.3(5) . . . . ? Co2 O4 C7 O3 45.7(6) 4_545 . . . ? Co2 O4 C7 C8 -140.4(5) 4_545 . . . ? Co2 O4 C7 C8' -114.1(9) 4_545 . . . ? Co1 O3 C7 O4 2.7(7) . . . . ? Co2 O3 C7 O4 -179.5(3) . . . . ? Co1 O3 C7 C8 -171.5(4) . . . . ? Co2 O3 C7 C8 6.3(6) . . . . ? Co1 O3 C7 C8' 164.0(8) . . . . ? Co2 O3 C7 C8' -18.2(9) . . . . ? C8' O5 C8 C9 39.1(14) . . . . ? Co2 O5 C8 C9 132.1(5) . . . . ? Co1 O5 C8 C9 -65.0(7) 4 . . . ? C8' O5 C8 C7 -76.0(15) . . . . ? Co2 O5 C8 C7 17.0(7) . . . . ? Co1 O5 C8 C7 179.9(4) 4 . . . ? O4 C7 C8 O5 170.6(5) . . . . ? O3 C7 C8 O5 -15.0(8) . . . . ? C8' C7 C8 O5 73.6(15) . . . . ? O4 C7 C8 C9 52.2(8) . . . . ? O3 C7 C8 C9 -133.4(6) . . . . ? C8' C7 C8 C9 -44.8(14) . . . . ? O5 C8 C9 C10 63.2(10) . . . . ? C7 C8 C9 C10 -177.4(6) . . . . ? C8 O5 C8' C9' -60.1(16) . . . . ? Co2 O5 C8' C9' -158.9(10) . . . . ? Co1 O5 C8' C9' 30.8(18) 4 . . . ? C8 O5 C8' C7 69.8(15) . . . . ? Co2 O5 C8' C7 -29.0(13) . . . . ? Co1 O5 C8' C7 160.7(6) 4 . . . ? O4 C7 C8' O5 -167.5(7) . . . . ? O3 C7 C8' O5 30.5(14) . . . . ? C8 C7 C8' O5 -70.9(16) . . . . ? O4 C7 C8' C9' -36.4(18) . . . . ? O3 C7 C8' C9' 161.6(12) . . . . ? C8 C7 C8' C9' 60.2(17) . . . . ? O5 C8' C9' C10 -73.6(18) . . . . ? C7 C8' C9' C10 158.6(10) . . . . ? Co2 O7 C10 O6 -41.1(7) 6_576 . . . ? Co2 O7 C10 C9 128.9(5) 6_576 . . . ? Co2 O7 C10 C9' 167.7(8) 6_576 . . . ? Co1 O6 C10 O7 176.3(3) 4 . . . ? Co1 O6 C10 O7 -10.6(7) 6_576 . . . ? Co1 O6 C10 C9 7.2(7) 4 . . . ? Co1 O6 C10 C9 -179.7(5) 6_576 . . . ? Co1 O6 C10 C9' -31.6(8) 4 . . . ? Co1 O6 C10 C9' 141.5(7) 6_576 . . . ? C8 C9 C10 O7 155.6(7) . . . . ? C8 C9 C10 O6 -34.1(10) . . . . ? C8 C9 C10 C9' 51.0(11) . . . . ? C8' C9' C10 O7 -132.7(11) . . . . ? C8' C9' C10 O6 72.9(14) . . . . ? C8' C9' C10 C9 -40.6(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2W H2B O4 0.88 2.11 2.972(11) 165.6 4_545 O2W H2A O2W 0.856(11) 2.726(18) 3.18(3) 115.1(16) 2_655 O1W H1B O7 0.97 2.32 2.775(17) 107.8 3_545 O1W H1A O2W 0.96 2.27 2.70(2) 106.0 . _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.827 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.107 #===============================END data_1.2H2O@93k _database_code_depnum_ccdc_archive 'CCDC 600567' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H7 Co2 N O7, 2(H2 O)' _chemical_formula_sum 'C10 H11 Co2 N O9' _chemical_formula_weight 407.06 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 Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.2260(17) _cell_length_b 10.1069(7) _cell_length_c 14.8903(11) _cell_angle_alpha 90.00 _cell_angle_beta 127.8080(10) _cell_angle_gamma 90.00 _cell_volume 2761.6(3) _cell_formula_units_Z 8 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.958 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 2.449 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7883 _exptl_absorpt_correction_T_max 0.8750 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8022 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 27.00 _reflns_number_total 2950 _reflns_number_gt 2598 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+27.7622P] 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 2950 _refine_ls_number_parameters 224 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1229 _refine_ls_wR_factor_gt 0.1179 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.073 _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 0.25710(3) 0.72063(6) 0.11542(5) 0.01390(16) Uani 1 1 d . . . Co2 Co 0.21528(3) 1.02933(6) 0.16912(5) 0.02117(18) Uani 1 1 d . . . C1 C 0.1048(2) 0.8387(5) -0.0094(4) 0.0199(9) Uani 1 1 d . . . C2 C 0.0244(2) 0.8214(5) -0.1024(4) 0.0200(9) Uani 1 1 d . . . C3 C -0.0079(3) 0.6977(5) -0.1399(4) 0.0258(10) Uani 1 1 d . . . H3 H 0.0211 0.6200 -0.1084 0.031 Uiso 1 1 calc R . . C4 C -0.0819(3) 0.6881(5) -0.2231(4) 0.0260(10) Uani 1 1 d . . . H4 H -0.1031 0.6024 -0.2456 0.031 Uiso 1 1 calc R . . C5 C -0.0941(3) 0.9129(5) -0.2403(4) 0.0263(10) Uani 1 1 d . . . H5 H -0.1238 0.9889 -0.2770 0.032 Uiso 1 1 calc R . . C6 C -0.0207(3) 0.9320(5) -0.1551(4) 0.0269(10) Uani 1 1 d . . . H6 H -0.0010 1.0188 -0.1327 0.032 Uiso 1 1 calc R . . C7 C 0.2933(3) 0.8235(5) 0.3363(4) 0.0240(10) Uani 1 1 d D . . C8 C 0.2954(6) 0.9467(8) 0.4002(8) 0.0261(18) Uani 0.630(12) 1 d PDU A 1 H8A H 0.3463 0.9817 0.4520 0.031 Uiso 0.630(12) 1 calc PR A 1 C9 C 0.2733(5) 0.8971(8) 0.4687(7) 0.0265(18) Uani 0.630(12) 1 d PU A 1 H9A H 0.3050 0.8210 0.5143 0.032 Uiso 0.630(12) 1 calc PR A 1 H9B H 0.2228 0.8633 0.4158 0.032 Uiso 0.630(12) 1 calc PR A 1 C8' C 0.2652(10) 0.9231(14) 0.3825(14) 0.033(3) Uani 0.370(12) 1 d PDU A 2 H8'A H 0.2189 0.8864 0.3635 0.040 Uiso 0.370(12) 1 calc PR A 2 C9' C 0.3184(9) 0.9379(14) 0.5098(13) 0.030(3) Uani 0.370(12) 1 d PU A 2 H9'A H 0.3588 0.9974 0.5308 0.037 Uiso 0.370(12) 1 calc PR A 2 H9'B H 0.3391 0.8507 0.5459 0.037 Uiso 0.370(12) 1 calc PR A 2 C10 C 0.2764(3) 0.9966(5) 0.5498(5) 0.0285(11) Uani 1 1 d . . . N1 N -0.1260(2) 0.7940(4) -0.2743(3) 0.0200(8) Uani 1 1 d . . . O1 O 0.14431(16) 0.7401(3) 0.0147(3) 0.0205(7) Uani 1 1 d . . . O2 O 0.12440(17) 0.9532(3) 0.0340(3) 0.0253(7) Uani 1 1 d . . . O3 O 0.26324(17) 0.8420(3) 0.2340(3) 0.0212(7) Uani 1 1 d . A . O4 O 0.3254(2) 0.7192(3) 0.3887(3) 0.0301(8) Uani 1 1 d . . . O5 O 0.24798(17) 1.0474(3) 0.3234(2) 0.0197(7) Uani 1 1 d . . . O7 O 0.2831(2) 0.9405(3) 0.6303(3) 0.0305(8) Uani 1 1 d . . . O6 O 0.25921(16) 1.1194(3) 0.5227(2) 0.0173(6) Uani 1 1 d . . . O1W O 0.4007(4) 0.7468(7) 0.7351(7) 0.115(3) Uani 1 1 d D . . H1A H 0.4397(6) 0.756(4) 0.8044(14) 0.138 Uiso 1 1 d D . . H1B H 0.3667 0.7909 0.7308 0.138 Uiso 1 1 d RD . . O2W O 0.5419(4) 0.7748(10) 0.8929(6) 0.122(3) Uani 1 1 d D . . H2A H 0.5470 0.7467 0.8436 0.147 Uiso 1 1 d RD . . H2B H 0.576(5) 0.741(11) 0.958(3) 0.147 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0117(3) 0.0164(3) 0.0134(3) 0.0014(2) 0.0076(2) 0.0020(2) Co2 0.0216(3) 0.0176(3) 0.0184(3) -0.0025(2) 0.0092(3) 0.0036(2) C1 0.015(2) 0.026(2) 0.019(2) 0.0001(18) 0.0106(18) 0.0003(18) C2 0.015(2) 0.025(2) 0.019(2) -0.0013(18) 0.0105(18) 0.0007(17) C3 0.020(2) 0.020(2) 0.032(2) -0.001(2) 0.013(2) 0.0046(18) C4 0.024(2) 0.019(2) 0.034(3) -0.008(2) 0.017(2) -0.0040(18) C5 0.019(2) 0.021(2) 0.034(3) 0.006(2) 0.014(2) 0.0026(19) C6 0.018(2) 0.021(2) 0.032(3) 0.002(2) 0.011(2) -0.0011(18) C7 0.028(2) 0.021(2) 0.023(2) -0.0050(19) 0.016(2) -0.0075(19) C8 0.029(4) 0.020(4) 0.029(4) -0.009(3) 0.017(4) -0.006(3) C9 0.026(4) 0.026(4) 0.029(4) 0.000(3) 0.018(3) 0.001(3) C8' 0.029(6) 0.025(5) 0.030(5) 0.008(4) 0.010(5) -0.011(5) C9' 0.029(5) 0.025(5) 0.033(5) -0.001(4) 0.016(4) -0.002(4) C10 0.027(3) 0.028(3) 0.039(3) -0.005(2) 0.024(2) 0.003(2) N1 0.0171(18) 0.023(2) 0.0203(18) -0.0019(15) 0.0119(16) -0.0020(15) O1 0.0141(14) 0.0173(15) 0.0260(16) 0.0008(13) 0.0102(13) 0.0030(12) O2 0.0156(15) 0.0221(17) 0.0249(17) -0.0047(14) 0.0056(13) 0.0014(13) O3 0.0254(17) 0.0160(15) 0.0229(16) -0.0039(13) 0.0152(14) 0.0016(13) O4 0.037(2) 0.0221(17) 0.0183(16) -0.0031(14) 0.0108(15) -0.0084(15) O5 0.0245(16) 0.0143(15) 0.0152(14) 0.0017(12) 0.0095(13) 0.0026(12) O7 0.0323(19) 0.0250(18) 0.042(2) 0.0089(16) 0.0267(18) 0.0071(15) O6 0.0171(15) 0.0176(15) 0.0177(15) -0.0034(12) 0.0109(13) -0.0038(12) O1W 0.080(5) 0.081(5) 0.111(6) -0.003(4) 0.021(4) 0.016(4) O2W 0.077(5) 0.163(8) 0.076(5) 0.031(5) 0.020(4) -0.003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O5 2.010(3) 4_545 ? Co1 O3 2.081(3) . ? Co1 O1 2.082(3) . ? Co1 O6 2.113(3) 4_545 ? Co1 O6 2.146(3) 6_575 ? Co1 N1 2.150(4) 8_566 ? Co2 O5 1.936(3) . ? Co2 O2 1.972(3) . ? Co2 O7 2.006(4) 6_575 ? Co2 O4 2.079(3) 4 ? Co2 O3 2.107(3) . ? C1 O1 1.249(5) . ? C1 O2 1.267(6) . ? C1 C2 1.505(6) . ? C2 C3 1.387(7) . ? C2 C6 1.398(7) . ? C3 C4 1.375(7) . ? C3 H3 0.9500 . ? C4 N1 1.348(6) . ? C4 H4 0.9500 . ? C5 N1 1.339(6) . ? C5 C6 1.379(7) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 O3 1.240(6) . ? C7 O4 1.250(6) . ? C7 C8 1.550(7) . ? C7 C8' 1.570(9) . ? C8 O5 1.419(10) . ? C8 C9 1.480(13) . ? C8 H8A 1.0000 . ? C9 C10 1.539(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C8' O5 1.443(16) . ? C8' C9' 1.51(2) . ? C8' H8'A 1.0000 . ? C9' C10 1.538(16) . ? C9' H9'A 0.9900 . ? C9' H9'B 0.9900 . ? C10 O7 1.248(6) . ? C10 O6 1.291(6) . ? N1 Co1 2.150(4) 8_465 ? O4 Co2 2.079(3) 4_545 ? O5 Co1 2.010(3) 4 ? O7 Co2 2.006(4) 6_576 ? O6 Co1 2.113(3) 4 ? O6 Co1 2.146(3) 6_576 ? O1W H1A 0.864(10) . ? O1W H1B 0.8744 . ? O2W H2A 0.8607 . ? O2W H2B 0.863(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 O5 Co1 O3 96.97(13) 4_545 . ? O5 Co1 O1 90.65(13) 4_545 . ? O3 Co1 O1 87.54(13) . . ? O5 Co1 O6 89.68(12) 4_545 4_545 ? O3 Co1 O6 171.49(12) . 4_545 ? O1 Co1 O6 87.07(12) . 4_545 ? O5 Co1 O6 168.11(12) 4_545 6_575 ? O3 Co1 O6 94.88(12) . 6_575 ? O1 Co1 O6 88.86(12) . 6_575 ? O6 Co1 O6 78.44(13) 4_545 6_575 ? O5 Co1 N1 89.53(14) 4_545 8_566 ? O3 Co1 N1 89.70(13) . 8_566 ? O1 Co1 N1 177.24(14) . 8_566 ? O6 Co1 N1 95.69(13) 4_545 8_566 ? O6 Co1 N1 91.53(13) 6_575 8_566 ? O5 Co2 O2 130.05(15) . . ? O5 Co2 O7 121.41(15) . 6_575 ? O2 Co2 O7 107.69(15) . 6_575 ? O5 Co2 O4 98.78(13) . 4 ? O2 Co2 O4 90.39(14) . 4 ? O7 Co2 O4 88.74(15) 6_575 4 ? O5 Co2 O3 80.12(12) . . ? O2 Co2 O3 92.96(13) . . ? O7 Co2 O3 88.90(14) 6_575 . ? O4 Co2 O3 176.37(14) 4 . ? O1 C1 O2 127.7(4) . . ? O1 C1 C2 116.8(4) . . ? O2 C1 C2 115.5(4) . . ? C3 C2 C6 117.4(4) . . ? C3 C2 C1 122.3(4) . . ? C6 C2 C1 120.2(4) . . ? C4 C3 C2 119.7(4) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? N1 C4 C3 123.4(4) . . ? N1 C4 H4 118.3 . . ? C3 C4 H4 118.3 . . ? N1 C5 C6 124.0(4) . . ? N1 C5 H5 118.0 . . ? C6 C5 H5 118.0 . . ? C5 C6 C2 118.9(4) . . ? C5 C6 H6 120.6 . . ? C2 C6 H6 120.6 . . ? O3 C7 O4 124.4(4) . . ? O3 C7 C8 114.6(5) . . ? O4 C7 C8 120.7(5) . . ? O3 C7 C8' 111.7(7) . . ? O4 C7 C8' 121.0(7) . . ? C8 C7 C8' 23.1(5) . . ? O5 C8 C9 112.0(8) . . ? O5 C8 C7 111.4(6) . . ? C9 C8 C7 104.9(7) . . ? O5 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? C8 C9 C10 116.7(7) . . ? C8 C9 H9A 108.1 . . ? C10 C9 H9A 108.1 . . ? C8 C9 H9B 108.1 . . ? C10 C9 H9B 108.1 . . ? H9A C9 H9B 107.3 . . ? O5 C8' C9' 112.8(12) . . ? O5 C8' C7 108.9(9) . . ? C9' C8' C7 112.0(12) . . ? O5 C8' H8'A 107.6 . . ? C9' C8' H8'A 107.6 . . ? C7 C8' H8'A 107.6 . . ? C8' C9' C10 107.4(11) . . ? C8' C9' H9'A 110.2 . . ? C10 C9' H9'A 110.2 . . ? C8' C9' H9'B 110.2 . . ? C10 C9' H9'B 110.2 . . ? H9'A C9' H9'B 108.5 . . ? O7 C10 O6 124.7(4) . . ? O7 C10 C9' 117.5(7) . . ? O6 C10 C9' 113.5(7) . . ? O7 C10 C9 112.1(5) . . ? O6 C10 C9 121.8(5) . . ? C9' C10 C9 35.0(6) . . ? C5 N1 C4 116.5(4) . . ? C5 N1 Co1 119.9(3) . 8_465 ? C4 N1 Co1 122.9(3) . 8_465 ? C1 O1 Co1 131.4(3) . . ? C1 O2 Co2 134.6(3) . . ? C7 O3 Co1 130.3(3) . . ? C7 O3 Co2 116.1(3) . . ? Co1 O3 Co2 113.50(15) . . ? C7 O4 Co2 125.0(3) . 4_545 ? C8 O5 C8' 25.2(6) . . ? C8 O5 Co2 115.8(3) . . ? C8' O5 Co2 113.7(5) . . ? C8 O5 Co1 119.4(3) . 4 ? C8' O5 Co1 123.6(5) . 4 ? Co2 O5 Co1 122.05(15) . 4 ? C10 O7 Co2 123.4(3) . 6_576 ? C10 O6 Co1 127.3(3) . 4 ? C10 O6 Co1 130.4(3) . 6_576 ? Co1 O6 Co1 101.56(13) 4 6_576 ? H1A O1W H1B 105.8 . . ? H2A O2W H2B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 16.3(6) . . . . ? O2 C1 C2 C3 -164.7(4) . . . . ? O1 C1 C2 C6 -163.0(4) . . . . ? O2 C1 C2 C6 16.0(6) . . . . ? C6 C2 C3 C4 -2.4(7) . . . . ? C1 C2 C3 C4 178.3(5) . . . . ? C2 C3 C4 N1 2.3(8) . . . . ? N1 C5 C6 C2 1.9(8) . . . . ? C3 C2 C6 C5 0.5(7) . . . . ? C1 C2 C6 C5 179.8(4) . . . . ? O3 C7 C8 O5 13.3(10) . . . . ? O4 C7 C8 O5 -172.3(6) . . . . ? C8' C7 C8 O5 -75(2) . . . . ? O3 C7 C8 C9 134.6(6) . . . . ? O4 C7 C8 C9 -51.0(9) . . . . ? C8' C7 C8 C9 46.7(19) . . . . ? O5 C8 C9 C10 -63.9(9) . . . . ? C7 C8 C9 C10 175.1(6) . . . . ? O3 C7 C8' O5 -33.0(14) . . . . ? O4 C7 C8' O5 165.3(7) . . . . ? C8 C7 C8' O5 68.9(18) . . . . ? O3 C7 C8' C9' -158.5(11) . . . . ? O4 C7 C8' C9' 39.9(16) . . . . ? C8 C7 C8' C9' -56.5(19) . . . . ? O5 C8' C9' C10 75.6(14) . . . . ? C7 C8' C9' C10 -161.2(10) . . . . ? C8' C9' C10 O7 130.4(10) . . . . ? C8' C9' C10 O6 -71.7(12) . . . . ? C8' C9' C10 C9 40.7(10) . . . . ? C8 C9 C10 O7 -155.8(7) . . . . ? C8 C9 C10 O6 37.0(10) . . . . ? C8 C9 C10 C9' -49.0(11) . . . . ? C6 C5 N1 C4 -2.1(7) . . . . ? C6 C5 N1 Co1 168.3(4) . . . 8_465 ? C3 C4 N1 C5 0.0(7) . . . . ? C3 C4 N1 Co1 -170.1(4) . . . 8_465 ? O2 C1 O1 Co1 -9.8(7) . . . . ? C2 C1 O1 Co1 169.1(3) . . . . ? O5 Co1 O1 C1 140.7(4) 4_545 . . . ? O3 Co1 O1 C1 43.8(4) . . . . ? O6 Co1 O1 C1 -129.7(4) 4_545 . . . ? O6 Co1 O1 C1 -51.2(4) 6_575 . . . ? N1 Co1 O1 C1 47(3) 8_566 . . . ? O1 C1 O2 Co2 -12.5(8) . . . . ? C2 C1 O2 Co2 168.6(3) . . . . ? O5 Co2 O2 C1 -89.7(5) . . . . ? O7 Co2 O2 C1 79.7(5) 6_575 . . . ? O4 Co2 O2 C1 168.5(4) 4 . . . ? O3 Co2 O2 C1 -10.1(5) . . . . ? O4 C7 O3 Co1 -2.7(7) . . . . ? C8 C7 O3 Co1 171.4(5) . . . . ? C8' C7 O3 Co1 -163.6(8) . . . . ? O4 C7 O3 Co2 -178.8(4) . . . . ? C8 C7 O3 Co2 -4.6(7) . . . . ? C8' C7 O3 Co2 20.4(9) . . . . ? O5 Co1 O3 C7 34.9(4) 4_545 . . . ? O1 Co1 O3 C7 125.2(4) . . . . ? O6 Co1 O3 C7 176.0(7) 4_545 . . . ? O6 Co1 O3 C7 -146.1(4) 6_575 . . . ? N1 Co1 O3 C7 -54.6(4) 8_566 . . . ? O5 Co1 O3 Co2 -149.03(15) 4_545 . . . ? O1 Co1 O3 Co2 -58.67(16) . . . . ? O6 Co1 O3 Co2 -7.9(9) 4_545 . . . ? O6 Co1 O3 Co2 29.98(16) 6_575 . . . ? N1 Co1 O3 Co2 121.49(17) 8_566 . . . ? O5 Co2 O3 C7 -3.2(3) . . . . ? O2 Co2 O3 C7 -133.4(3) . . . . ? O7 Co2 O3 C7 118.9(3) 6_575 . . . ? O4 Co2 O3 C7 69(2) 4 . . . ? O5 Co2 O3 Co1 -179.92(18) . . . . ? O2 Co2 O3 Co1 49.91(17) . . . . ? O7 Co2 O3 Co1 -57.75(17) 6_575 . . . ? O4 Co2 O3 Co1 -107(2) 4 . . . ? O3 C7 O4 Co2 -46.4(7) . . . 4_545 ? C8 C7 O4 Co2 139.8(6) . . . 4_545 ? C8' C7 O4 Co2 112.8(9) . . . 4_545 ? C9 C8 O5 C8' -42.0(14) . . . . ? C7 C8 O5 C8' 75.1(13) . . . . ? C9 C8 O5 Co2 -133.3(5) . . . . ? C7 C8 O5 Co2 -16.2(9) . . . . ? C9 C8 O5 Co1 65.0(8) . . . 4 ? C7 C8 O5 Co1 -177.9(4) . . . 4 ? C9' C8' O5 C8 55.1(17) . . . . ? C7 C8' O5 C8 -69.9(12) . . . . ? C9' C8' O5 Co2 155.6(9) . . . . ? C7 C8' O5 Co2 30.6(13) . . . . ? C9' C8' O5 Co1 -33.5(15) . . . 4 ? C7 C8' O5 Co1 -158.5(6) . . . 4 ? O2 Co2 O5 C8 96.6(6) . . . . ? O7 Co2 O5 C8 -71.5(6) 6_575 . . . ? O4 Co2 O5 C8 -165.5(5) 4 . . . ? O3 Co2 O5 C8 11.0(5) . . . . ? O2 Co2 O5 C8' 68.8(8) . . . . ? O7 Co2 O5 C8' -99.3(8) 6_575 . . . ? O4 Co2 O5 C8' 166.8(8) 4 . . . ? O3 Co2 O5 C8' -16.7(8) . . . . ? O2 Co2 O5 Co1 -102.2(2) . . . 4 ? O7 Co2 O5 Co1 89.7(2) 6_575 . . 4 ? O4 Co2 O5 Co1 -4.2(2) 4 . . 4 ? O3 Co2 O5 Co1 172.3(2) . . . 4 ? O6 C10 O7 Co2 41.0(7) . . . 6_576 ? C9' C10 O7 Co2 -163.9(7) . . . 6_576 ? C9 C10 O7 Co2 -125.7(5) . . . 6_576 ? O7 C10 O6 Co1 -177.5(4) . . . 4 ? C9' C10 O6 Co1 26.5(8) . . . 4 ? C9 C10 O6 Co1 -12.1(7) . . . 4 ? O7 C10 O6 Co1 13.9(7) . . . 6_576 ? C9' C10 O6 Co1 -142.1(7) . . . 6_576 ? C9 C10 O6 Co1 179.4(4) . . . 6_576 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2W H2A O1W 0.86 2.14 2.934(14) 152.6 2_656 O2W H2B O4 0.863(10) 2.02(5) 2.846(8) 160(13) 2_656 O1W H1B O7 0.87 2.18 2.916(8) 142.3 . O1W H1A O2W 0.864(10) 1.891(11) 2.627(10) 142(2) . _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.163 _refine_diff_density_min -0.716 _refine_diff_density_rms 0.135 #===============================END data_1.MeOH@293k _database_code_depnum_ccdc_archive 'CCDC 600568' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H7 Co2 N O7, C H4 O' _chemical_formula_sum 'C11 H11 Co2 N O8' _chemical_formula_weight 403.07 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 Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.46(2) _cell_length_b 10.094(9) _cell_length_c 15.044(14) _cell_angle_alpha 90.00 _cell_angle_beta 128.249(13) _cell_angle_gamma 90.00 _cell_volume 2798(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 784 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 25.69 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.914 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 2.412 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6190 _exptl_absorpt_correction_T_max 0.7607 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6933 _diffrn_reflns_av_R_equivalents 0.0601 _diffrn_reflns_av_sigmaI/netI 0.0755 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.93 _reflns_number_total 2699 _reflns_number_gt 1950 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0823P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2699 _refine_ls_number_parameters 227 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1438 _refine_ls_wR_factor_gt 0.1286 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.005 _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 0.24398(3) 0.72280(7) 0.10270(5) 0.0222(2) Uani 1 1 d . . . Co2 Co 0.28379(4) 1.03435(7) 0.23454(6) 0.0292(2) Uani 1 1 d . . . C1 C 0.3955(3) 0.8411(6) 0.2778(4) 0.0296(12) Uani 1 1 d . . . C2 C 0.4769(3) 0.8227(6) 0.3492(4) 0.0303(12) Uani 1 1 d . . . C3 C 0.5082(3) 0.7002(6) 0.3751(5) 0.0429(15) Uani 1 1 d . . . H3A H 0.4794 0.6245 0.3483 0.051 Uiso 1 1 calc R . . C4 C 0.5831(3) 0.6895(6) 0.4416(5) 0.0412(15) Uani 1 1 d . . . H4A H 0.6034 0.6052 0.4576 0.049 Uiso 1 1 calc R . . C5 C 0.5961(3) 0.9131(6) 0.4560(6) 0.0496(17) Uani 1 1 d . . . H5A H 0.6255 0.9878 0.4816 0.060 Uiso 1 1 calc R . . C6 C 0.5214(3) 0.9308(6) 0.3905(6) 0.0498(17) Uani 1 1 d . . . H6A H 0.5019 1.0156 0.3751 0.060 Uiso 1 1 calc R . . C7 C 0.2045(3) 0.8279(6) 0.2481(4) 0.0309(12) Uani 1 1 d . B . C8 C 0.2101(6) 0.9444(7) 0.3187(9) 0.071(3) Uani 1 1 d D . . H8A H 0.1635 0.9827 0.2556 0.085 Uiso 1 1 calc R A 1 C9 C 0.1886(14) 0.927(2) 0.3852(18) 0.091(8) Uani 0.50 1 d PD B 1 H9A H 0.1910 0.8325 0.3992 0.109 Uiso 0.50 1 calc PR B 1 H9B H 0.1377 0.9511 0.3387 0.109 Uiso 0.50 1 calc PR B 1 C9' C 0.2292(7) 0.9001(15) 0.4226(10) 0.031(3) Uani 0.50 1 d PD B 2 H9'A H 0.2787 0.8678 0.4673 0.037 Uiso 0.50 1 calc PR B 2 H9'B H 0.1986 0.8245 0.4067 0.037 Uiso 0.50 1 calc PR B 2 C10 C 0.2249(3) 0.9943(6) 0.4971(5) 0.0356(13) Uani 1 1 d . . . N1 N 0.6278(2) 0.7938(4) 0.4840(4) 0.0298(10) Uani 1 1 d . . . O1 O 0.35650(18) 0.7450(4) 0.2201(3) 0.0319(9) Uani 1 1 d . . . O2 O 0.3755(2) 0.9542(4) 0.2831(4) 0.0465(11) Uani 1 1 d . . . O3 O 0.23475(19) 0.8469(4) 0.2038(3) 0.0312(8) Uani 1 1 d . . . O4 O 0.1733(2) 0.7237(4) 0.2397(4) 0.0401(10) Uani 1 1 d . . . O5 O 0.25069(19) 1.0506(3) 0.3243(3) 0.0269(8) Uani 1 1 d . . . O7 O 0.2212(2) 0.9374(4) 0.5670(3) 0.0450(11) Uani 1 1 d . . . O6 O 0.23964(17) 1.1185(3) 0.5028(3) 0.0255(8) Uani 1 1 d . . . C11 C 0.532(2) 0.348(5) 0.380(5) 0.34(5) Uani 0.50 1 d PD C 3 H11A H 0.5386 0.3700 0.4484 0.503 Uiso 0.50 1 calc PR C 3 H11B H 0.5251 0.4272 0.3399 0.503 Uiso 0.50 1 calc PR C 3 H11C H 0.5734 0.3006 0.3990 0.503 Uiso 0.50 1 calc PR C 3 O8 O 0.4691(14) 0.266(3) 0.311(3) 0.217(16) Uani 0.50 1 d PD C 3 H8B H 0.4371 0.2501 0.2442 0.325 Uiso 0.50 1 d PR C 3 C11' C 0.527(3) 0.322(5) 0.433(5) 0.32(5) Uani 0.50 1 d PD D 4 H11D H 0.5355 0.4020 0.4746 0.485 Uiso 0.50 1 calc PR D 4 H11E H 0.5008 0.2603 0.4453 0.485 Uiso 0.50 1 calc PR D 4 H11F H 0.4981 0.3418 0.3540 0.485 Uiso 0.50 1 calc PR D 4 O8' O 0.594(3) 0.265(4) 0.472(7) 0.55(7) Uani 0.50 1 d PD D 4 H8C H 0.6239 0.3243 0.4939 0.818 Uiso 0.50 1 calc PR D 4 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 0.0208(4) 0.0212(4) 0.0260(4) -0.0010(3) 0.0152(3) -0.0016(3) Co2 0.0307(4) 0.0228(4) 0.0412(5) -0.0039(3) 0.0258(4) -0.0010(3) C1 0.021(2) 0.030(3) 0.037(3) 0.003(2) 0.018(2) 0.003(2) C2 0.023(3) 0.032(3) 0.032(3) -0.002(2) 0.015(2) 0.003(2) C3 0.022(3) 0.032(3) 0.060(4) -0.007(3) 0.018(3) -0.004(2) C4 0.032(3) 0.029(3) 0.054(4) 0.001(3) 0.022(3) 0.003(2) C5 0.026(3) 0.030(3) 0.066(4) 0.002(3) 0.015(3) 0.002(3) C6 0.027(3) 0.028(3) 0.067(4) 0.000(3) 0.015(3) 0.001(3) C7 0.033(3) 0.029(3) 0.037(3) -0.001(2) 0.024(3) 0.002(2) C8 0.126(7) 0.035(4) 0.118(7) -0.023(4) 0.109(7) -0.024(4) C9 0.15(2) 0.086(17) 0.099(17) -0.055(13) 0.107(18) -0.090(17) C9' 0.033(7) 0.018(5) 0.040(7) -0.006(5) 0.022(6) 0.001(6) C10 0.045(3) 0.030(3) 0.035(3) -0.007(3) 0.026(3) -0.003(3) N1 0.022(2) 0.033(3) 0.034(2) 0.001(2) 0.017(2) 0.0000(19) O1 0.0208(18) 0.029(2) 0.039(2) -0.0036(16) 0.0151(17) -0.0011(16) O2 0.028(2) 0.029(2) 0.070(3) -0.0093(19) 0.025(2) 0.0008(17) O3 0.036(2) 0.0235(19) 0.042(2) -0.0093(17) 0.0287(18) -0.0049(17) O4 0.049(2) 0.025(2) 0.068(3) 0.0057(19) 0.047(2) 0.0042(19) O5 0.034(2) 0.0135(17) 0.042(2) -0.0033(14) 0.0277(18) -0.0052(14) O7 0.059(3) 0.035(2) 0.039(2) -0.0033(18) 0.029(2) -0.014(2) O6 0.0274(18) 0.0251(19) 0.0298(18) 0.0002(15) 0.0206(15) 0.0005(15) C11 0.18(4) 0.30(6) 0.50(9) -0.33(7) 0.20(6) -0.10(4) O8 0.20(3) 0.24(3) 0.32(4) 0.13(3) 0.22(3) 0.09(3) C11' 0.63(14) 0.19(5) 0.52(12) -0.01(6) 0.54(13) -0.09(7) O8' 0.53(7) 0.14(3) 1.4(2) 0.09(5) 0.78(12) 0.01(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O5 2.018(4) 4_545 ? Co1 O3 2.083(4) . ? Co1 O1 2.089(4) . ? Co1 O6 2.129(4) 4_545 ? Co1 N1 2.150(5) 8_465 ? Co1 O6 2.156(4) 6_575 ? Co2 O5 1.936(4) . ? Co2 O2 1.968(4) . ? Co2 O7 2.001(5) 6_575 ? Co2 O4 2.082(4) 4 ? Co2 O3 2.111(4) . ? C1 O1 1.244(7) . ? C1 O2 1.255(7) . ? C1 C2 1.515(7) . ? C2 C6 1.365(8) . ? C2 C3 1.365(8) . ? C3 C4 1.388(8) . ? C3 H3A 0.9300 . ? C4 N1 1.336(7) . ? C4 H4A 0.9300 . ? C5 N1 1.338(7) . ? C5 C6 1.392(8) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 O4 1.242(7) . ? C7 O3 1.253(6) . ? C7 C8 1.536(9) . ? C8 C9 1.382(14) . ? C8 O5 1.402(7) . ? C8 C9' 1.406(14) . ? C8 H8A 0.9800 . ? C9 C10 1.499(18) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9' C10 1.519(15) . ? C9' H9'A 0.9700 . ? C9' H9'B 0.9700 . ? C10 O7 1.248(7) . ? C10 O6 1.289(7) . ? N1 Co1 2.150(5) 8_566 ? O4 Co2 2.082(4) 4_545 ? O5 Co1 2.018(4) 4 ? O7 Co2 2.001(5) 6_576 ? O6 Co1 2.129(4) 4 ? O6 Co1 2.156(4) 6_576 ? C11 O8 1.419(9) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? O8 H8B 0.8196 . ? C11' O8' 1.419(10) . ? C11' H11D 0.9600 . ? C11' H11E 0.9600 . ? C11' H11F 0.9600 . ? O8' H8C 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Co1 O3 96.89(16) 4_545 . ? O5 Co1 O1 90.69(15) 4_545 . ? O3 Co1 O1 88.05(15) . . ? O5 Co1 O6 90.05(15) 4_545 4_545 ? O3 Co1 O6 172.10(14) . 4_545 ? O1 Co1 O6 88.11(15) . 4_545 ? O5 Co1 N1 90.25(16) 4_545 8_465 ? O3 Co1 N1 90.12(16) . 8_465 ? O1 Co1 N1 178.03(16) . 8_465 ? O6 Co1 N1 93.63(16) 4_545 8_465 ? O5 Co1 O6 168.49(13) 4_545 6_575 ? O3 Co1 O6 94.62(15) . 6_575 ? O1 Co1 O6 89.97(14) . 6_575 ? O6 Co1 O6 78.48(16) 4_545 6_575 ? N1 Co1 O6 89.46(16) 8_465 6_575 ? O5 Co2 O2 126.45(18) . . ? O5 Co2 O7 124.58(18) . 6_575 ? O2 Co2 O7 107.90(19) . 6_575 ? O5 Co2 O4 98.56(15) . 4 ? O2 Co2 O4 90.97(17) . 4 ? O7 Co2 O4 89.80(17) 6_575 4 ? O5 Co2 O3 80.16(14) . . ? O2 Co2 O3 92.02(16) . . ? O7 Co2 O3 88.67(16) 6_575 . ? O4 Co2 O3 176.94(15) 4 . ? O1 C1 O2 127.6(5) . . ? O1 C1 C2 117.3(5) . . ? O2 C1 C2 115.1(5) . . ? C6 C2 C3 118.1(5) . . ? C6 C2 C1 119.8(5) . . ? C3 C2 C1 122.1(5) . . ? C2 C3 C4 119.5(6) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? N1 C4 C3 123.4(6) . . ? N1 C4 H4A 118.3 . . ? C3 C4 H4A 118.3 . . ? N1 C5 C6 123.3(6) . . ? N1 C5 H5A 118.4 . . ? C6 C5 H5A 118.4 . . ? C2 C6 C5 119.5(6) . . ? C2 C6 H6A 120.3 . . ? C5 C6 H6A 120.3 . . ? O4 C7 O3 124.7(5) . . ? O4 C7 C8 120.7(5) . . ? O3 C7 C8 114.6(5) . . ? C9 C8 O5 126.4(10) . . ? O5 C8 C9' 116.1(10) . . ? C9 C8 C7 119.3(10) . . ? O5 C8 C7 113.0(5) . . ? C9' C8 C7 111.0(8) . . ? C9 C8 H8A 93.7 . . ? O5 C8 H8A 93.7 . . ? C9' C8 H8A 126.9 . . ? C7 C8 H8A 93.7 . . ? C8 C9 C10 123.1(13) . . ? C8 C9 H9A 106.6 . . ? C10 C9 H9A 106.6 . . ? C8 C9 H9B 106.6 . . ? C10 C9 H9B 106.6 . . ? H9A C9 H9B 106.5 . . ? C8 C9' C10 120.0(10) . . ? C8 C9' H9'A 107.3 . . ? C10 C9' H9'A 107.3 . . ? C8 C9' H9'B 107.3 . . ? C10 C9' H9'B 107.3 . . ? H9'A C9' H9'B 106.9 . . ? O7 C10 O6 123.2(5) . . ? O7 C10 C9 116.7(8) . . ? O6 C10 C9 117.3(9) . . ? O7 C10 C9' 113.8(7) . . ? O6 C10 C9' 121.3(7) . . ? C4 N1 C5 116.2(5) . . ? C4 N1 Co1 123.4(4) . 8_566 ? C5 N1 Co1 120.2(4) . 8_566 ? C1 O1 Co1 132.2(3) . . ? C1 O2 Co2 135.8(4) . . ? C7 O3 Co1 130.2(4) . . ? C7 O3 Co2 115.6(3) . . ? Co1 O3 Co2 114.20(17) . . ? C7 O4 Co2 124.9(4) . 4_545 ? C8 O5 Co2 116.4(3) . . ? C8 O5 Co1 120.1(3) . 4 ? Co2 O5 Co1 122.41(17) . 4 ? C10 O7 Co2 128.0(4) . 6_576 ? C10 O6 Co1 126.6(3) . 4 ? C10 O6 Co1 131.6(3) . 6_576 ? Co1 O6 Co1 101.51(16) 4 6_576 ? O8 C11 H11A 109.5 . . ? O8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C11 O8 H8B 139.5 . . ? O8' C11' H11D 109.5 . . ? O8' C11' H11E 109.5 . . ? H11D C11' H11E 109.5 . . ? O8' C11' H11F 109.5 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? C11' O8' H8C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C6 163.1(6) . . . . ? O2 C1 C2 C6 -15.8(8) . . . . ? O1 C1 C2 C3 -17.5(8) . . . . ? O2 C1 C2 C3 163.6(6) . . . . ? C6 C2 C3 C4 0.0(10) . . . . ? C1 C2 C3 C4 -179.4(6) . . . . ? C2 C3 C4 N1 0.7(10) . . . . ? C3 C2 C6 C5 0.6(10) . . . . ? C1 C2 C6 C5 -180.0(6) . . . . ? N1 C5 C6 C2 -1.9(12) . . . . ? O4 C7 C8 C9 8.4(18) . . . . ? O3 C7 C8 C9 -170.1(15) . . . . ? O4 C7 C8 O5 176.4(6) . . . . ? O3 C7 C8 O5 -2.1(10) . . . . ? O4 C7 C8 C9' 44.0(11) . . . . ? O3 C7 C8 C9' -134.5(8) . . . . ? O5 C8 C9 C10 -21(3) . . . . ? C9' C8 C9 C10 62(2) . . . . ? C7 C8 C9 C10 145.7(16) . . . . ? C9 C8 C9' C10 -57.4(19) . . . . ? O5 C8 C9' C10 60.0(13) . . . . ? C7 C8 C9' C10 -169.2(9) . . . . ? C8 C9 C10 O7 -153.6(18) . . . . ? C8 C9 C10 O6 45(3) . . . . ? C8 C9 C10 C9' -61.4(17) . . . . ? C8 C9' C10 O7 159.3(10) . . . . ? C8 C9' C10 O6 -34.8(14) . . . . ? C8 C9' C10 C9 56.6(15) . . . . ? C3 C4 N1 C5 -1.9(9) . . . . ? C3 C4 N1 Co1 172.5(5) . . . 8_566 ? C6 C5 N1 C4 2.5(10) . . . . ? C6 C5 N1 Co1 -172.1(6) . . . 8_566 ? O2 C1 O1 Co1 3.1(9) . . . . ? C2 C1 O1 Co1 -175.7(3) . . . . ? O5 Co1 O1 C1 -133.8(5) 4_545 . . . ? O3 Co1 O1 C1 -37.0(5) . . . . ? O6 Co1 O1 C1 136.2(5) 4_545 . . . ? O6 Co1 O1 C1 57.7(5) 6_575 . . . ? O1 C1 O2 Co2 12.9(10) . . . . ? C2 C1 O2 Co2 -168.3(4) . . . . ? O5 Co2 O2 C1 92.3(6) . . . . ? O7 Co2 O2 C1 -76.2(6) 6_575 . . . ? O4 Co2 O2 C1 -166.3(6) 4 . . . ? O3 Co2 O2 C1 13.1(6) . . . . ? O4 C7 O3 Co1 0.9(8) . . . . ? C8 C7 O3 Co1 179.4(5) . . . . ? O4 C7 O3 Co2 -179.6(4) . . . . ? C8 C7 O3 Co2 -1.1(7) . . . . ? O5 Co1 O3 C7 -33.3(5) 4_545 . . . ? O1 Co1 O3 C7 -123.7(5) . . . . ? N1 Co1 O3 C7 57.0(5) 8_465 . . . ? O6 Co1 O3 C7 146.5(5) 6_575 . . . ? O5 Co1 O3 Co2 147.25(18) 4_545 . . . ? O1 Co1 O3 Co2 56.79(19) . . . . ? N1 Co1 O3 Co2 -122.5(2) 8_465 . . . ? O6 Co1 O3 Co2 -33.02(18) 6_575 . . . ? O5 Co2 O3 C7 2.8(4) . . . . ? O2 Co2 O3 C7 129.5(4) . . . . ? O7 Co2 O3 C7 -122.6(4) 6_575 . . . ? O5 Co2 O3 Co1 -177.6(2) . . . . ? O2 Co2 O3 Co1 -50.9(2) . . . . ? O7 Co2 O3 Co1 57.0(2) 6_575 . . . ? O3 C7 O4 Co2 47.9(8) . . . 4_545 ? C8 C7 O4 Co2 -130.5(6) . . . 4_545 ? C9 C8 O5 Co2 171.6(17) . . . . ? C9' C8 O5 Co2 134.4(7) . . . . ? C7 C8 O5 Co2 4.6(9) . . . . ? C9 C8 O5 Co1 -20.0(19) . . . 4 ? C9' C8 O5 Co1 -57.1(10) . . . 4 ? C7 C8 O5 Co1 173.0(5) . . . 4 ? O2 Co2 O5 C8 -89.2(6) . . . . ? O7 Co2 O5 C8 77.5(6) 6_575 . . . ? O4 Co2 O5 C8 173.2(5) 4 . . . ? O3 Co2 O5 C8 -4.0(5) . . . . ? O2 Co2 O5 Co1 102.6(2) . . . 4 ? O7 Co2 O5 Co1 -90.7(2) 6_575 . . 4 ? O4 Co2 O5 Co1 5.0(2) 4 . . 4 ? O3 Co2 O5 Co1 -172.2(2) . . . 4 ? O6 C10 O7 Co2 -38.3(8) . . . 6_576 ? C9 C10 O7 Co2 161.1(13) . . . 6_576 ? C9' C10 O7 Co2 127.3(6) . . . 6_576 ? O7 C10 O6 Co1 174.5(4) . . . 4 ? C9 C10 O6 Co1 -24.9(13) . . . 4 ? C9' C10 O6 Co1 10.0(8) . . . 4 ? O7 C10 O6 Co1 -12.4(8) . . . 6_576 ? C9 C10 O6 Co1 148.2(11) . . . 6_576 ? C9' C10 O6 Co1 -176.9(6) . . . 6_576 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8 H8B O4 0.82 2.76 2.96(2) 96.1 4_545 O8 H8B O8 0.82 2.80 2.97(5) 93.7 2_655 O8' H8C O7 0.82 2.15 2.95(4) 165.6 3_545 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.93 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.722 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.136 #===============================END data_1.MeOH@93k _database_code_depnum_ccdc_archive 'CCDC 600569' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H7 Co2 N O7, C H4 O' _chemical_formula_sum 'C11 H11 Co2 N O8' _chemical_formula_weight 403.07 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 Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.5214(17) _cell_length_b 10.0276(7) _cell_length_c 14.9851(11) _cell_angle_alpha 90.00 _cell_angle_beta 128.6180(10) _cell_angle_gamma 90.00 _cell_volume 2761.5(3) _cell_formula_units_Z 8 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour PURPLE _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.939 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 2.443 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7402 _exptl_absorpt_correction_T_max 0.8814 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7738 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.02 _reflns_number_total 2947 _reflns_number_gt 2599 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+13.6110P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2947 _refine_ls_number_parameters 229 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1458 _refine_ls_wR_factor_gt 0.1420 _refine_ls_goodness_of_fit_ref 1.218 _refine_ls_restrained_S_all 1.231 _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 0.24435(3) 0.72232(6) 0.10222(5) 0.01150(19) Uani 1 1 d . . . Co2 Co 0.28452(4) 1.03394(6) 0.23625(6) 0.0167(2) Uani 1 1 d . . . C1 C 0.3959(3) 0.8404(5) 0.2773(4) 0.0164(10) Uani 1 1 d . . . C2 C 0.4771(3) 0.8223(5) 0.3477(4) 0.0173(10) Uani 1 1 d . . . C3 C 0.5092(3) 0.6986(5) 0.3736(4) 0.0203(10) Uani 1 1 d D . . H3A H 0.4798 0.6206 0.3446 0.024 Uiso 1 1 calc R . . C4 C 0.5838(3) 0.6877(5) 0.4416(4) 0.0215(11) Uani 1 1 d . . . H4A H 0.6048 0.6012 0.4605 0.026 Uiso 1 1 calc R . . C5 C 0.5967(3) 0.9136(5) 0.4536(5) 0.0284(13) Uani 1 1 d . . . H5A H 0.6270 0.9902 0.4792 0.034 Uiso 1 1 calc R . . C6 C 0.5225(3) 0.9317(5) 0.3885(5) 0.0290(13) Uani 1 1 d . . . H6A H 0.5028 1.0191 0.3718 0.035 Uiso 1 1 calc R . . C7 C 0.2035(3) 0.8275(5) 0.2458(4) 0.0197(10) Uani 1 1 d D . . C8 C 0.2003(5) 0.9507(7) 0.3053(7) 0.016(2) Uani 0.650(17) 1 d PD A 1 H8A H 0.1499 0.9879 0.2581 0.019 Uiso 0.650(17) 1 calc PR A 1 C9 C 0.2223(5) 0.8958(7) 0.4174(7) 0.018(2) Uani 0.650(17) 1 d PD A 1 H9A H 0.2711 0.8550 0.4589 0.022 Uiso 0.650(17) 1 calc PR A 1 H9B H 0.1880 0.8233 0.3993 0.022 Uiso 0.650(17) 1 calc PR A 1 C8' C 0.2333(11) 0.9251(14) 0.3481(15) 0.028(5) Uani 0.350(17) 1 d PDU A 2 H8'A H 0.2799 0.8864 0.4165 0.033 Uiso 0.350(17) 1 calc PR A 2 C9' C 0.1816(10) 0.9359(17) 0.3768(12) 0.028(5) Uani 0.350(17) 1 d PD A 2 H9'A H 0.1619 0.8469 0.3729 0.034 Uiso 0.350(17) 1 calc PR A 2 H9'B H 0.1404 0.9956 0.3217 0.034 Uiso 0.350(17) 1 calc PR A 2 C10 C 0.2251(3) 0.9929(5) 0.4987(4) 0.0253(11) Uani 1 1 d D . . N1 N 0.6280(2) 0.7937(4) 0.4821(3) 0.0159(8) Uani 1 1 d . . . O1 O 0.35674(18) 0.7425(3) 0.2203(3) 0.0174(7) Uani 1 1 d . . . O2 O 0.37667(19) 0.9538(3) 0.2845(3) 0.0233(8) Uani 1 1 d . . . O3 O 0.23496(18) 0.8453(3) 0.2042(3) 0.0177(7) Uani 1 1 d . A . O4 O 0.1712(2) 0.7233(3) 0.2357(4) 0.0260(8) Uani 1 1 d . . . O5 O 0.25045(18) 1.0492(3) 0.3251(3) 0.0165(7) Uani 1 1 d D . . O6 O 0.23995(17) 1.1169(3) 0.5033(3) 0.0141(7) Uani 1 1 d . . . O7 O 0.2211(2) 0.9338(4) 0.5682(3) 0.0280(9) Uani 1 1 d . . . C11 C 0.9720(7) 0.8047(13) 0.0752(10) 0.047(4) Uani 0.56(2) 1 d PDU B 3 H11A H 0.9278 0.8156 0.0678 0.056 Uiso 0.56(2) 1 calc PR B 3 H11B H 0.9629 0.7401 0.0184 0.056 Uiso 0.56(2) 1 calc PR B 3 H11C H 0.9857 0.8907 0.0625 0.056 Uiso 0.56(2) 1 calc PR B 3 O8 O 1.0293(6) 0.7578(11) 0.1864(9) 0.145(4) Uani 0.56(2) 1 d PDU B 3 H8B H 1.0668 0.7579 0.1911 0.173 Uiso 0.56(2) 1 d PR B 3 C11' C 0.9692(10) 0.8453(16) 0.1408(17) 0.134(14) Uani 0.44(2) 1 d PDU B 4 H11D H 0.9355 0.8057 0.1510 0.161 Uiso 0.44(2) 1 calc PR B 4 H11E H 0.9439 0.8594 0.0592 0.161 Uiso 0.44(2) 1 calc PR B 4 H11F H 0.9867 0.9311 0.1808 0.161 Uiso 0.44(2) 1 calc PR B 4 O8' O 1.0293(6) 0.7578(11) 0.1864(9) 0.145(4) Uani 0.44(2) 1 d PU B 4 H8'B H 1.0686 0.7636 0.1893 0.173 Uiso 0.44(2) 1 d PR B 4 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 0.0076(3) 0.0133(3) 0.0107(3) -0.0009(2) 0.0043(3) -0.0016(2) Co2 0.0160(4) 0.0144(3) 0.0223(4) -0.0044(3) 0.0131(3) -0.0020(2) C1 0.011(2) 0.020(2) 0.014(2) 0.0001(18) 0.0059(19) -0.0015(18) C2 0.011(2) 0.021(2) 0.014(2) -0.0012(19) 0.0058(19) -0.0012(18) C3 0.011(2) 0.017(2) 0.022(2) -0.0023(19) 0.006(2) -0.0009(18) C4 0.014(2) 0.020(2) 0.026(3) -0.001(2) 0.011(2) 0.0031(19) C5 0.011(2) 0.017(2) 0.034(3) 0.004(2) 0.003(2) -0.0010(19) C6 0.012(2) 0.020(3) 0.037(3) 0.001(2) 0.006(2) 0.000(2) C7 0.021(2) 0.019(2) 0.019(2) -0.0019(19) 0.013(2) 0.002(2) C8 0.004(4) 0.016(4) 0.017(4) -0.004(3) 0.002(3) 0.003(3) C9 0.015(5) 0.014(4) 0.018(4) 0.001(3) 0.007(4) 0.001(3) C8' 0.019(8) 0.026(7) 0.038(8) 0.003(6) 0.018(6) -0.002(6) C9' 0.032(12) 0.022(9) 0.026(9) 0.000(7) 0.016(9) -0.007(8) C10 0.023(3) 0.024(3) 0.021(3) -0.010(2) 0.010(2) -0.005(2) N1 0.0110(19) 0.019(2) 0.0145(19) 0.0037(15) 0.0065(16) 0.0034(15) O1 0.0109(16) 0.0196(17) 0.0160(17) -0.0040(13) 0.0056(14) -0.0036(13) O2 0.0141(17) 0.0183(18) 0.031(2) -0.0051(15) 0.0112(16) -0.0006(13) O3 0.0175(17) 0.0161(16) 0.0181(16) -0.0047(13) 0.0103(15) -0.0026(13) O4 0.031(2) 0.0187(18) 0.044(2) 0.0009(17) 0.031(2) 0.0017(16) O5 0.0188(18) 0.0108(16) 0.0228(18) -0.0027(13) 0.0144(16) -0.0026(12) O6 0.0118(16) 0.0144(16) 0.0130(15) 0.0018(12) 0.0063(13) 0.0018(12) O7 0.038(2) 0.0195(19) 0.025(2) -0.0004(15) 0.0193(19) -0.0079(16) C11 0.068(8) 0.045(7) 0.046(7) 0.010(5) 0.044(6) 0.007(5) O8 0.127(6) 0.152(6) 0.173(7) -0.022(5) 0.103(5) -0.004(5) C11' 0.125(16) 0.156(17) 0.132(17) 0.039(9) 0.085(12) -0.005(9) O8' 0.127(6) 0.152(6) 0.173(7) -0.022(5) 0.103(5) -0.004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O5 2.012(3) 4_545 ? Co1 O1 2.079(3) . ? Co1 O3 2.080(3) . ? Co1 O6 2.118(3) 4_545 ? Co1 N1 2.146(4) 8_465 ? Co1 O6 2.148(3) 6_575 ? Co2 O5 1.942(3) . ? Co2 O2 1.977(4) . ? Co2 O7 1.996(4) 6_575 ? Co2 O4 2.078(4) 4 ? Co2 O3 2.114(3) . ? C1 O1 1.249(6) . ? C1 O2 1.253(6) . ? C1 C2 1.510(7) . ? C2 C3 1.376(7) . ? C2 C6 1.378(7) . ? C3 C4 1.378(7) . ? C3 H3A 0.9500 . ? C4 N1 1.338(7) . ? C4 H4A 0.9500 . ? C5 N1 1.333(7) . ? C5 C6 1.380(7) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 O3 1.243(6) . ? C7 O4 1.244(6) . ? C7 C8 1.553(8) . ? C7 C8' 1.568(13) . ? C8 O5 1.420(8) . ? C8 C9 1.518(10) . ? C8 H8A 1.0000 . ? C9 C10 1.529(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C8' O5 1.415(14) . ? C8' C9' 1.526(14) . ? C8' H8'A 1.0000 . ? C9' C10 1.541(12) . ? C9' H9'A 0.9900 . ? C9' H9'B 0.9900 . ? C10 O7 1.250(7) . ? C10 O6 1.281(6) . ? N1 Co1 2.146(4) 8_566 ? O4 Co2 2.078(4) 4_545 ? O5 Co1 2.012(3) 4 ? O6 Co1 2.118(3) 4 ? O6 Co1 2.148(3) 6_576 ? O7 Co2 1.996(4) 6_576 ? C11 O8 1.418(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? O8 H8B 0.8400 . ? O8 H8'B 0.8985 . ? C11' H11D 0.9800 . ? C11' H11E 0.9800 . ? C11' H11F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Co1 O1 90.45(14) 4_545 . ? O5 Co1 O3 96.46(14) 4_545 . ? O1 Co1 O3 88.79(13) . . ? O5 Co1 O6 89.63(13) 4_545 4_545 ? O1 Co1 O6 87.83(13) . 4_545 ? O3 Co1 O6 173.06(13) . 4_545 ? O5 Co1 N1 90.27(15) 4_545 8_465 ? O1 Co1 N1 178.46(15) . 8_465 ? O3 Co1 N1 89.77(14) . 8_465 ? O6 Co1 N1 93.54(14) 4_545 8_465 ? O5 Co1 O6 168.94(13) 4_545 6_575 ? O1 Co1 O6 90.13(13) . 6_575 ? O3 Co1 O6 94.59(13) . 6_575 ? O6 Co1 O6 79.36(13) 4_545 6_575 ? N1 Co1 O6 89.43(14) 8_465 6_575 ? O5 Co2 O2 127.47(16) . . ? O5 Co2 O7 123.35(16) . 6_575 ? O2 Co2 O7 108.20(16) . 6_575 ? O5 Co2 O4 99.10(14) . 4 ? O2 Co2 O4 90.06(15) . 4 ? O7 Co2 O4 89.58(16) 6_575 4 ? O5 Co2 O3 79.73(13) . . ? O2 Co2 O3 92.43(14) . . ? O7 Co2 O3 89.21(15) 6_575 . ? O4 Co2 O3 177.47(15) 4 . ? O1 C1 O2 128.4(5) . . ? O1 C1 C2 117.1(4) . . ? O2 C1 C2 114.6(4) . . ? C3 C2 C6 117.1(5) . . ? C3 C2 C1 122.4(4) . . ? C6 C2 C1 120.4(5) . . ? C2 C3 C4 120.0(5) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? N1 C4 C3 122.9(5) . . ? N1 C4 H4A 118.6 . . ? C3 C4 H4A 118.6 . . ? N1 C5 C6 123.1(5) . . ? N1 C5 H5A 118.5 . . ? C6 C5 H5A 118.5 . . ? C2 C6 C5 119.8(5) . . ? C2 C6 H6A 120.1 . . ? C5 C6 H6A 120.1 . . ? O3 C7 O4 124.6(5) . . ? O3 C7 C8 115.5(5) . . ? O4 C7 C8 119.6(5) . . ? O3 C7 C8' 111.0(6) . . ? O4 C7 C8' 120.7(6) . . ? C8 C7 C8' 25.1(6) . . ? O5 C8 C9 110.8(6) . . ? O5 C8 C7 110.0(5) . . ? C9 C8 C7 103.9(6) . . ? O5 C8 H8A 110.6 . . ? C9 C8 H8A 110.6 . . ? C7 C8 H8A 110.6 . . ? C8 C9 C10 117.8(6) . . ? C8 C9 H9A 107.9 . . ? C10 C9 H9A 107.9 . . ? C8 C9 H9B 107.9 . . ? C10 C9 H9B 107.9 . . ? H9A C9 H9B 107.2 . . ? O5 C8' C9' 113.9(12) . . ? O5 C8' C7 109.4(9) . . ? C9' C8' C7 111.8(11) . . ? O5 C8' H8'A 107.2 . . ? C9' C8' H8'A 107.2 . . ? C7 C8' H8'A 107.2 . . ? C8' C9' C10 107.7(12) . . ? C8' C9' H9'A 110.2 . . ? C10 C9' H9'A 110.2 . . ? C8' C9' H9'B 110.2 . . ? C10 C9' H9'B 110.2 . . ? H9'A C9' H9'B 108.5 . . ? O7 C10 O6 125.0(5) . . ? O7 C10 C9 111.9(5) . . ? O6 C10 C9 122.4(5) . . ? O7 C10 C9' 118.2(7) . . ? O6 C10 C9' 112.4(8) . . ? C9 C10 C9' 32.1(7) . . ? C5 N1 C4 117.0(4) . . ? C5 N1 Co1 119.7(3) . 8_566 ? C4 N1 Co1 123.0(3) . 8_566 ? C1 O1 Co1 131.4(3) . . ? C1 O2 Co2 135.2(3) . . ? C7 O3 Co1 130.8(3) . . ? C7 O3 Co2 115.5(3) . . ? Co1 O3 Co2 113.67(16) . . ? C7 O4 Co2 123.5(3) . 4_545 ? C8' O5 C8 27.6(7) . . ? C8' O5 Co2 113.6(6) . . ? C8 O5 Co2 116.5(3) . . ? C8' O5 Co1 123.9(5) . 4 ? C8 O5 Co1 118.4(3) . 4 ? Co2 O5 Co1 121.84(16) . 4 ? C10 O6 Co1 127.8(3) . 4 ? C10 O6 Co1 131.3(3) . 6_576 ? Co1 O6 Co1 100.64(13) 4 6_576 ? C10 O7 Co2 126.1(3) . 6_576 ? C11 O8 H8B 106.1 . . ? C11 O8 H8'B 103.4 . . ? H8B O8 H8'B 4.0 . . ? H11D C11' H11E 109.5 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -16.7(7) . . . . ? O2 C1 C2 C3 163.2(5) . . . . ? O1 C1 C2 C6 163.0(5) . . . . ? O2 C1 C2 C6 -17.2(7) . . . . ? C6 C2 C3 C4 2.6(8) . . . . ? C1 C2 C3 C4 -177.7(5) . . . . ? C2 C3 C4 N1 -2.2(8) . . . . ? C3 C2 C6 C5 -0.9(9) . . . . ? C1 C2 C6 C5 179.4(5) . . . . ? N1 C5 C6 C2 -1.5(10) . . . . ? O3 C7 C8 O5 -15.0(8) . . . . ? O4 C7 C8 O5 170.0(5) . . . . ? C8' C7 C8 O5 70.1(13) . . . . ? O3 C7 C8 C9 -133.6(6) . . . . ? O4 C7 C8 C9 51.3(8) . . . . ? C8' C7 C8 C9 -48.5(13) . . . . ? O5 C8 C9 C10 61.8(9) . . . . ? C7 C8 C9 C10 179.9(6) . . . . ? O3 C7 C8' O5 35.5(14) . . . . ? O4 C7 C8' O5 -165.2(8) . . . . ? C8 C7 C8' O5 -70.2(15) . . . . ? O3 C7 C8' C9' 162.6(12) . . . . ? O4 C7 C8' C9' -38.1(18) . . . . ? C8 C7 C8' C9' 56.9(15) . . . . ? O5 C8' C9' C10 -74.1(18) . . . . ? C7 C8' C9' C10 161.4(11) . . . . ? C8 C9 C10 O7 159.2(7) . . . . ? C8 C9 C10 O6 -29.9(10) . . . . ? C8 C9 C10 C9' 50.8(11) . . . . ? C8' C9' C10 O7 -130.3(11) . . . . ? C8' C9' C10 O6 72.1(14) . . . . ? C8' C9' C10 C9 -43.5(11) . . . . ? C6 C5 N1 C4 2.1(9) . . . . ? C6 C5 N1 Co1 -171.6(5) . . . 8_566 ? C3 C4 N1 C5 -0.2(8) . . . . ? C3 C4 N1 Co1 173.2(4) . . . 8_566 ? O2 C1 O1 Co1 5.9(8) . . . . ? C2 C1 O1 Co1 -174.3(3) . . . . ? O5 Co1 O1 C1 -135.3(4) 4_545 . . . ? O3 Co1 O1 C1 -38.8(4) . . . . ? O6 Co1 O1 C1 135.1(4) 4_545 . . . ? N1 Co1 O1 C1 -18(6) 8_465 . . . ? O6 Co1 O1 C1 55.8(4) 6_575 . . . ? O1 C1 O2 Co2 10.7(9) . . . . ? C2 C1 O2 Co2 -169.1(3) . . . . ? O5 Co2 O2 C1 92.6(5) . . . . ? O7 Co2 O2 C1 -76.3(5) 6_575 . . . ? O4 Co2 O2 C1 -165.9(5) 4 . . . ? O3 Co2 O2 C1 13.6(5) . . . . ? O4 C7 O3 Co1 2.3(8) . . . . ? C8 C7 O3 Co1 -172.5(4) . . . . ? C8' C7 O3 Co1 160.6(8) . . . . ? O4 C7 O3 Co2 179.8(4) . . . . ? C8 C7 O3 Co2 5.0(6) . . . . ? C8' C7 O3 Co2 -21.9(9) . . . . ? O5 Co1 O3 C7 -35.2(4) 4_545 . . . ? O1 Co1 O3 C7 -125.5(4) . . . . ? O6 Co1 O3 C7 173.6(9) 4_545 . . . ? N1 Co1 O3 C7 55.1(4) 8_465 . . . ? O6 Co1 O3 C7 144.5(4) 6_575 . . . ? O5 Co1 O3 Co2 147.22(17) 4_545 . . . ? O1 Co1 O3 Co2 56.90(17) . . . . ? O6 Co1 O3 Co2 -4.0(12) 4_545 . . . ? N1 Co1 O3 Co2 -122.54(18) 8_465 . . . ? O6 Co1 O3 Co2 -33.13(17) 6_575 . . . ? O5 Co2 O3 C7 4.0(3) . . . . ? O2 Co2 O3 C7 131.7(4) . . . . ? O7 Co2 O3 C7 -120.1(4) 6_575 . . . ? O4 Co2 O3 C7 -59(3) 4 . . . ? O5 Co2 O3 Co1 -178.01(19) . . . . ? O2 Co2 O3 Co1 -50.34(18) . . . . ? O7 Co2 O3 Co1 57.84(18) 6_575 . . . ? O4 Co2 O3 Co1 119(3) 4 . . . ? O3 C7 O4 Co2 47.7(7) . . . 4_545 ? C8 C7 O4 Co2 -137.7(5) . . . 4_545 ? C8' C7 O4 Co2 -108.6(10) . . . 4_545 ? C9' C8' O5 C8 -56.0(14) . . . . ? C7 C8' O5 C8 69.9(14) . . . . ? C9' C8' O5 Co2 -158.5(10) . . . . ? C7 C8' O5 Co2 -32.6(14) . . . . ? C9' C8' O5 Co1 31.3(18) . . . 4 ? C7 C8' O5 Co1 157.1(6) . . . 4 ? C9 C8 O5 C8' 42.2(12) . . . . ? C7 C8 O5 C8' -72.1(12) . . . . ? C9 C8 O5 Co2 132.9(5) . . . . ? C7 C8 O5 Co2 18.5(7) . . . . ? C9 C8 O5 Co1 -67.3(7) . . . 4 ? C7 C8 O5 Co1 178.4(4) . . . 4 ? O2 Co2 O5 C8' -67.7(9) . . . . ? O7 Co2 O5 C8' 99.6(9) 6_575 . . . ? O4 Co2 O5 C8' -164.8(9) 4 . . . ? O3 Co2 O5 C8' 17.5(9) . . . . ? O2 Co2 O5 C8 -98.1(5) . . . . ? O7 Co2 O5 C8 69.2(5) 6_575 . . . ? O4 Co2 O5 C8 164.8(4) 4 . . . ? O3 Co2 O5 C8 -13.0(4) . . . . ? O2 Co2 O5 Co1 102.8(2) . . . 4 ? O7 Co2 O5 Co1 -89.9(2) 6_575 . . 4 ? O4 Co2 O5 Co1 5.6(2) 4 . . 4 ? O3 Co2 O5 Co1 -172.1(2) . . . 4 ? O7 C10 O6 Co1 174.9(4) . . . 4 ? C9 C10 O6 Co1 5.3(8) . . . 4 ? C9' C10 O6 Co1 -29.3(9) . . . 4 ? O7 C10 O6 Co1 -12.7(8) . . . 6_576 ? C9 C10 O6 Co1 177.6(5) . . . 6_576 ? C9' C10 O6 Co1 143.0(8) . . . 6_576 ? O6 C10 O7 Co2 -37.2(8) . . . 6_576 ? C9 C10 O7 Co2 133.4(5) . . . 6_576 ? C9' C10 O7 Co2 168.3(9) . . . 6_576 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8 H8B O4 0.84 2.13 2.954(11) 165.9 1_655 _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.02 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 2.313 _refine_diff_density_min -0.982 _refine_diff_density_rms 0.151 #===============================END data_1.HCONH2@293k _database_code_depnum_ccdc_archive 'CCDC 600570' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H7 Co2 N O7, C H3 N O' _chemical_formula_sum 'C11 H10 Co2 N2 O8' _chemical_formula_weight 416.07 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 Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.583(9) _cell_length_b 10.104(4) _cell_length_c 15.060(6) _cell_angle_alpha 90.00 _cell_angle_beta 128.540(5) _cell_angle_gamma 90.00 _cell_volume 2806.8(18) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 838 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 26.95 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.969 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 2.409 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6710 _exptl_absorpt_correction_T_max 0.8306 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7322 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2696 _reflns_number_gt 2067 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1097P)^2^+4.8934P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2696 _refine_ls_number_parameters 252 _refine_ls_number_restraints 64 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1644 _refine_ls_wR_factor_gt 0.1472 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.24397(3) 0.72359(7) 0.10275(6) 0.0183(2) Uani 1 1 d . . . Co2 Co 0.28406(4) 1.03496(7) 0.23474(6) 0.0256(3) Uani 1 1 d . . . C1 C 0.3956(3) 0.8434(6) 0.2781(4) 0.0260(12) Uani 1 1 d . . . C2 C 0.4771(3) 0.8240(6) 0.3495(5) 0.0285(12) Uani 1 1 d . . . C3 C 0.5079(3) 0.7023(6) 0.3706(6) 0.0428(17) Uani 1 1 d . . . H3A H 0.4789 0.6271 0.3403 0.051 Uiso 1 1 calc R . . C4 C 0.5821(3) 0.6907(6) 0.4367(6) 0.0417(16) Uani 1 1 d . . . H4A H 0.6018 0.6066 0.4496 0.050 Uiso 1 1 calc R . . C5 C 0.5959(3) 0.9136(7) 0.4602(6) 0.0478(18) Uani 1 1 d . . . H5A H 0.6257 0.9878 0.4893 0.057 Uiso 1 1 calc R . . C6 C 0.5227(3) 0.9323(7) 0.3960(6) 0.0480(18) Uani 1 1 d . . . H6A H 0.5039 1.0171 0.3839 0.058 Uiso 1 1 calc R . . C7 C 0.2048(3) 0.8294(6) 0.2476(4) 0.0265(12) Uani 1 1 d D . . C8 C 0.2024(6) 0.9504(9) 0.3072(9) 0.032(3) Uani 0.695(19) 1 d PD A 1 H8A H 0.1527 0.9843 0.2623 0.039 Uiso 0.695(19) 1 calc PR A 1 C9 C 0.2259(7) 0.8996(9) 0.4200(8) 0.040(3) Uani 0.695(19) 1 d PD A 1 H9A H 0.2745 0.8643 0.4613 0.048 Uiso 0.695(19) 1 calc PR A 1 H9B H 0.1945 0.8261 0.4049 0.048 Uiso 0.695(19) 1 calc PR A 1 C8' C 0.2317(12) 0.9290(15) 0.3461(17) 0.029(6) Uani 0.305(19) 1 d PDU A 2 H8'A H 0.2771 0.8928 0.4139 0.035 Uiso 0.305(19) 1 calc PR A 2 C9' C 0.1802(10) 0.9414(19) 0.3748(12) 0.031(6) Uani 0.305(19) 1 d PD A 2 H9C H 0.1596 0.8558 0.3697 0.037 Uiso 0.305(19) 1 calc PR A 2 H9D H 0.1410 1.0020 0.3229 0.037 Uiso 0.305(19) 1 calc PR A 2 C10 C 0.2262(3) 0.9949(6) 0.4977(5) 0.0302(13) Uani 1 1 d D . . N1 N 0.6271(2) 0.7943(5) 0.4834(4) 0.0261(10) Uani 1 1 d . . . O1 O 0.35675(19) 0.7468(4) 0.2204(3) 0.0288(9) Uani 1 1 d . . . O2 O 0.3760(2) 0.9556(4) 0.2841(4) 0.0425(12) Uani 1 1 d . . . O3 O 0.2347(2) 0.8477(4) 0.2037(3) 0.0271(9) Uani 1 1 d . A . O4 O 0.1746(2) 0.7247(4) 0.2412(4) 0.0351(10) Uani 1 1 d . . . O5 O 0.2496(2) 1.0518(3) 0.3226(3) 0.0237(8) Uani 1 1 d D . . O6 O 0.23943(19) 1.1188(4) 0.5013(3) 0.0239(8) Uani 1 1 d . . . O7 O 0.2228(3) 0.9375(4) 0.5670(4) 0.0425(11) Uani 1 1 d . . . N2 N 0.434(3) 0.225(5) 0.216(4) 0.30(3) Uani 0.45(2) 1 d PDU B 3 H2C H 0.4413 0.2423 0.1673 0.361 Uiso 0.45(2) 1 calc PR B 3 H2D H 0.3986 0.1752 0.1965 0.361 Uiso 0.45(2) 1 calc PR B 3 O8 O 0.531(3) 0.346(7) 0.356(4) 0.31(3) Uani 0.45(2) 1 d PDU B 3 C11 C 0.478(3) 0.274(4) 0.320(4) 0.160(17) Uani 0.45(2) 1 d PDU B 3 H11A H 0.4691 0.2528 0.3695 0.192 Uiso 0.45(2) 1 calc PR B 3 C11' C 0.5643(19) 0.351(5) 0.494(4) 0.30(3) Uani 0.55(2) 1 d PDU B 4 H11B H 0.5863 0.4139 0.5509 0.356 Uiso 0.55(2) 1 calc PR B 4 N2' N 0.6043(17) 0.253(3) 0.502(2) 0.215(17) Uani 0.55(2) 1 d PDU B 4 H2E H 0.5852 0.1934 0.4500 0.259 Uiso 0.55(2) 1 calc PR B 4 H2F H 0.6497 0.2490 0.5594 0.259 Uiso 0.55(2) 1 calc PR B 4 O8' O 0.4987(17) 0.362(3) 0.413(2) 0.234(14) Uani 0.55(2) 1 d PRDU B 4 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 0.0074(4) 0.0228(4) 0.0162(4) -0.0012(3) 0.0031(3) -0.0018(3) Co2 0.0179(4) 0.0247(4) 0.0312(5) -0.0042(3) 0.0137(4) -0.0010(3) C1 0.011(3) 0.029(3) 0.025(3) 0.000(2) 0.005(2) -0.001(2) C2 0.010(3) 0.033(3) 0.025(3) -0.004(2) 0.002(2) -0.001(2) C3 0.012(3) 0.034(3) 0.053(4) -0.011(3) 0.006(3) -0.007(2) C4 0.014(3) 0.035(3) 0.053(4) -0.007(3) 0.009(3) 0.001(2) C5 0.009(3) 0.034(3) 0.059(4) -0.003(3) 0.001(3) -0.002(3) C6 0.009(3) 0.034(3) 0.063(4) 0.002(3) 0.004(3) 0.002(2) C7 0.018(3) 0.030(3) 0.025(3) 0.002(2) 0.010(2) 0.005(2) C8 0.022(6) 0.031(5) 0.042(6) 0.005(4) 0.019(5) 0.007(4) C9 0.050(8) 0.024(5) 0.043(6) -0.002(4) 0.028(6) -0.001(5) C8' 0.022(9) 0.020(9) 0.045(10) 0.007(7) 0.021(8) 0.007(6) C9' 0.024(12) 0.021(10) 0.018(10) 0.002(7) -0.001(9) 0.005(9) C10 0.030(3) 0.031(3) 0.026(3) -0.006(2) 0.015(3) -0.005(3) N1 0.007(2) 0.036(3) 0.021(2) -0.0001(19) 0.0016(19) -0.0013(18) O1 0.0077(18) 0.032(2) 0.028(2) -0.0037(16) 0.0021(17) -0.0007(15) O2 0.009(2) 0.035(2) 0.062(3) -0.009(2) 0.011(2) -0.0011(16) O3 0.030(2) 0.0234(19) 0.030(2) -0.0095(16) 0.0192(19) -0.0041(17) O4 0.034(2) 0.031(2) 0.052(3) 0.0007(19) 0.033(2) 0.0023(19) O5 0.017(2) 0.0224(19) 0.031(2) -0.0047(15) 0.0150(18) -0.0057(14) O6 0.0165(19) 0.027(2) 0.0229(19) 0.0000(15) 0.0099(16) 0.0008(15) O7 0.045(3) 0.036(2) 0.031(2) -0.0035(19) 0.016(2) -0.011(2) N2 0.30(3) 0.30(3) 0.30(3) 0.010(10) 0.19(2) -0.004(10) O8 0.31(3) 0.31(3) 0.31(3) -0.015(10) 0.194(18) 0.006(10) C11 0.156(19) 0.152(19) 0.168(19) 0.000(10) 0.099(13) 0.009(10) C11' 0.30(3) 0.30(3) 0.30(3) 0.013(10) 0.19(2) -0.008(10) N2' 0.214(19) 0.217(19) 0.227(19) 0.017(9) 0.142(13) -0.015(10) O8' 0.236(17) 0.238(17) 0.225(16) 0.028(10) 0.142(12) -0.022(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O5 2.021(4) 4_545 ? Co1 O3 2.085(3) . ? Co1 O1 2.097(4) . ? Co1 O6 2.120(4) 4_545 ? Co1 O6 2.162(4) 6_575 ? Co1 N1 2.164(4) 8_465 ? Co2 O5 1.944(4) . ? Co2 O2 1.971(4) . ? Co2 O7 2.000(4) 6_575 ? Co2 O4 2.078(4) 4 ? Co2 O3 2.115(4) . ? C1 O1 1.247(7) . ? C1 O2 1.249(7) . ? C1 C2 1.521(7) . ? C2 C3 1.362(9) . ? C2 C6 1.380(9) . ? C3 C4 1.376(9) . ? C3 H3A 0.9300 . ? C4 N1 1.338(8) . ? C4 H4A 0.9300 . ? C5 N1 1.340(8) . ? C5 C6 1.367(9) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 O3 1.244(7) . ? C7 O4 1.245(7) . ? C7 C8 1.539(9) . ? C7 C8' 1.563(14) . ? C8 O5 1.422(9) . ? C8 C9 1.511(11) . ? C8 H8A 0.9800 . ? C9 C10 1.512(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C8' O5 1.425(15) . ? C8' C9' 1.527(15) . ? C8' H8'A 0.9800 . ? C9' C10 1.547(12) . ? C9' H9C 0.9700 . ? C9' H9D 0.9700 . ? C10 O7 1.238(7) . ? C10 O6 1.284(7) . ? N1 Co1 2.164(4) 8_566 ? O4 Co2 2.078(4) 4_545 ? O5 Co1 2.021(4) 4 ? O6 Co1 2.120(4) 4 ? O6 Co1 2.162(4) 6_576 ? O7 Co2 1.999(4) 6_576 ? N2 C11 1.324(10) . ? N2 H2C 0.8600 . ? N2 H2D 0.8600 . ? O8 C11 1.238(10) . ? C11 H11A 0.9300 . ? C11' O8' 1.242(10) . ? C11' N2' 1.315(10) . ? C11' H11B 0.9300 . ? N2' H2E 0.8600 . ? N2' H2F 0.8600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Co1 O3 96.70(15) 4_545 . ? O5 Co1 O1 90.57(16) 4_545 . ? O3 Co1 O1 88.34(15) . . ? O5 Co1 O6 89.89(14) 4_545 4_545 ? O3 Co1 O6 172.31(15) . 4_545 ? O1 Co1 O6 87.64(15) . 4_545 ? O5 Co1 O6 168.09(14) 4_545 6_575 ? O3 Co1 O6 95.20(15) . 6_575 ? O1 Co1 O6 89.59(15) . 6_575 ? O6 Co1 O6 78.22(15) 4_545 6_575 ? O5 Co1 N1 90.33(16) 4_545 8_465 ? O3 Co1 N1 89.90(16) . 8_465 ? O1 Co1 N1 178.10(17) . 8_465 ? O6 Co1 N1 94.03(16) 4_545 8_465 ? O6 Co1 N1 89.87(16) 6_575 8_465 ? O5 Co2 O2 127.36(19) . . ? O5 Co2 O7 124.63(19) . 6_575 ? O2 Co2 O7 107.0(2) . 6_575 ? O5 Co2 O4 98.62(15) . 4 ? O2 Co2 O4 91.35(17) . 4 ? O7 Co2 O4 89.02(19) 6_575 4 ? O5 Co2 O3 79.78(14) . . ? O2 Co2 O3 92.53(16) . . ? O7 Co2 O3 88.89(17) 6_575 . ? O4 Co2 O3 175.99(16) 4 . ? O1 C1 O2 128.0(5) . . ? O1 C1 C2 116.6(5) . . ? O2 C1 C2 115.3(5) . . ? C3 C2 C6 117.6(6) . . ? C3 C2 C1 122.4(5) . . ? C6 C2 C1 119.9(5) . . ? C2 C3 C4 119.9(6) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? N1 C4 C3 123.3(6) . . ? N1 C4 H4A 118.3 . . ? C3 C4 H4A 118.3 . . ? N1 C5 C6 123.7(6) . . ? N1 C5 H5A 118.1 . . ? C6 C5 H5A 118.1 . . ? C5 C6 C2 119.4(6) . . ? C5 C6 H6A 120.3 . . ? C2 C6 H6A 120.3 . . ? O3 C7 O4 124.8(5) . . ? O3 C7 C8 115.5(5) . . ? O4 C7 C8 119.6(5) . . ? O3 C7 C8' 112.3(7) . . ? O4 C7 C8' 119.7(7) . . ? C8 C7 C8' 22.4(7) . . ? O5 C8 C9 111.1(8) . . ? O5 C8 C7 110.9(6) . . ? C9 C8 C7 105.4(7) . . ? O5 C8 H8A 109.8 . . ? C9 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 . . ? C8 C9 C10 118.4(8) . . ? C8 C9 H9A 107.7 . . ? C10 C9 H9A 107.7 . . ? C8 C9 H9B 107.7 . . ? C10 C9 H9B 107.7 . . ? H9A C9 H9B 107.1 . . ? O5 C8' C9' 114.2(14) . . ? O5 C8' C7 109.4(10) . . ? C9' C8' C7 113.4(12) . . ? O5 C8' H8'A 106.4 . . ? C9' C8' H8'A 106.4 . . ? C7 C8' H8'A 106.4 . . ? C8' C9' C10 106.2(13) . . ? C8' C9' H9C 110.5 . . ? C10 C9' H9C 110.5 . . ? C8' C9' H9D 110.5 . . ? C10 C9' H9D 110.5 . . ? H9C C9' H9D 108.7 . . ? O7 C10 O6 124.3(5) . . ? O7 C10 C9 112.4(6) . . ? O6 C10 C9 122.5(6) . . ? O7 C10 C9' 118.6(9) . . ? O6 C10 C9' 111.2(9) . . ? C9 C10 C9' 35.9(7) . . ? C4 N1 C5 116.0(5) . . ? C4 N1 Co1 123.7(4) . 8_566 ? C5 N1 Co1 120.0(4) . 8_566 ? C1 O1 Co1 132.1(4) . . ? C1 O2 Co2 135.4(4) . . ? C7 O3 Co1 130.5(4) . . ? C7 O3 Co2 115.6(3) . . ? Co1 O3 Co2 113.93(17) . . ? C7 O4 Co2 126.0(4) . 4_545 ? C8 O5 C8' 24.4(8) . . ? C8 O5 Co2 116.3(4) . . ? C8' O5 Co2 114.0(6) . . ? C8 O5 Co1 119.3(4) . 4 ? C8' O5 Co1 122.7(6) . 4 ? Co2 O5 Co1 122.35(18) . 4 ? C10 O6 Co1 127.5(3) . 4 ? C10 O6 Co1 130.7(3) . 6_576 ? Co1 O6 Co1 101.78(15) 4 6_576 ? C10 O7 Co2 128.6(4) . 6_576 ? C11 N2 H2C 120.0 . . ? C11 N2 H2D 120.0 . . ? H2C N2 H2D 120.0 . . ? O8 C11 N2 125(2) . . ? O8 C11 H11A 117.5 . . ? N2 C11 H11A 117.4 . . ? O8' C11' N2' 123.2(12) . . ? O8' C11' H11B 118.4 . . ? N2' C11' H11B 118.4 . . ? C11' N2' H2E 120.0 . . ? C11' N2' H2F 120.0 . . ? H2E N2' H2F 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -14.2(9) . . . . ? O2 C1 C2 C3 166.5(6) . . . . ? O1 C1 C2 C6 166.1(6) . . . . ? O2 C1 C2 C6 -13.2(9) . . . . ? C6 C2 C3 C4 0.4(11) . . . . ? C1 C2 C3 C4 -179.4(6) . . . . ? C2 C3 C4 N1 0.3(12) . . . . ? N1 C5 C6 C2 -1.5(13) . . . . ? C3 C2 C6 C5 0.2(11) . . . . ? C1 C2 C6 C5 179.9(7) . . . . ? O3 C7 C8 O5 -13.3(10) . . . . ? O4 C7 C8 O5 170.2(6) . . . . ? C8' C7 C8 O5 73.5(17) . . . . ? O3 C7 C8 C9 -133.7(8) . . . . ? O4 C7 C8 C9 49.8(10) . . . . ? C8' C7 C8 C9 -46.9(17) . . . . ? O5 C8 C9 C10 62.3(12) . . . . ? C7 C8 C9 C10 -177.5(7) . . . . ? O3 C7 C8' O5 31.9(17) . . . . ? O4 C7 C8' O5 -167.5(9) . . . . ? C8 C7 C8' O5 -71.3(18) . . . . ? O3 C7 C8' C9' 160.7(13) . . . . ? O4 C7 C8' C9' -39(2) . . . . ? C8 C7 C8' C9' 57.5(19) . . . . ? O5 C8' C9' C10 -75.7(19) . . . . ? C7 C8' C9' C10 158.0(12) . . . . ? C8 C9 C10 O7 157.9(9) . . . . ? C8 C9 C10 O6 -31.8(13) . . . . ? C8 C9 C10 C9' 49.6(13) . . . . ? C8' C9' C10 O7 -130.3(12) . . . . ? C8' C9' C10 O6 75.5(14) . . . . ? C8' C9' C10 C9 -41.1(11) . . . . ? C3 C4 N1 C5 -1.5(11) . . . . ? C3 C4 N1 Co1 172.8(6) . . . 8_566 ? C6 C5 N1 C4 2.1(11) . . . . ? C6 C5 N1 Co1 -172.4(7) . . . 8_566 ? O2 C1 O1 Co1 3.2(9) . . . . ? C2 C1 O1 Co1 -176.0(4) . . . . ? O5 Co1 O1 C1 -133.4(5) 4_545 . . . ? O3 Co1 O1 C1 -36.7(5) . . . . ? O6 Co1 O1 C1 136.8(5) 4_545 . . . ? O6 Co1 O1 C1 58.5(5) 6_575 . . . ? N1 Co1 O1 C1 -15(6) 8_465 . . . ? O1 C1 O2 Co2 12.0(10) . . . . ? C2 C1 O2 Co2 -168.8(4) . . . . ? O5 Co2 O2 C1 92.8(6) . . . . ? O7 Co2 O2 C1 -75.9(6) 6_575 . . . ? O4 Co2 O2 C1 -165.3(6) 4 . . . ? O3 Co2 O2 C1 13.7(6) . . . . ? O4 C7 O3 Co1 2.3(9) . . . . ? C8 C7 O3 Co1 -174.0(5) . . . . ? C8' C7 O3 Co1 161.7(10) . . . . ? O4 C7 O3 Co2 -178.1(5) . . . . ? C8 C7 O3 Co2 5.6(7) . . . . ? C8' C7 O3 Co2 -18.6(11) . . . . ? O5 Co1 O3 C7 -33.8(5) 4_545 . . . ? O1 Co1 O3 C7 -124.2(5) . . . . ? O6 Co1 O3 C7 177.3(9) 4_545 . . . ? O6 Co1 O3 C7 146.4(5) 6_575 . . . ? N1 Co1 O3 C7 56.5(5) 8_465 . . . ? O5 Co1 O3 Co2 146.54(18) 4_545 . . . ? O1 Co1 O3 Co2 56.2(2) . . . . ? O6 Co1 O3 Co2 -2.3(12) 4_545 . . . ? O6 Co1 O3 Co2 -33.27(19) 6_575 . . . ? N1 Co1 O3 Co2 -123.1(2) 8_465 . . . ? O5 Co2 O3 C7 2.1(4) . . . . ? O2 Co2 O3 C7 129.6(4) . . . . ? O7 Co2 O3 C7 -123.5(4) 6_575 . . . ? O4 Co2 O3 C7 -65(2) 4 . . . ? O5 Co2 O3 Co1 -178.3(2) . . . . ? O2 Co2 O3 Co1 -50.7(2) . . . . ? O7 Co2 O3 Co1 56.2(2) 6_575 . . . ? O4 Co2 O3 Co1 115(2) 4 . . . ? O3 C7 O4 Co2 45.6(8) . . . 4_545 ? C8 C7 O4 Co2 -138.2(6) . . . 4_545 ? C8' C7 O4 Co2 -112.4(11) . . . 4_545 ? C9 C8 O5 C8' 41.4(16) . . . . ? C7 C8 O5 C8' -75.5(16) . . . . ? C9 C8 O5 Co2 132.0(6) . . . . ? C7 C8 O5 Co2 15.1(9) . . . . ? C9 C8 O5 Co1 -63.9(9) . . . 4 ? C7 C8 O5 Co1 179.2(5) . . . 4 ? C9' C8' O5 C8 -57.7(18) . . . . ? C7 C8' O5 C8 70.7(18) . . . . ? C9' C8' O5 Co2 -158.7(11) . . . . ? C7 C8' O5 Co2 -30.4(17) . . . . ? C9' C8' O5 Co1 32(2) . . . 4 ? C7 C8' O5 Co1 160.1(7) . . . 4 ? O2 Co2 O5 C8 -95.2(6) . . . . ? O7 Co2 O5 C8 71.6(6) 6_575 . . . ? O4 Co2 O5 C8 166.4(6) 4 . . . ? O3 Co2 O5 C8 -9.9(6) . . . . ? O2 Co2 O5 C8' -68.3(11) . . . . ? O7 Co2 O5 C8' 98.5(11) 6_575 . . . ? O4 Co2 O5 C8' -166.7(11) 4 . . . ? O3 Co2 O5 C8' 17.0(10) . . . . ? O2 Co2 O5 Co1 101.2(2) . . . 4 ? O7 Co2 O5 Co1 -91.9(3) 6_575 . . 4 ? O4 Co2 O5 Co1 2.9(2) 4 . . 4 ? O3 Co2 O5 Co1 -173.4(2) . . . 4 ? O7 C10 O6 Co1 173.8(4) . . . 4 ? C9 C10 O6 Co1 4.7(9) . . . 4 ? C9' C10 O6 Co1 -33.7(10) . . . 4 ? O7 C10 O6 Co1 -10.6(9) . . . 6_576 ? C9 C10 O6 Co1 -179.7(6) . . . 6_576 ? C9' C10 O6 Co1 141.8(8) . . . 6_576 ? O6 C10 O7 Co2 -38.5(9) . . . 6_576 ? C9 C10 O7 Co2 131.6(6) . . . 6_576 ? C9' C10 O7 Co2 170.9(9) . . . 6_576 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2D O4 0.86 2.48 3.02(7) 121.6 4_545 N2 H2C N2 0.86 2.30 2.58(12) 99.3 2_655 N2' H2F O7 0.86 2.52 2.97(3) 113.3 3_545 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.370 _refine_diff_density_min -1.089 _refine_diff_density_rms 0.170 #===============================END data_1.HCONH2@93k _database_code_depnum_ccdc_archive 'CCDC 600571' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H7 Co2 N O7, C H3 N O' _chemical_formula_sum 'C11 H10 Co2 N2 O8' _chemical_formula_weight 416.07 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 Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.702(3) _cell_length_b 10.0616(11) _cell_length_c 15.0200(17) _cell_angle_alpha 90.00 _cell_angle_beta 129.070(2) _cell_angle_gamma 90.00 _cell_volume 2780.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.988 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 2.431 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7792 _exptl_absorpt_correction_T_max 0.9306 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7199 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 26.02 _reflns_number_total 2673 _reflns_number_gt 2176 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+4.9841P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2673 _refine_ls_number_parameters 246 _refine_ls_number_restraints 85 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1237 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.150 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 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 0.24480(3) 0.72309(6) 0.10301(5) 0.01119(19) Uani 1 1 d . . . Co2 Co 0.28517(3) 1.03475(6) 0.23702(6) 0.0161(2) Uani 1 1 d . . . C1 C 0.3964(2) 0.8436(5) 0.2782(4) 0.0169(10) Uani 1 1 d . . . C2 C 0.4782(2) 0.8249(5) 0.3491(4) 0.0183(10) Uani 1 1 d . . . C3 C 0.5092(3) 0.7020(5) 0.3702(5) 0.0259(12) Uani 1 1 d . . . H3A H 0.4797 0.6246 0.3384 0.031 Uiso 1 1 calc R . . C4 C 0.5834(3) 0.6916(5) 0.4377(5) 0.0264(12) Uani 1 1 d . . . H4A H 0.6038 0.6052 0.4532 0.032 Uiso 1 1 calc R . . C5 C 0.5971(3) 0.9152(5) 0.4586(5) 0.0306(13) Uani 1 1 d . . . H5A H 0.6273 0.9917 0.4864 0.037 Uiso 1 1 calc R . . C6 C 0.5236(3) 0.9332(5) 0.3958(5) 0.0323(14) Uani 1 1 d . . . H6A H 0.5043 1.0199 0.3847 0.039 Uiso 1 1 calc R . . C7 C 0.2045(3) 0.8289(5) 0.2468(4) 0.0189(10) Uani 1 1 d D . . C8 C 0.2003(5) 0.9521(9) 0.3050(8) 0.017(2) Uani 0.648(17) 1 d PD A 1 H8A H 0.1495 0.9865 0.2582 0.021 Uiso 0.648(17) 1 calc PR A 1 C9 C 0.2253(4) 0.8973(7) 0.4194(6) 0.014(2) Uani 0.648(17) 1 d PD A 1 H9A H 0.1937 0.8211 0.4035 0.017 Uiso 0.648(17) 1 calc PR A 1 H9B H 0.2753 0.8624 0.4618 0.017 Uiso 0.648(17) 1 calc PR A 1 C8' C 0.2279(8) 0.9314(13) 0.3421(13) 0.037(7) Uani 0.352(17) 1 d PD A 2 H8'A H 0.2745 0.8950 0.4125 0.045 Uiso 0.352(17) 1 calc PR A 2 C9' C 0.1786(9) 0.9387(18) 0.3729(13) 0.034(5) Uani 0.352(17) 1 d PD A 2 H9C H 0.1595 0.8494 0.3688 0.041 Uiso 0.352(17) 1 calc PR A 2 H9D H 0.1370 0.9985 0.3194 0.041 Uiso 0.352(17) 1 calc PR A 2 C10 C 0.2253(3) 0.9941(5) 0.4979(4) 0.0244(11) Uani 1 1 d D . . N1 N 0.6286(2) 0.7951(4) 0.4828(3) 0.0165(8) Uani 1 1 d . . . O1 O 0.35716(16) 0.7465(3) 0.2205(3) 0.0162(7) Uani 1 1 d . . . O2 O 0.37706(18) 0.9572(3) 0.2848(3) 0.0254(8) Uani 1 1 d . . . O3 O 0.23691(17) 0.8463(3) 0.2060(3) 0.0167(7) Uani 1 1 d . A . O4 O 0.17240(18) 0.7240(3) 0.2362(3) 0.0219(8) Uani 1 1 d . . . O5 O 0.24823(17) 1.0515(3) 0.3208(3) 0.0161(7) Uani 1 1 d D . . O6 O 0.23913(16) 1.1178(3) 0.5019(3) 0.0133(7) Uani 1 1 d . . . O7 O 0.2218(2) 0.9358(3) 0.5673(3) 0.0250(8) Uani 1 1 d . . . C11 C 0.5097(13) 0.323(2) 0.3432(19) 0.218(12) Uani 0.533(17) 1 d PDU B 3 H11A H 0.5471 0.3414 0.3386 0.262 Uiso 0.533(17) 1 calc PR B 3 N2 N 0.4526(12) 0.250(3) 0.2627(18) 0.207(12) Uani 0.533(17) 1 d PDU B 3 H2A H 0.4182 0.2333 0.2674 0.248 Uiso 0.533(17) 1 calc PR B 3 H2B H 0.4491 0.2198 0.2046 0.248 Uiso 0.533(17) 1 calc PR B 3 O8 O 0.5137(10) 0.3652(17) 0.4251(15) 0.235(6) Uani 0.533(17) 1 d PDU B 3 C11' C 0.5779(10) 0.325(3) 0.4988(19) 0.124(8) Uani 0.467(17) 1 d PDU B 4 H11B H 0.6087 0.3629 0.5733 0.149 Uiso 0.467(17) 1 calc PR B 4 N2' N 0.6013(10) 0.228(2) 0.470(2) 0.149(9) Uani 0.467(17) 1 d PDU B 4 H2C H 0.5722 0.1935 0.4011 0.179 Uiso 0.467(17) 1 calc PR B 4 H2D H 0.6460 0.1982 0.5206 0.179 Uiso 0.467(17) 1 calc PR B 4 O8' O 0.5137(10) 0.3652(17) 0.4251(15) 0.235(6) Uani 0.467(17) 1 d PU B 4 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 0.0081(3) 0.0132(3) 0.0114(3) -0.0007(2) 0.0057(3) -0.0010(2) Co2 0.0149(3) 0.0144(3) 0.0218(4) -0.0028(3) 0.0128(3) -0.0011(2) C1 0.011(2) 0.021(3) 0.015(2) 0.0002(19) 0.007(2) -0.0011(19) C2 0.015(2) 0.019(2) 0.021(2) 0.000(2) 0.011(2) 0.0000(19) C3 0.015(2) 0.019(3) 0.036(3) -0.009(2) 0.012(2) -0.008(2) C4 0.015(2) 0.020(3) 0.034(3) -0.005(2) 0.010(2) 0.004(2) C5 0.015(2) 0.021(3) 0.039(3) -0.002(2) 0.008(2) -0.004(2) C6 0.013(2) 0.019(3) 0.044(3) -0.001(2) 0.008(3) 0.000(2) C7 0.017(2) 0.023(3) 0.017(2) 0.002(2) 0.011(2) 0.003(2) C8 0.012(5) 0.020(5) 0.022(5) 0.002(4) 0.011(4) 0.002(3) C9 0.013(4) 0.011(4) 0.018(4) 0.002(3) 0.010(4) 0.002(3) C8' 0.041(15) 0.015(10) 0.08(2) -0.004(10) 0.049(15) -0.006(9) C9' 0.028(11) 0.036(10) 0.033(10) -0.010(8) 0.016(9) -0.005(8) C10 0.026(3) 0.025(3) 0.019(3) -0.005(2) 0.013(2) -0.006(2) N1 0.0115(18) 0.020(2) 0.016(2) 0.0031(16) 0.0078(17) 0.0037(15) O1 0.0082(15) 0.0188(17) 0.0170(17) -0.0015(13) 0.0058(14) -0.0012(13) O2 0.0124(16) 0.0193(19) 0.039(2) -0.0072(16) 0.0135(17) -0.0016(14) O3 0.0188(16) 0.0169(16) 0.0191(17) -0.0047(14) 0.0143(15) -0.0028(13) O4 0.0220(18) 0.0189(17) 0.036(2) 0.0010(15) 0.0234(17) 0.0001(15) O5 0.0176(17) 0.0137(17) 0.0254(18) -0.0024(13) 0.0176(16) -0.0019(12) O6 0.0108(15) 0.0133(16) 0.0169(16) -0.0003(13) 0.0092(14) 0.0003(12) O7 0.032(2) 0.0196(18) 0.0225(19) -0.0013(15) 0.0165(17) -0.0075(15) C11 0.217(14) 0.214(14) 0.210(14) 0.000(9) 0.128(10) 0.015(9) N2 0.195(14) 0.209(15) 0.230(14) 0.029(9) 0.141(10) 0.003(9) O8 0.230(11) 0.233(12) 0.207(11) 0.077(10) 0.122(10) 0.023(10) C11' 0.132(11) 0.134(12) 0.142(11) 0.033(8) 0.103(8) -0.022(8) N2' 0.140(12) 0.152(13) 0.163(13) 0.015(8) 0.098(9) -0.032(8) O8' 0.230(11) 0.233(12) 0.207(11) 0.077(10) 0.122(10) 0.023(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O5 2.020(3) 4_545 ? Co1 O3 2.080(3) . ? Co1 O1 2.083(3) . ? Co1 O6 2.123(3) 4_545 ? Co1 N1 2.146(4) 8_465 ? Co1 O6 2.151(3) 6_575 ? Co2 O5 1.941(3) . ? Co2 O2 1.974(3) . ? Co2 O7 2.004(4) 6_575 ? Co2 O4 2.071(3) 4 ? Co2 O3 2.109(3) . ? C1 O1 1.247(6) . ? C1 O2 1.258(6) . ? C1 C2 1.525(6) . ? C2 C3 1.370(7) . ? C2 C6 1.373(7) . ? C3 C4 1.371(7) . ? C3 H3A 0.9500 . ? C4 N1 1.333(7) . ? C4 H4A 0.9500 . ? C5 N1 1.345(7) . ? C5 C6 1.374(7) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 O4 1.252(6) . ? C7 O3 1.260(6) . ? C7 C8 1.555(10) . ? C7 C8' 1.555(15) . ? C8 O5 1.416(9) . ? C8 C9 1.525(11) . ? C8 H8A 1.0000 . ? C9 C10 1.529(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C8' O5 1.411(14) . ? C8' C9' 1.505(16) . ? C8' H8'A 1.0000 . ? C9' C10 1.563(14) . ? C9' H9C 0.9900 . ? C9' H9D 0.9900 . ? C10 O7 1.243(6) . ? C10 O6 1.279(6) . ? N1 Co1 2.146(4) 8_566 ? O4 Co2 2.071(3) 4_545 ? O5 Co1 2.020(3) 4 ? O6 Co1 2.123(3) 4 ? O6 Co1 2.151(3) 6_576 ? O7 Co2 2.004(4) 6_576 ? C11 O8 1.249(10) . ? C11 N2 1.325(10) . ? C11 H11A 0.9500 . ? N2 H2A 0.8800 . ? N2 H2B 0.8800 . ? C11' N2' 1.317(10) . ? C11' H11B 0.9500 . ? N2' H2C 0.8800 . ? N2' H2D 0.8800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Co1 O3 95.85(13) 4_545 . ? O5 Co1 O1 90.71(13) 4_545 . ? O3 Co1 O1 88.21(13) . . ? O5 Co1 O6 90.31(12) 4_545 4_545 ? O3 Co1 O6 172.44(12) . 4_545 ? O1 Co1 O6 87.34(12) . 4_545 ? O5 Co1 N1 90.41(14) 4_545 8_465 ? O3 Co1 N1 90.42(14) . 8_465 ? O1 Co1 N1 178.31(14) . 8_465 ? O6 Co1 N1 93.92(13) 4_545 8_465 ? O5 Co1 O6 169.21(12) 4_545 6_575 ? O3 Co1 O6 94.94(12) . 6_575 ? O1 Co1 O6 89.51(12) . 6_575 ? O6 Co1 O6 78.92(12) 4_545 6_575 ? N1 Co1 O6 89.62(13) 8_465 6_575 ? O5 Co2 O2 130.08(16) . . ? O5 Co2 O7 121.95(15) . 6_575 ? O2 Co2 O7 106.94(16) . 6_575 ? O5 Co2 O4 99.03(13) . 4 ? O2 Co2 O4 90.19(14) . 4 ? O7 Co2 O4 89.64(15) 6_575 4 ? O5 Co2 O3 79.51(13) . . ? O2 Co2 O3 92.60(13) . . ? O7 Co2 O3 89.11(14) 6_575 . ? O4 Co2 O3 177.17(13) 4 . ? O1 C1 O2 128.1(4) . . ? O1 C1 C2 116.9(4) . . ? O2 C1 C2 115.0(4) . . ? C3 C2 C6 117.7(5) . . ? C3 C2 C1 122.3(4) . . ? C6 C2 C1 120.0(4) . . ? C2 C3 C4 119.4(5) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? N1 C4 C3 124.2(5) . . ? N1 C4 H4A 117.9 . . ? C3 C4 H4A 117.9 . . ? N1 C5 C6 123.5(5) . . ? N1 C5 H5A 118.2 . . ? C6 C5 H5A 118.2 . . ? C5 C6 C2 119.5(5) . . ? C5 C6 H6A 120.2 . . ? C2 C6 H6A 120.2 . . ? O4 C7 O3 124.3(5) . . ? O4 C7 C8 119.6(5) . . ? O3 C7 C8 115.9(5) . . ? O4 C7 C8' 120.7(6) . . ? O3 C7 C8' 112.5(6) . . ? C8 C7 C8' 21.0(4) . . ? O5 C8 C9 111.4(7) . . ? O5 C8 C7 109.2(6) . . ? C9 C8 C7 103.2(6) . . ? O5 C8 H8A 110.9 . . ? C9 C8 H8A 110.9 . . ? C7 C8 H8A 110.9 . . ? C10 C9 C8 116.8(6) . . ? C10 C9 H9A 108.1 . . ? C8 C9 H9A 108.1 . . ? C10 C9 H9B 108.1 . . ? C8 C9 H9B 108.1 . . ? H9A C9 H9B 107.3 . . ? O5 C8' C9' 118.0(12) . . ? O5 C8' C7 109.5(10) . . ? C9' C8' C7 114.9(10) . . ? O5 C8' H8'A 104.2 . . ? C9' C8' H8'A 104.2 . . ? C7 C8' H8'A 104.2 . . ? C8' C9' C10 106.7(11) . . ? C8' C9' H9C 110.4 . . ? C10 C9' H9C 110.4 . . ? C8' C9' H9D 110.4 . . ? C10 C9' H9D 110.4 . . ? H9C C9' H9D 108.6 . . ? O7 C10 O6 124.7(5) . . ? O7 C10 C9 112.2(5) . . ? O6 C10 C9 122.1(5) . . ? O7 C10 C9' 117.9(8) . . ? O6 C10 C9' 111.7(8) . . ? C9 C10 C9' 36.0(7) . . ? C4 N1 C5 115.6(4) . . ? C4 N1 Co1 123.8(3) . 8_566 ? C5 N1 Co1 120.3(3) . 8_566 ? C1 O1 Co1 132.3(3) . . ? C1 O2 Co2 134.7(3) . . ? C7 O3 Co1 130.3(3) . . ? C7 O3 Co2 115.4(3) . . ? Co1 O3 Co2 114.20(14) . . ? C7 O4 Co2 124.6(3) . 4_545 ? C8 O5 C8' 23.1(4) . . ? C8 O5 Co2 118.1(4) . . ? C8' O5 Co2 115.5(6) . . ? C8 O5 Co1 118.0(4) . 4 ? C8' O5 Co1 121.4(6) . 4 ? Co2 O5 Co1 122.16(16) . 4 ? C10 O6 Co1 127.6(3) . 4 ? C10 O6 Co1 131.1(3) . 6_576 ? Co1 O6 Co1 101.08(12) 4 6_576 ? C10 O7 Co2 127.1(3) . 6_576 ? O8 C11 N2 119(2) . . ? O8 C11 H11A 120.4 . . ? N2 C11 H11A 120.4 . . ? C11 N2 H2A 120.0 . . ? C11 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? N2' C11' H11B 120.8 . . ? C11' N2' H2C 120.0 . . ? C11' N2' H2D 120.0 . . ? H2C N2' H2D 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -14.2(7) . . . . ? O2 C1 C2 C3 166.5(5) . . . . ? O1 C1 C2 C6 166.7(5) . . . . ? O2 C1 C2 C6 -12.6(7) . . . . ? C6 C2 C3 C4 1.1(8) . . . . ? C1 C2 C3 C4 -178.0(5) . . . . ? C2 C3 C4 N1 -2.1(9) . . . . ? N1 C5 C6 C2 -3.6(10) . . . . ? C3 C2 C6 C5 1.5(9) . . . . ? C1 C2 C6 C5 -179.3(5) . . . . ? O4 C7 C8 O5 172.3(5) . . . . ? O3 C7 C8 O5 -12.5(8) . . . . ? C8' C7 C8 O5 73.1(18) . . . . ? O4 C7 C8 C9 53.6(8) . . . . ? O3 C7 C8 C9 -131.1(6) . . . . ? C8' C7 C8 C9 -45.5(17) . . . . ? O5 C8 C9 C10 64.8(9) . . . . ? C7 C8 C9 C10 -178.2(5) . . . . ? O4 C7 C8' O5 -167.4(6) . . . . ? O3 C7 C8' O5 29.6(11) . . . . ? C8 C7 C8' O5 -74.3(18) . . . . ? O4 C7 C8' C9' -31.9(15) . . . . ? O3 C7 C8' C9' 165.2(11) . . . . ? C8 C7 C8' C9' 61.3(18) . . . . ? O5 C8' C9' C10 -72.6(16) . . . . ? C7 C8' C9' C10 155.8(10) . . . . ? C8 C9 C10 O7 157.0(6) . . . . ? C8 C9 C10 O6 -33.3(9) . . . . ? C8 C9 C10 C9' 49.7(12) . . . . ? C8' C9' C10 O7 -132.8(10) . . . . ? C8' C9' C10 O6 72.4(14) . . . . ? C8' C9' C10 C9 -42.8(9) . . . . ? C3 C4 N1 C5 0.2(8) . . . . ? C3 C4 N1 Co1 173.0(4) . . . 8_566 ? C6 C5 N1 C4 2.7(9) . . . . ? C6 C5 N1 Co1 -170.4(5) . . . 8_566 ? O2 C1 O1 Co1 4.0(8) . . . . ? C2 C1 O1 Co1 -175.2(3) . . . . ? O5 Co1 O1 C1 -133.4(4) 4_545 . . . ? O3 Co1 O1 C1 -37.6(4) . . . . ? O6 Co1 O1 C1 136.3(4) 4_545 . . . ? N1 Co1 O1 C1 -2(5) 8_465 . . . ? O6 Co1 O1 C1 57.3(4) 6_575 . . . ? O1 C1 O2 Co2 12.5(8) . . . . ? C2 C1 O2 Co2 -168.3(3) . . . . ? O5 Co2 O2 C1 91.3(5) . . . . ? O7 Co2 O2 C1 -77.0(5) 6_575 . . . ? O4 Co2 O2 C1 -166.7(5) 4 . . . ? O3 Co2 O2 C1 12.8(5) . . . . ? O4 C7 O3 Co1 4.1(7) . . . . ? C8 C7 O3 Co1 -170.9(5) . . . . ? C8' C7 O3 Co1 166.3(6) . . . . ? O4 C7 O3 Co2 179.5(4) . . . . ? C8 C7 O3 Co2 4.5(6) . . . . ? C8' C7 O3 Co2 -18.3(7) . . . . ? O5 Co1 O3 C7 -37.4(4) 4_545 . . . ? O1 Co1 O3 C7 -128.0(4) . . . . ? O6 Co1 O3 C7 178.1(8) 4_545 . . . ? N1 Co1 O3 C7 53.0(4) 8_465 . . . ? O6 Co1 O3 C7 142.7(4) 6_575 . . . ? O5 Co1 O3 Co2 147.12(16) 4_545 . . . ? O1 Co1 O3 Co2 56.59(17) . . . . ? O6 Co1 O3 Co2 2.7(11) 4_545 . . . ? N1 Co1 O3 Co2 -122.42(18) 8_465 . . . ? O6 Co1 O3 Co2 -32.76(16) 6_575 . . . ? O5 Co2 O3 C7 3.0(3) . . . . ? O2 Co2 O3 C7 133.4(3) . . . . ? O7 Co2 O3 C7 -119.7(3) 6_575 . . . ? O4 Co2 O3 C7 -56(3) 4 . . . ? O5 Co2 O3 Co1 179.17(18) . . . . ? O2 Co2 O3 Co1 -50.51(18) . . . . ? O7 Co2 O3 Co1 56.41(17) 6_575 . . . ? O4 Co2 O3 Co1 120(3) 4 . . . ? O3 C7 O4 Co2 46.4(7) . . . 4_545 ? C8 C7 O4 Co2 -138.8(5) . . . 4_545 ? C8' C7 O4 Co2 -114.5(7) . . . 4_545 ? C9 C8 O5 C8' 39.2(17) . . . . ? C7 C8 O5 C8' -74.2(19) . . . . ? C9 C8 O5 Co2 128.7(5) . . . . ? C7 C8 O5 Co2 15.4(8) . . . . ? C9 C8 O5 Co1 -65.8(8) . . . 4 ? C7 C8 O5 Co1 -179.2(4) . . . 4 ? C9' C8' O5 C8 -59.3(17) . . . . ? C7 C8' O5 C8 74.6(18) . . . . ? C9' C8' O5 Co2 -161.6(10) . . . . ? C7 C8' O5 Co2 -27.6(10) . . . . ? C9' C8' O5 Co1 28.9(15) . . . 4 ? C7 C8' O5 Co1 162.9(5) . . . 4 ? O2 Co2 O5 C8 -95.3(5) . . . . ? O7 Co2 O5 C8 71.5(5) 6_575 . . . ? O4 Co2 O5 C8 166.8(5) 4 . . . ? O3 Co2 O5 C8 -10.8(5) . . . . ? O2 Co2 O5 C8' -69.5(7) . . . . ? O7 Co2 O5 C8' 97.3(7) 6_575 . . . ? O4 Co2 O5 C8' -167.4(7) 4 . . . ? O3 Co2 O5 C8' 15.0(7) . . . . ? O2 Co2 O5 Co1 99.9(2) . . . 4 ? O7 Co2 O5 Co1 -93.3(2) 6_575 . . 4 ? O4 Co2 O5 Co1 2.0(2) 4 . . 4 ? O3 Co2 O5 Co1 -175.5(2) . . . 4 ? O7 C10 O6 Co1 174.3(4) . . . 4 ? C9 C10 O6 Co1 6.0(7) . . . 4 ? C9' C10 O6 Co1 -32.9(9) . . . 4 ? O7 C10 O6 Co1 -10.7(8) . . . 6_576 ? C9 C10 O6 Co1 -179.1(4) . . . 6_576 ? C9' C10 O6 Co1 142.0(7) . . . 6_576 ? O6 C10 O7 Co2 -38.5(7) . . . 6_576 ? C9 C10 O7 Co2 130.8(5) . . . 6_576 ? C9' C10 O7 Co2 170.2(8) . . . 6_576 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A O4 0.88 2.11 2.98(3) 170.0 4_545 N2 H2B N2 0.88 2.08 2.51(6) 108.9 2_655 N2' H2D O7 0.88 2.80 3.07(2) 99.1 3_545 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.398 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.168 #===============================END data_1@293k _database_code_depnum_ccdc_archive 'CCDC 600572' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H7 Co2 N O7' _chemical_formula_sum 'C10 H7 Co2 N O7' _chemical_formula_weight 371.03 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 Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.482(3) _cell_length_b 10.0597(12) _cell_length_c 14.9495(18) _cell_angle_alpha 90.00 _cell_angle_beta 128.342(2) _cell_angle_gamma 90.00 _cell_volume 2769.8(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.780 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 2.422 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6807 _exptl_absorpt_correction_T_max 0.8298 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7387 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2655 _reflns_number_gt 2333 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0868P)^2^+7.4289P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2655 _refine_ls_number_parameters 195 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1295 _refine_ls_wR_factor_gt 0.1247 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.020 _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 0.24422(2) 0.72243(5) 0.10312(4) 0.02004(18) Uani 1 1 d . . . Co2 Co 0.28458(3) 1.03307(5) 0.23597(4) 0.02700(19) Uani 1 1 d . . . O2 O 0.37587(16) 0.9548(3) 0.2822(3) 0.0442(8) Uani 1 1 d . . . O1 O 0.35683(14) 0.7443(3) 0.2208(2) 0.0307(6) Uani 1 1 d . . . O3 O 0.23583(15) 0.8449(3) 0.2061(2) 0.0302(6) Uani 1 1 d . A . O4 O 0.17388(18) 0.7228(3) 0.2415(3) 0.0373(7) Uani 1 1 d . . . O5 O 0.24983(15) 1.0499(2) 0.3240(2) 0.0270(6) Uani 1 1 d D . . O6 O 0.23983(14) 1.1189(2) 0.5033(2) 0.0241(5) Uani 1 1 d . . . O7 O 0.21931(18) 0.9394(3) 0.5669(3) 0.0393(7) Uani 1 1 d . . . N1 N 0.62726(17) 0.7935(3) 0.4846(3) 0.0281(7) Uani 1 1 d . . . C1 C 0.3957(2) 0.8404(4) 0.2783(3) 0.0278(8) Uani 1 1 d . . . C2 C 0.4770(2) 0.8231(4) 0.3502(3) 0.0281(8) Uani 1 1 d . . . C3 C 0.5088(2) 0.6983(4) 0.3775(4) 0.0401(11) Uani 1 1 d . . . H3A H 0.4800 0.6227 0.3499 0.048 Uiso 1 1 d R . . C4 C 0.5829(2) 0.6894(4) 0.4455(4) 0.0404(11) Uani 1 1 d . . . H4A H 0.6033 0.6052 0.4632 0.048 Uiso 1 1 d R . . C5 C 0.5960(2) 0.9122(5) 0.4558(4) 0.0425(11) Uani 1 1 d . . . H5A H 0.6257 0.9865 0.4815 0.051 Uiso 1 1 d R . . C6 C 0.5211(2) 0.9304(5) 0.3903(4) 0.0433(11) Uani 1 1 d . . . H6A H 0.5020 1.0156 0.3749 0.052 Uiso 1 1 d R . . C7 C 0.2056(2) 0.8277(4) 0.2501(3) 0.0295(9) Uani 1 1 d D . . C8 C 0.2020(4) 0.9502(6) 0.3069(6) 0.0246(18) Uani 0.627(16) 1 d PD A 1 H8A H 0.1522 0.9846 0.2607 0.030 Uiso 0.627(16) 1 calc PR A 1 C9 C 0.2248(5) 0.8996(6) 0.4209(6) 0.032(2) Uani 0.627(16) 1 d PD A 1 H9A H 0.1932 0.8260 0.4056 0.038 Uiso 0.627(16) 1 calc PR A 1 H9B H 0.2736 0.8642 0.4630 0.038 Uiso 0.627(16) 1 calc PR A 1 C8' C 0.2317(9) 0.9281(12) 0.3485(13) 0.039(4) Uiso 0.373(16) 1 d PD A 2 H8'A H 0.2772 0.8922 0.4168 0.047 Uiso 0.373(16) 1 calc PR A 2 C9' C 0.1806(8) 0.9406(16) 0.3770(11) 0.046(4) Uani 0.373(16) 1 d PD A 2 H9'A H 0.1606 0.8543 0.3729 0.055 Uiso 0.373(16) 1 calc PR A 2 H9'B H 0.1409 1.0000 0.3237 0.055 Uiso 0.373(16) 1 calc PR A 2 C10 C 0.2243(2) 0.9959(4) 0.4976(4) 0.0342(9) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0182(3) 0.0197(3) 0.0214(3) -0.00109(17) 0.0119(2) -0.00149(17) Co2 0.0273(3) 0.0221(3) 0.0354(3) -0.0042(2) 0.0213(3) -0.00072(19) O2 0.0231(14) 0.0316(16) 0.068(2) -0.0112(15) 0.0232(15) -0.0004(12) O1 0.0182(13) 0.0302(14) 0.0329(15) -0.0036(12) 0.0105(12) -0.0019(11) O3 0.0368(15) 0.0230(13) 0.0376(15) -0.0091(11) 0.0264(13) -0.0048(11) O4 0.0445(18) 0.0257(14) 0.058(2) -0.0010(13) 0.0401(17) 0.0015(13) O5 0.0329(15) 0.0183(12) 0.0400(15) -0.0037(11) 0.0277(13) -0.0036(10) O6 0.0273(13) 0.0201(12) 0.0259(13) 0.0013(10) 0.0170(11) 0.0016(10) O7 0.0500(19) 0.0296(15) 0.0370(16) -0.0016(13) 0.0264(15) -0.0130(14) N1 0.0188(15) 0.0318(17) 0.0278(17) 0.0019(13) 0.0115(14) 0.0031(13) C1 0.0198(18) 0.028(2) 0.0293(19) -0.0016(16) 0.0122(16) 0.0012(15) C2 0.0186(18) 0.032(2) 0.0252(18) -0.0020(15) 0.0096(15) 0.0012(15) C3 0.023(2) 0.029(2) 0.052(3) -0.0062(19) 0.016(2) -0.0025(16) C4 0.026(2) 0.028(2) 0.054(3) -0.0039(19) 0.018(2) 0.0020(17) C5 0.020(2) 0.031(2) 0.052(3) 0.002(2) 0.0098(19) -0.0009(17) C6 0.025(2) 0.029(2) 0.056(3) 0.001(2) 0.015(2) 0.0039(17) C7 0.032(2) 0.025(2) 0.035(2) 0.0022(16) 0.0229(18) 0.0040(16) C8 0.023(4) 0.019(3) 0.031(4) 0.001(3) 0.016(3) -0.001(2) C9 0.035(5) 0.022(3) 0.036(4) -0.001(3) 0.021(4) 0.002(3) C9' 0.046(10) 0.044(8) 0.047(8) -0.009(6) 0.029(8) -0.009(7) C10 0.037(2) 0.030(2) 0.032(2) -0.0060(17) 0.0198(19) -0.0033(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O5 2.008(3) 4_545 ? Co1 O3 2.074(3) . ? Co1 O1 2.089(3) . ? Co1 O6 2.120(3) 4_545 ? Co1 O6 2.144(3) 6_575 ? Co1 N1 2.161(3) 8_465 ? Co2 O5 1.938(3) . ? Co2 O2 1.964(3) . ? Co2 O7 2.002(3) 6_575 ? Co2 O4 2.073(3) 4 ? Co2 O3 2.112(3) . ? O2 C1 1.256(5) . ? O1 C1 1.238(5) . ? O3 C7 1.243(5) . ? O4 C7 1.252(5) . ? O4 Co2 2.073(3) 4_545 ? O5 C8 1.407(6) . ? O5 C8' 1.418(12) . ? O5 Co1 2.008(3) 4 ? O6 C10 1.278(5) . ? O6 Co1 2.120(3) 4 ? O6 Co1 2.144(3) 6_576 ? O7 C10 1.250(6) . ? O7 Co2 2.002(3) 6_576 ? N1 C5 1.326(6) . ? N1 C4 1.330(6) . ? N1 Co1 2.161(3) 8_566 ? C1 C2 1.512(5) . ? C2 C6 1.352(6) . ? C2 C3 1.386(6) . ? C3 C4 1.369(6) . ? C3 H3A 0.9276 . ? C4 H4A 0.9270 . ? C5 C6 1.397(6) . ? C5 H5A 0.9274 . ? C6 H6A 0.9269 . ? C7 C8 1.529(7) . ? C7 C8' 1.562(11) . ? C8 C9 1.521(9) . ? C8 H8A 0.9800 . ? C9 C10 1.506(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C8' C9' 1.508(13) . ? C8' H8'A 0.9800 . ? C9' C10 1.522(11) . ? C9' H9'A 0.9700 . ? C9' H9'B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Co1 O3 96.72(11) 4_545 . ? O5 Co1 O1 90.48(12) 4_545 . ? O3 Co1 O1 88.05(11) . . ? O5 Co1 O6 89.86(10) 4_545 4_545 ? O3 Co1 O6 172.29(11) . 4_545 ? O1 Co1 O6 87.88(11) . 4_545 ? O5 Co1 O6 168.18(10) 4_545 6_575 ? O3 Co1 O6 95.10(11) . 6_575 ? O1 Co1 O6 89.83(11) . 6_575 ? O6 Co1 O6 78.35(10) 4_545 6_575 ? O5 Co1 N1 90.33(12) 4_545 8_465 ? O3 Co1 N1 89.70(12) . 8_465 ? O1 Co1 N1 177.68(12) . 8_465 ? O6 Co1 N1 94.29(12) 4_545 8_465 ? O6 Co1 N1 89.82(11) 6_575 8_465 ? O5 Co2 O2 128.58(15) . . ? O5 Co2 O7 122.00(13) . 6_575 ? O2 Co2 O7 108.26(15) . 6_575 ? O5 Co2 O4 99.37(11) . 4 ? O2 Co2 O4 90.64(13) . 4 ? O7 Co2 O4 89.57(13) 6_575 4 ? O5 Co2 O3 79.67(11) . . ? O2 Co2 O3 92.58(12) . . ? O7 Co2 O3 88.12(12) 6_575 . ? O4 Co2 O3 176.50(12) 4 . ? C1 O2 Co2 134.9(3) . . ? C1 O1 Co1 132.0(3) . . ? C7 O3 Co1 131.2(3) . . ? C7 O3 Co2 115.1(2) . . ? Co1 O3 Co2 113.62(13) . . ? C7 O4 Co2 124.7(3) . 4_545 ? C8 O5 C8' 25.4(6) . . ? C8 O5 Co2 116.1(3) . . ? C8' O5 Co2 114.9(5) . . ? C8 O5 Co1 119.5(3) . 4 ? C8' O5 Co1 122.5(5) . 4 ? Co2 O5 Co1 121.81(13) . 4 ? C10 O6 Co1 127.0(3) . 4 ? C10 O6 Co1 131.0(3) . 6_576 ? Co1 O6 Co1 101.65(10) 4 6_576 ? C10 O7 Co2 126.3(3) . 6_576 ? C5 N1 C4 116.3(4) . . ? C5 N1 Co1 119.9(3) . 8_566 ? C4 N1 Co1 123.5(3) . 8_566 ? O1 C1 O2 127.8(4) . . ? O1 C1 C2 117.7(4) . . ? O2 C1 C2 114.4(3) . . ? C6 C2 C3 117.9(4) . . ? C6 C2 C1 120.4(4) . . ? C3 C2 C1 121.8(4) . . ? C4 C3 C2 118.9(4) . . ? C4 C3 H3A 121.1 . . ? C2 C3 H3A 120.0 . . ? N1 C4 C3 124.2(4) . . ? N1 C4 H4A 118.0 . . ? C3 C4 H4A 117.7 . . ? N1 C5 C6 123.2(4) . . ? N1 C5 H5A 118.0 . . ? C6 C5 H5A 118.8 . . ? C2 C6 C5 119.4(4) . . ? C2 C6 H6A 120.5 . . ? C5 C6 H6A 120.0 . . ? O3 C7 O4 124.1(4) . . ? O3 C7 C8 115.4(4) . . ? O4 C7 C8 120.1(4) . . ? O3 C7 C8' 112.9(5) . . ? O4 C7 C8' 120.2(5) . . ? C8 C7 C8' 23.1(5) . . ? O5 C8 C9 110.4(6) . . ? O5 C8 C7 111.1(4) . . ? C9 C8 C7 104.5(5) . . ? O5 C8 H8A 110.2 . . ? C9 C8 H8A 110.2 . . ? C7 C8 H8A 110.2 . . ? C10 C9 C8 118.3(5) . . ? C10 C9 H9A 107.7 . . ? C8 C9 H9A 107.7 . . ? C10 C9 H9B 107.7 . . ? C8 C9 H9B 107.7 . . ? H9A C9 H9B 107.1 . . ? O5 C8' C9' 114.9(11) . . ? O5 C8' C7 108.7(8) . . ? C9' C8' C7 113.8(10) . . ? O5 C8' H8'A 106.3 . . ? C9' C8' H8'A 106.3 . . ? C7 C8' H8'A 106.3 . . ? C8' C9' C10 107.1(10) . . ? C8' C9' H9'A 110.3 . . ? C10 C9' H9'A 110.3 . . ? C8' C9' H9'B 110.3 . . ? C10 C9' H9'B 110.3 . . ? H9'A C9' H9'B 108.5 . . ? O7 C10 O6 123.7(4) . . ? O7 C10 C9 112.8(4) . . ? O6 C10 C9 122.5(4) . . ? O7 C10 C9' 118.3(6) . . ? O6 C10 C9' 112.8(7) . . ? C9 C10 C9' 35.1(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Co2 O2 C1 89.5(5) . . . . ? O7 Co2 O2 C1 -78.2(5) 6_575 . . . ? O4 Co2 O2 C1 -167.9(5) 4 . . . ? O3 Co2 O2 C1 10.7(5) . . . . ? O5 Co1 O1 C1 -134.4(4) 4_545 . . . ? O3 Co1 O1 C1 -37.7(4) . . . . ? O6 Co1 O1 C1 135.8(4) 4_545 . . . ? O6 Co1 O1 C1 57.4(4) 6_575 . . . ? N1 Co1 O1 C1 -24(3) 8_465 . . . ? O5 Co1 O3 C7 -34.8(4) 4_545 . . . ? O1 Co1 O3 C7 -125.0(4) . . . . ? O6 Co1 O3 C7 176.9(7) 4_545 . . . ? O6 Co1 O3 C7 145.3(4) 6_575 . . . ? N1 Co1 O3 C7 55.5(4) 8_465 . . . ? O5 Co1 O3 Co2 147.48(14) 4_545 . . . ? O1 Co1 O3 Co2 57.23(15) . . . . ? O6 Co1 O3 Co2 -0.9(9) 4_545 . . . ? O6 Co1 O3 Co2 -32.42(14) 6_575 . . . ? N1 Co1 O3 Co2 -122.22(15) 8_465 . . . ? O5 Co2 O3 C7 2.5(3) . . . . ? O2 Co2 O3 C7 131.2(3) . . . . ? O7 Co2 O3 C7 -120.6(3) 6_575 . . . ? O4 Co2 O3 C7 -72(2) 4 . . . ? O5 Co2 O3 Co1 -179.40(16) . . . . ? O2 Co2 O3 Co1 -50.62(17) . . . . ? O7 Co2 O3 Co1 57.58(15) 6_575 . . . ? O4 Co2 O3 Co1 106.2(19) 4 . . . ? O2 Co2 O5 C8 -96.4(4) . . . . ? O7 Co2 O5 C8 69.8(4) 6_575 . . . ? O4 Co2 O5 C8 165.2(4) 4 . . . ? O3 Co2 O5 C8 -11.4(4) . . . . ? O2 Co2 O5 C8' -68.3(8) . . . . ? O7 Co2 O5 C8' 97.9(8) 6_575 . . . ? O4 Co2 O5 C8' -166.7(8) 4 . . . ? O3 Co2 O5 C8' 16.7(8) . . . . ? O2 Co2 O5 Co1 101.62(18) . . . 4 ? O7 Co2 O5 Co1 -92.18(19) 6_575 . . 4 ? O4 Co2 O5 Co1 3.22(18) 4 . . 4 ? O3 Co2 O5 Co1 -173.36(18) . . . 4 ? Co1 O1 C1 O2 1.7(7) . . . . ? Co1 O1 C1 C2 -175.8(3) . . . . ? Co2 O2 C1 O1 16.1(8) . . . . ? Co2 O2 C1 C2 -166.2(3) . . . . ? O1 C1 C2 C6 162.4(4) . . . . ? O2 C1 C2 C6 -15.5(6) . . . . ? O1 C1 C2 C3 -17.7(6) . . . . ? O2 C1 C2 C3 164.4(4) . . . . ? C6 C2 C3 C4 1.6(7) . . . . ? C1 C2 C3 C4 -178.3(5) . . . . ? C5 N1 C4 C3 1.0(8) . . . . ? Co1 N1 C4 C3 174.7(4) 8_566 . . . ? C2 C3 C4 N1 -2.5(8) . . . . ? C4 N1 C5 C6 1.4(8) . . . . ? Co1 N1 C5 C6 -172.5(4) 8_566 . . . ? C3 C2 C6 C5 0.6(8) . . . . ? C1 C2 C6 C5 -179.5(5) . . . . ? N1 C5 C6 C2 -2.3(9) . . . . ? Co1 O3 C7 O4 2.2(6) . . . . ? Co2 O3 C7 O4 179.9(3) . . . . ? Co1 O3 C7 C8 -171.5(4) . . . . ? Co2 O3 C7 C8 6.3(5) . . . . ? Co1 O3 C7 C8' 163.3(7) . . . . ? Co2 O3 C7 C8' -19.0(8) . . . . ? Co2 O4 C7 O3 46.2(6) 4_545 . . . ? Co2 O4 C7 C8 -140.5(4) 4_545 . . . ? Co2 O4 C7 C8' -113.7(8) 4_545 . . . ? C8' O5 C8 C9 39.6(12) . . . . ? Co2 O5 C8 C9 132.9(5) . . . . ? Co1 O5 C8 C9 -64.7(7) 4 . . . ? C8' O5 C8 C7 -75.9(12) . . . . ? Co2 O5 C8 C7 17.4(7) . . . . ? Co1 O5 C8 C7 179.8(3) 4 . . . ? O3 C7 C8 O5 -15.2(7) . . . . ? O4 C7 C8 O5 170.8(5) . . . . ? C8' C7 C8 O5 73.8(13) . . . . ? O3 C7 C8 C9 -134.3(5) . . . . ? O4 C7 C8 C9 51.7(7) . . . . ? C8' C7 C8 C9 -45.3(12) . . . . ? O5 C8 C9 C10 62.7(9) . . . . ? C7 C8 C9 C10 -177.7(5) . . . . ? C8 O5 C8' C9' -59.6(14) . . . . ? Co2 O5 C8' C9' -158.6(9) . . . . ? Co1 O5 C8' C9' 31.6(15) 4 . . . ? C8 O5 C8' C7 69.2(13) . . . . ? Co2 O5 C8' C7 -29.8(12) . . . . ? Co1 O5 C8' C7 160.4(5) 4 . . . ? O3 C7 C8' O5 31.6(12) . . . . ? O4 C7 C8' O5 -166.4(7) . . . . ? C8 C7 C8' O5 -69.8(13) . . . . ? O3 C7 C8' C9' 161.0(11) . . . . ? O4 C7 C8' C9' -37.0(16) . . . . ? C8 C7 C8' C9' 59.6(14) . . . . ? O5 C8' C9' C10 -75.0(16) . . . . ? C7 C8' C9' C10 158.8(9) . . . . ? Co2 O7 C10 O6 -40.5(6) 6_576 . . . ? Co2 O7 C10 C9 128.2(4) 6_576 . . . ? Co2 O7 C10 C9' 166.7(8) 6_576 . . . ? Co1 O6 C10 O7 176.1(3) 4 . . . ? Co1 O6 C10 O7 -12.1(6) 6_576 . . . ? Co1 O6 C10 C9 8.5(7) 4 . . . ? Co1 O6 C10 C9 -179.7(4) 6_576 . . . ? Co1 O6 C10 C9' -29.8(8) 4 . . . ? Co1 O6 C10 C9' 142.0(7) 6_576 . . . ? C8 C9 C10 O7 157.1(6) . . . . ? C8 C9 C10 O6 -34.1(9) . . . . ? C8 C9 C10 C9' 49.9(10) . . . . ? C8' C9' C10 O7 -131.5(10) . . . . ? C8' C9' C10 O6 72.9(13) . . . . ? C8' C9' C10 C9 -41.6(9) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.487 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.148 #===============================END