Electronic Supplementary Material for CrystEngComm This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _ccdc_journal_manuscript_code B510684B _publ_contact_author_name 'Susan A Bourne' _publ_contact_author_address ;Department of Chemistry University of Cape Town Rondebosch 7701 South Africa ; _publ_contact_author_email xraysue@science.uct.ac.za _publ_contact_author_phone '+27 21 650 2563' _publ_contact_author_fax '+27 21 689 7499' loop_ _publ_author_name _publ_author_address S.Bourne ;Department of Chemistry University of Cape Town Rondebosch 7701 South Africa ; L.Moitsheki ;Department of Chemistry University of Cape Town Rondebosch 7701 South Africa ; _publ_section_title ; Anion dependent structural diversity in cobalt (II) complexes of 4,4'-bipyridine-N,N'-dioxide ; data_1 _database_code_depnum_ccdc_archive 'CCDC 279570' _ccdc_journal_manuscript_code B510684B _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Co(H2O)6]Br2 . 2(bpdo) . 2H2O ; _chemical_name_common '(Co(H2O)6)Br2 . 2(bpdo) . 2H2O' _chemical_melting_point ? _chemical_formula_moiety '(Co (H2O)6), Br2, 2(C10 H8 N2 O2), 2(H2 O)' _chemical_formula_sum 'C20 H28 Br2 Co N4 O12' _chemical_formula_weight 735.21 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.3728(2) _cell_length_b 6.6329(1) _cell_length_c 20.0945(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.336(1) _cell_angle_gamma 90.00 _cell_volume 1378.58(4) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.771 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 738 _exptl_absorpt_coefficient_mu 3.587 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4333 _exptl_absorpt_correction_T_max 0.5340 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(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 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22395 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 27.88 _reflns_number_total 3295 _reflns_number_gt 2882 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+11.0541P] 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 3295 _refine_ls_number_parameters 209 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1138 _refine_ls_wR_factor_gt 0.1116 _refine_ls_goodness_of_fit_ref 1.171 _refine_ls_restrained_S_all 1.170 _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 Br1A Br 0.39143(4) 0.73924(7) 0.02844(2) 0.01497(15) Uani 0.925(3) 1 d P A 1 O1WA O 1.3435(3) 1.2370(6) 0.05481(18) 0.0241(7) Uani 0.925(3) 1 d P A 1 Br1B Br 1.3909(6) 1.2630(11) 0.0287(3) 0.0241(7) Uani 0.08 1 d P A 2 O1WB O 0.324(4) 0.800(6) 0.058(2) 0.01497(15) Uani 0.08 1 d P A 2 Co1 Co 1.0000 1.0000 0.0000 0.0096(2) Uani 1 2 d S . . O2 O 1.1075(3) 0.8546(5) 0.08105(16) 0.0192(7) Uani 1 1 d D . . H21 H 1.076(7) 0.713(8) 0.090(4) 0.06(2) Uiso 1 1 d D . . H22 H 1.198(4) 0.824(10) 0.074(3) 0.045(19) Uiso 1 1 d D . . O3 O 0.8490(3) 1.0574(6) 0.05963(17) 0.0244(8) Uani 1 1 d D . . H31 H 0.840(6) 0.912(6) 0.063(3) 0.05(2) Uiso 1 1 d D . . H32 H 0.766(5) 1.121(9) 0.044(3) 0.047(19) Uiso 1 1 d D . . O4 O 1.0866(3) 1.2721(5) 0.02800(16) 0.0197(7) Uani 1 1 d D . . H41 H 1.181(5) 1.241(12) 0.045(4) 0.07(2) Uiso 1 1 d D . . H42 H 1.055(6) 1.346(10) 0.065(3) 0.05(2) Uiso 1 1 d D . . O1 O 1.0265(3) 0.5073(5) 0.13435(15) 0.0151(6) Uani 1 1 d . . . N2 N 0.9116(3) 0.5054(5) 0.15945(18) 0.0129(7) Uani 1 1 d . . . C3 C 0.8034(4) 0.5173(7) 0.1179(2) 0.0148(8) Uani 1 1 d . . . H3 H 0.8102 0.5273 0.0711 0.018 Uiso 1 1 calc R . . C4 C 0.6832(4) 0.5151(7) 0.1428(2) 0.0137(8) Uani 1 1 d . . . H4 H 0.6079 0.5234 0.1129 0.016 Uiso 1 1 calc R . . C5 C 0.6708(4) 0.5006(6) 0.21201(19) 0.0091(7) Uani 1 1 d . . . C6 C 0.7859(4) 0.4900(7) 0.2529(2) 0.0143(8) Uani 1 1 d . . . H6 H 0.7825 0.4817 0.2999 0.017 Uiso 1 1 calc R . . C7 C 0.9042(4) 0.4915(7) 0.2261(2) 0.0146(8) Uani 1 1 d . . . H7 H 0.9812 0.4827 0.2547 0.017 Uiso 1 1 calc R . . O8 O 0.1832(3) 0.4910(5) 0.31379(15) 0.0182(7) Uani 1 1 d . . . N9 N 0.2986(3) 0.4946(5) 0.29060(17) 0.0124(7) Uani 1 1 d . . . C10 C 0.3084(4) 0.4932(6) 0.2234(2) 0.0127(8) Uani 1 1 d . . . H10 H 0.2322 0.4904 0.1940 0.015 Uiso 1 1 calc R . . C11 C 0.4273(4) 0.4956(6) 0.1978(2) 0.0123(8) Uani 1 1 d . . . H11 H 0.4319 0.4950 0.1508 0.015 Uiso 1 1 calc R . . C12 C 0.5420(4) 0.4991(6) 0.23926(19) 0.0095(7) Uani 1 1 d . . . C13 C 0.5284(4) 0.5005(6) 0.3080(2) 0.0126(8) Uani 1 1 d . . . H13 H 0.6034 0.5030 0.3381 0.015 Uiso 1 1 calc R . . C14 C 0.4072(4) 0.4981(6) 0.3328(2) 0.0134(8) Uani 1 1 d . . . H14 H 0.4002 0.4989 0.3796 0.016 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1A 0.0114(2) 0.0190(2) 0.0144(2) 0.00089(18) -0.00037(15) 0.00291(18) O1WA 0.0175(18) 0.0342(18) 0.0209(19) -0.0013(16) 0.0030(11) -0.0019(16) Br1B 0.0175(18) 0.0342(18) 0.0209(19) -0.0013(16) 0.0030(11) -0.0019(16) O1WB 0.0114(2) 0.0190(2) 0.0144(2) 0.00089(18) -0.00037(15) 0.00291(18) Co1 0.0077(3) 0.0139(4) 0.0073(4) -0.0001(3) 0.0015(3) 0.0008(3) O2 0.0165(15) 0.0233(17) 0.0176(16) 0.0034(13) 0.0008(12) 0.0000(13) O3 0.0147(15) 0.042(2) 0.0171(16) 0.0051(15) 0.0047(12) 0.0086(15) O4 0.0171(15) 0.0219(17) 0.0201(16) -0.0026(14) 0.0020(12) -0.0012(13) O1 0.0075(13) 0.0223(16) 0.0161(14) 0.0001(12) 0.0049(11) 0.0010(12) N2 0.0079(15) 0.0156(18) 0.0154(17) 0.0003(14) 0.0027(13) 0.0005(13) C3 0.0131(19) 0.021(2) 0.0106(18) 0.0002(16) 0.0005(15) -0.0001(17) C4 0.0098(18) 0.019(2) 0.0127(19) -0.0002(16) 0.0011(14) -0.0009(16) C5 0.0081(17) 0.0080(18) 0.0111(18) -0.0003(14) 0.0003(14) 0.0002(14) C6 0.0134(19) 0.019(2) 0.0110(18) 0.0015(16) 0.0009(15) 0.0001(16) C7 0.0090(18) 0.020(2) 0.0141(19) 0.0026(17) -0.0013(14) 0.0005(16) O8 0.0091(13) 0.0325(19) 0.0136(15) -0.0014(13) 0.0045(11) -0.0005(13) N9 0.0073(15) 0.0171(18) 0.0133(17) 0.0002(14) 0.0028(12) -0.0003(13) C10 0.0099(17) 0.017(2) 0.0106(18) -0.0006(16) -0.0024(14) 0.0001(15) C11 0.0121(18) 0.016(2) 0.0089(17) 0.0004(15) -0.0005(14) 0.0007(16) C12 0.0089(17) 0.0080(17) 0.0114(18) 0.0011(14) -0.0001(14) 0.0004(14) C13 0.0102(18) 0.015(2) 0.0121(19) -0.0005(16) 0.0004(14) 0.0004(16) C14 0.0152(19) 0.015(2) 0.0096(18) -0.0001(15) 0.0005(15) 0.0008(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O4 2.075(3) 3_775 ? Co1 O4 2.075(3) . ? Co1 O3 2.078(3) 3_775 ? Co1 O3 2.078(3) . ? Co1 O2 2.134(3) 3_775 ? Co1 O2 2.134(3) . ? O1 N2 1.329(4) . ? N2 C7 1.350(5) . ? N2 C3 1.350(5) . ? C3 C4 1.378(5) . ? C4 C5 1.410(5) . ? C5 C6 1.400(5) . ? C5 C12 1.481(5) . ? C6 C7 1.377(6) . ? O8 N9 1.317(4) . ? N9 C14 1.358(5) . ? N9 C10 1.361(5) . ? C10 C11 1.372(5) . ? C11 C12 1.400(5) . ? C12 C13 1.398(5) . ? C13 C14 1.387(5) . ? 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 O4 Co1 O4 180.00(17) 3_775 . ? O4 Co1 O3 90.80(14) 3_775 3_775 ? O4 Co1 O3 89.20(14) . 3_775 ? O4 Co1 O3 89.20(14) 3_775 . ? O4 Co1 O3 90.80(14) . . ? O3 Co1 O3 180.0(2) 3_775 . ? O4 Co1 O2 89.76(13) 3_775 3_775 ? O4 Co1 O2 90.24(13) . 3_775 ? O3 Co1 O2 90.92(13) 3_775 3_775 ? O3 Co1 O2 89.08(13) . 3_775 ? O4 Co1 O2 90.24(13) 3_775 . ? O4 Co1 O2 89.76(13) . . ? O3 Co1 O2 89.08(13) 3_775 . ? O3 Co1 O2 90.92(13) . . ? O2 Co1 O2 180.00(12) 3_775 . ? O1 N2 C7 119.8(3) . . ? O1 N2 C3 119.5(3) . . ? C7 N2 C3 120.7(3) . . ? N2 C3 C4 120.5(4) . . ? C3 C4 C5 120.8(4) . . ? C6 C5 C4 116.4(4) . . ? C6 C5 C12 122.4(4) . . ? C4 C5 C12 121.2(3) . . ? C7 C6 C5 121.0(4) . . ? N2 C7 C6 120.6(4) . . ? O8 N9 C14 120.9(3) . . ? O8 N9 C10 119.2(3) . . ? C14 N9 C10 119.9(3) . . ? N9 C10 C11 120.5(4) . . ? C10 C11 C12 121.7(4) . . ? C13 C12 C11 116.2(3) . . ? C13 C12 C5 121.7(3) . . ? C11 C12 C5 122.0(4) . . ? C14 C13 C12 121.1(4) . . ? N9 C14 C13 120.5(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.924 _refine_diff_density_min -3.105 _refine_diff_density_rms 0.143 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 279571' _audit_creation_method SHELXL-97 _chemical_name_systematic '[Co(H2O)6]Cl2 . 2(bpdo) . 2(H2O)' _chemical_name_common '(Co(H2O)6)Cl2 . 2(bpdo) . 2(H2O)' _chemical_melting_point ? _chemical_formula_moiety '(Co (H2 O)6), Cl2, 2(C10 H8 N2 O2), 2(H2 O)' _chemical_formula_sum 'C20 H32 Cl2 Co N4 O12' _chemical_formula_weight 650.33 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' O O 0.0106 0.0060 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.7328(2) _cell_length_b 10.2841(3) _cell_length_c 10.6577(3) _cell_angle_alpha 85.2000(10) _cell_angle_beta 70.0230(10) _cell_angle_gamma 91.1030(10) _cell_volume 690.21(3) _cell_formula_units_Z 1 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour Pink _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 337 _exptl_absorpt_coefficient_mu 0.882 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9016 _exptl_absorpt_correction_T_max 0.9572 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71070 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13961 _diffrn_reflns_av_R_equivalents 0.1876 _diffrn_reflns_av_sigmaI/netI 0.1139 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.68 _reflns_number_total 2614 _reflns_number_gt 1648 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1699P)^2^+2.0496P] 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 SHELXL _refine_ls_extinction_coef 0.031(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2614 _refine_ls_number_parameters 179 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1552 _refine_ls_R_factor_gt 0.1055 _refine_ls_wR_factor_ref 0.3124 _refine_ls_wR_factor_gt 0.2736 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.0000 0.5000 1.0000 0.0342(6) Uani 1 2 d S . . O2 O 0.0096(11) 0.3425(6) 0.8879(6) 0.0561(18) Uani 1 1 d . . . O3 O 0.2298(10) 0.4125(6) 1.0637(7) 0.0533(17) Uani 1 1 d . . . O4 O 0.2403(10) 0.6113(6) 0.8374(6) 0.0492(16) Uani 1 1 d . . . O1 O 0.1884(11) 0.3133(5) 0.6326(6) 0.0510(17) Uani 1 1 d . . . N2 N 0.2079(10) 0.1971(6) 0.5863(6) 0.0335(15) Uani 1 1 d . . . C3 C 0.1633(13) 0.0867(8) 0.6698(8) 0.0384(19) Uani 1 1 d . . . H3 H 0.1160 0.0916 0.7640 0.046 Uiso 1 1 calc R . . C4 C 0.1855(12) -0.0328(7) 0.6203(7) 0.0348(18) Uani 1 1 d . . . H4 H 0.1510 -0.1096 0.6811 0.042 Uiso 1 1 calc R . . C5 C 0.2573(11) -0.0444(7) 0.4829(7) 0.0291(16) Uani 1 1 d . . . C6 C 0.3039(12) 0.0723(8) 0.4011(8) 0.0347(18) Uani 1 1 d . . . H6 H 0.3555 0.0699 0.3066 0.042 Uiso 1 1 calc R . . C7 C 0.2781(12) 0.1897(8) 0.4520(8) 0.0367(19) Uani 1 1 d . . . H7 H 0.3095 0.2677 0.3929 0.044 Uiso 1 1 calc R . . O8 O 0.3632(9) -0.5276(5) 0.2701(6) 0.0437(15) Uani 1 1 d . . . N9 N 0.3393(10) -0.4128(6) 0.3212(6) 0.0329(15) Uani 1 1 d . . . C10 C 0.2625(13) -0.4085(8) 0.4550(8) 0.040(2) Uani 1 1 d . . . H10 H 0.2271 -0.4878 0.5119 0.048 Uiso 1 1 calc R . . C11 C 0.2342(13) -0.2915(7) 0.5109(7) 0.0365(19) Uani 1 1 d . . . H11 H 0.1798 -0.2901 0.6055 0.044 Uiso 1 1 calc R . . C12 C 0.2869(11) -0.1732(7) 0.4262(8) 0.0307(17) Uani 1 1 d . . . C13 C 0.3661(13) -0.1824(8) 0.2892(8) 0.040(2) Uani 1 1 d . . . H13 H 0.4034 -0.1048 0.2295 0.048 Uiso 1 1 calc R . . C14 C 0.3916(13) -0.3016(8) 0.2381(8) 0.041(2) Uani 1 1 d . . . H14 H 0.4464 -0.3057 0.1438 0.049 Uiso 1 1 calc R . . Cl1 Cl 0.2713(4) 0.8897(2) 0.9386(2) 0.0554(8) Uani 1 1 d . . . O1W O 0.7517(14) 0.8513(7) 0.9113(8) 0.076(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0533(11) 0.0224(9) 0.0249(9) -0.0070(6) -0.0099(7) 0.0024(6) O2 0.097(5) 0.031(3) 0.027(3) -0.010(3) -0.004(3) -0.016(3) O3 0.071(4) 0.044(4) 0.056(4) -0.010(3) -0.035(3) 0.010(3) O4 0.066(4) 0.034(3) 0.041(3) -0.009(3) -0.008(3) 0.000(3) O1 0.096(5) 0.014(3) 0.033(3) -0.010(2) -0.007(3) 0.004(3) N2 0.049(4) 0.020(3) 0.027(3) -0.006(3) -0.006(3) 0.002(3) C3 0.060(5) 0.027(4) 0.023(4) -0.004(3) -0.006(3) 0.002(4) C4 0.054(5) 0.022(4) 0.023(4) -0.001(3) -0.007(3) -0.002(3) C5 0.037(4) 0.022(4) 0.028(4) -0.003(3) -0.010(3) 0.000(3) C6 0.048(5) 0.025(4) 0.027(4) -0.004(3) -0.007(3) 0.003(3) C7 0.050(5) 0.027(4) 0.024(4) 0.004(3) -0.002(3) -0.002(3) O8 0.070(4) 0.021(3) 0.038(3) -0.010(2) -0.014(3) 0.004(3) N9 0.047(4) 0.022(3) 0.028(3) -0.005(3) -0.010(3) 0.003(3) C10 0.058(5) 0.031(5) 0.025(4) 0.001(3) -0.009(4) 0.000(4) C11 0.065(5) 0.022(4) 0.019(4) 0.000(3) -0.010(4) 0.001(4) C12 0.037(4) 0.022(4) 0.035(4) -0.007(3) -0.013(3) 0.004(3) C13 0.067(5) 0.023(4) 0.021(4) 0.001(3) -0.004(4) -0.001(4) C14 0.061(5) 0.029(4) 0.026(4) -0.002(3) -0.008(4) -0.002(4) Cl1 0.0736(17) 0.0348(14) 0.0496(15) -0.0033(11) -0.0112(12) -0.0068(11) O1W 0.127(6) 0.040(4) 0.062(5) 0.005(4) -0.037(5) 0.001(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 O2 2.081(6) 2_567 ? Co1 O2 2.081(6) . ? Co1 O3 2.082(6) . ? Co1 O3 2.082(6) 2_567 ? Co1 O4 2.148(6) . ? Co1 O4 2.148(6) 2_567 ? O1 N2 1.323(8) . ? N2 C3 1.344(11) . ? N2 C7 1.355(10) . ? C3 C4 1.368(11) . ? C4 C5 1.392(11) . ? C5 C6 1.387(11) . ? C5 C12 1.490(10) . ? C6 C7 1.355(11) . ? O8 N9 1.332(8) . ? N9 C10 1.345(10) . ? N9 C14 1.349(11) . ? C10 C11 1.375(11) . ? C11 C12 1.415(11) . ? C12 C13 1.384(11) . ? C13 C14 1.373(11) . ? 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 O2 Co1 O2 179.999(2) 2_567 . ? O2 Co1 O3 92.3(3) 2_567 . ? O2 Co1 O3 87.7(3) . . ? O2 Co1 O3 87.7(3) 2_567 2_567 ? O2 Co1 O3 92.3(3) . 2_567 ? O3 Co1 O3 179.999(2) . 2_567 ? O2 Co1 O4 87.3(2) 2_567 . ? O2 Co1 O4 92.7(2) . . ? O3 Co1 O4 90.7(3) . . ? O3 Co1 O4 89.3(3) 2_567 . ? O2 Co1 O4 92.7(2) 2_567 2_567 ? O2 Co1 O4 87.3(2) . 2_567 ? O3 Co1 O4 89.3(3) . 2_567 ? O3 Co1 O4 90.7(3) 2_567 2_567 ? O4 Co1 O4 180.000(1) . 2_567 ? O1 N2 C3 121.3(6) . . ? O1 N2 C7 119.1(6) . . ? C3 N2 C7 119.6(7) . . ? N2 C3 C4 120.6(7) . . ? C3 C4 C5 121.6(7) . . ? C6 C5 C4 115.6(7) . . ? C6 C5 C12 121.6(7) . . ? C4 C5 C12 122.7(7) . . ? C7 C6 C5 122.0(7) . . ? C6 C7 N2 120.7(7) . . ? O8 N9 C10 119.9(6) . . ? O8 N9 C14 119.5(6) . . ? C10 N9 C14 120.6(7) . . ? N9 C10 C11 121.3(7) . . ? C10 C11 C12 119.4(7) . . ? C13 C12 C11 117.2(7) . . ? C13 C12 C5 121.8(7) . . ? C11 C12 C5 121.0(7) . . ? C14 C13 C12 121.2(7) . . ? N9 C14 C13 120.2(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.936 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.185 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 279572' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '(CoI2(H2O)4) . 2(bpdo)' _chemical_melting_point ? _chemical_formula_moiety '(Co I2 (H2O)4), 2(C10 H8 N2 O2)' _chemical_formula_sum 'C20 H24 Co I2 N4 O8' _chemical_formula_weight 761.16 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' I I -0.4742 1.8119 '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 tetragonal _symmetry_space_group_name_H-M 'I 41/a c d' _symmetry_int_tables_number 142 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/4, x+3/4, z+1/4' '-x, -y+1/2, z' 'y+1/4, -x+1/4, z+3/4' 'x, -y, -z+1/2' '-x+1/2, y, -z' 'y+3/4, x+1/4, -z+1/4' '-y+1/4, -x+1/4, -z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+3/4, x+5/4, z+3/4' '-x+1/2, -y+1, z+1/2' 'y+3/4, -x+3/4, z+5/4' 'x+1/2, -y+1/2, -z+1' '-x+1, y+1/2, -z+1/2' 'y+5/4, x+3/4, -z+3/4' '-y+3/4, -x+3/4, -z+3/4' '-x, -y, -z' 'y-1/4, -x-3/4, -z-1/4' 'x, y-1/2, -z' '-y-1/4, x-1/4, -z-3/4' '-x, y, z-1/2' 'x-1/2, -y, z' '-y-3/4, -x-1/4, z-1/4' 'y-1/4, x-1/4, z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'y+1/4, -x-1/4, -z+1/4' 'x+1/2, y, -z+1/2' '-y+1/4, x+1/4, -z-1/4' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-y-1/4, -x+1/4, z+1/4' 'y+1/4, x+1/4, z+1/4' _cell_length_a 19.149(3) _cell_length_b 19.149(3) _cell_length_c 13.917(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5102.9(14) _cell_formula_units_Z 8 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour purple _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.982 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2952 _exptl_absorpt_coefficient_mu 3.144 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6854 _exptl_absorpt_correction_T_max 0.7870 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24777 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 27.91 _reflns_number_total 1533 _reflns_number_gt 1089 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0163P)^2^+5.8784P] 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 1533 _refine_ls_number_parameters 89 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0186 _refine_ls_wR_factor_ref 0.0441 _refine_ls_wR_factor_gt 0.0399 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.003 _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 0.5000 0.7500 0.1250 0.00891(12) Uani 1 4 d S . . I1 I 0.392789(7) 0.642789(7) 0.1250 0.01423(7) Uani 1 2 d S . . O2 O 0.44977(9) 0.80598(8) 0.01985(10) 0.0120(3) Uani 1 1 d . . . H2A H 0.4277(15) 0.7863(14) -0.020(2) 0.031(9) Uiso 1 1 d . . . H2B H 0.4774(15) 0.8292(15) -0.009(2) 0.027(8) Uiso 1 1 d . . . O1 O 0.51272(7) 0.87940(7) -0.12244(13) 0.0126(3) Uani 1 1 d . . . N2 N 0.56305(8) 0.92718(8) -0.12128(12) 0.0101(3) Uani 1 1 d . . . C3 C 0.63074(11) 0.90757(11) -0.11850(15) 0.0123(4) Uani 1 1 d . . . H3 H 0.6423 0.8594 -0.1155 0.015 Uiso 1 1 calc R . . C4 C 0.68325(10) 0.95692(10) -0.11994(15) 0.0123(4) Uani 1 1 d . . . H4 H 0.7307 0.9424 -0.1184 0.015 Uiso 1 1 calc R . . C5 C 0.66740(10) 1.02803(10) -0.12371(15) 0.0094(4) Uani 1 1 d . . . C6 C 0.59646(10) 1.04575(10) -0.12481(17) 0.0142(4) Uani 1 1 d . . . H6 H 0.5834 1.0936 -0.1264 0.017 Uiso 1 1 calc R . . C7 C 0.54548(10) 0.99562(10) -0.12368(16) 0.0136(4) Uani 1 1 d . . . H7 H 0.4977 1.0089 -0.1246 0.016 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.00921(16) 0.00921(16) 0.0083(2) 0.000 0.000 0.0015(2) I1 0.01455(8) 0.01455(8) 0.01360(11) -0.00140(6) 0.00140(6) -0.00358(7) O2 0.0112(9) 0.0134(9) 0.0115(7) 0.0013(7) -0.0016(7) -0.0024(6) O1 0.0111(7) 0.0121(7) 0.0148(7) -0.0005(8) -0.0006(8) -0.0070(6) N2 0.0108(8) 0.0094(7) 0.0100(8) 0.0004(8) 0.0009(8) -0.0039(7) C3 0.0146(9) 0.0104(9) 0.0117(10) 0.0005(8) 0.0004(9) -0.0014(8) C4 0.0098(9) 0.0142(10) 0.0128(9) -0.0006(9) -0.0003(9) 0.0011(8) C5 0.0092(9) 0.0116(9) 0.0074(8) 0.0004(9) 0.0017(9) -0.0007(8) C6 0.0143(10) 0.0094(9) 0.0188(10) -0.0003(10) 0.0014(10) -0.0001(8) C7 0.0109(9) 0.0125(9) 0.0175(10) -0.0021(10) 0.0000(10) 0.0013(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 O2 2.0531(14) . ? Co1 O2 2.0532(14) 7_455 ? Co1 O2 2.0532(14) 3_665 ? Co1 O2 2.0532(14) 8_665 ? Co1 I1 2.9032(5) 3_665 ? Co1 I1 2.9033(4) . ? O1 N2 1.329(2) . ? N2 C3 1.350(3) . ? N2 C7 1.353(3) . ? C3 C4 1.380(3) . ? C4 C5 1.396(3) . ? C5 C6 1.400(3) . ? C5 C5 1.478(4) 16_664 ? C6 C7 1.369(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 O2 175.65(10) . 7_455 ? O2 Co1 O2 89.09(8) . 3_665 ? O2 Co1 O2 91.08(8) 7_455 3_665 ? O2 Co1 O2 91.08(8) . 8_665 ? O2 Co1 O2 89.09(8) 7_455 8_665 ? O2 Co1 O2 175.65(10) 3_665 8_665 ? O2 Co1 I1 87.82(5) . 3_665 ? O2 Co1 I1 87.83(5) 7_455 3_665 ? O2 Co1 I1 92.17(5) 3_665 3_665 ? O2 Co1 I1 92.18(5) 8_665 3_665 ? O2 Co1 I1 92.17(5) . . ? O2 Co1 I1 92.17(5) 7_455 . ? O2 Co1 I1 87.83(5) 3_665 . ? O2 Co1 I1 87.83(5) 8_665 . ? I1 Co1 I1 180.0 3_665 . ? O1 N2 C3 120.34(15) . . ? O1 N2 C7 119.08(15) . . ? C3 N2 C7 120.57(17) . . ? N2 C3 C4 120.58(18) . . ? C3 C4 C5 120.66(18) . . ? C4 C5 C6 116.60(17) . . ? C4 C5 C5 122.46(11) . 16_664 ? C6 C5 C5 120.94(11) . 16_664 ? C7 C6 C5 121.44(19) . . ? N2 C7 C6 120.12(18) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.467 _refine_diff_density_min -0.511 _refine_diff_density_rms 0.079 #===END data_4_RT _database_code_depnum_ccdc_archive 'CCDC 279573' _audit_creation_method SHELXL-97 _chemical_name_systematic '[Co(H2O)3(bpdo)(NO3)] NO3 . bpdo . H2O' _chemical_name_common '(Co(H2O)3(bpdo)(NO3)) NO3 . bpdo . H2O' _chemical_melting_point ? _chemical_formula_moiety '(Co 3(H2 O) (C10 H8 N2 O2) (N O3)), N O3, C10 H8 N2 O2, H2 O' _chemical_formula_sum 'C20 H24 Co N6 O14' _chemical_formula_weight 631.38 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' O O 0.0106 0.0060 '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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8139(2) _cell_length_b 9.9126(3) _cell_length_c 17.1863(5) _cell_angle_alpha 78.607(1) _cell_angle_beta 83.460(1) _cell_angle_gamma 85.615(1) _cell_volume 1294.47(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour Orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 650 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8072 _exptl_absorpt_correction_T_max 0.9427 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71070 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32831 _diffrn_reflns_av_R_equivalents 0.1229 _diffrn_reflns_av_sigmaI/netI 0.0918 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 27.84 _reflns_number_total 6132 _reflns_number_gt 3422 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1204P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6132 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1355 _refine_ls_R_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.2094 _refine_ls_wR_factor_gt 0.1793 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 0.97329(7) 0.93732(5) 0.21233(3) 0.0409(2) Uani 1 1 d . . . O2 O 1.2387(4) 0.8886(3) 0.2079(2) 0.0584(8) Uani 1 1 d . . . O3 O 0.7117(4) 0.9975(4) 0.22126(19) 0.0613(8) Uani 1 1 d . . . O4 O 0.9953(4) 1.0624(3) 0.29138(18) 0.0596(8) Uani 1 1 d . . . O5 O 0.9396(4) 0.7352(3) 0.29327(16) 0.0532(8) Uani 1 1 d . . . O6 O 0.9360(4) 0.7525(3) 0.16756(17) 0.0561(8) Uani 1 1 d . . . O1 O 1.0155(4) 1.0582(3) 0.10312(16) 0.0561(8) Uani 1 1 d . . . N2 N 0.9314(4) 1.1786(3) 0.07868(19) 0.0432(8) Uani 1 1 d . . . C3 C 0.9038(6) 1.2735(4) 0.1250(3) 0.0511(11) Uani 1 1 d . . . H3 H 0.9356 1.2526 0.1767 0.061 Uiso 1 1 calc R . . C4 C 0.8291(6) 1.4012(4) 0.0972(2) 0.0473(10) Uani 1 1 d . . . H4 H 0.8091 1.4654 0.1304 0.057 Uiso 1 1 calc R . . C5 C 0.7830(5) 1.4352(4) 0.0194(2) 0.0362(8) Uani 1 1 d . . . C6 C 0.8100(6) 1.3318(4) -0.0255(2) 0.0469(10) Uani 1 1 d . . . H6 H 0.7775 1.3489 -0.0771 0.056 Uiso 1 1 calc R . . O7 O 0.9241(5) 0.5509(3) 0.2436(2) 0.0761(11) Uani 1 1 d . . . C7 C 0.8831(6) 1.2062(4) 0.0045(2) 0.0486(10) Uani 1 1 d . . . H7 H 0.8998 1.1387 -0.0267 0.058 Uiso 1 1 calc R . . O8 O 0.5163(4) 1.9620(3) -0.10625(17) 0.0498(7) Uani 1 1 d . . . N8 N 0.9313(5) 0.6760(4) 0.2357(2) 0.0495(9) Uani 1 1 d . . . N9 N 0.5779(4) 1.8358(3) -0.0766(2) 0.0402(8) Uani 1 1 d . . . C10 C 0.6195(6) 1.8080(4) -0.0015(3) 0.0501(11) Uani 1 1 d . . . H10 H 0.6037 1.8767 0.0289 0.060 Uiso 1 1 calc R . . C11 C 0.6851(6) 1.6797(4) 0.0313(2) 0.0467(10) Uani 1 1 d . . . H11 H 0.7139 1.6625 0.0835 0.056 Uiso 1 1 calc R . . C12 C 0.7091(5) 1.5744(4) -0.0134(2) 0.0373(9) Uani 1 1 d . . . C13 C 0.6644(6) 1.6095(4) -0.0906(2) 0.0480(10) Uani 1 1 d . . . H13 H 0.6797 1.5436 -0.1228 0.058 Uiso 1 1 calc R . . C14 C 0.5983(6) 1.7386(4) -0.1211(2) 0.0485(10) Uani 1 1 d . . . H14 H 0.5674 1.7585 -0.1730 0.058 Uiso 1 1 calc R . . O1G O 1.2703(6) 1.0937(4) 0.3584(4) 0.127(2) Uani 1 1 d . . . N2G N 1.2580(5) 1.2010(4) 0.3938(3) 0.0795(14) Uani 1 1 d . . . C3G C 1.3094(8) 1.1944(6) 0.4668(4) 0.094(2) Uani 1 1 d . . . H3G H 1.3514 1.1104 0.4945 0.113 Uiso 1 1 calc R . . C4G C 1.3016(7) 1.3054(5) 0.5001(4) 0.0747(16) Uani 1 1 d . . . H4G H 1.3399 1.2970 0.5502 0.090 Uiso 1 1 calc R . . C5G C 1.2382(5) 1.4330(5) 0.4625(3) 0.0486(10) Uani 1 1 d . . . C6G C 1.1798(6) 1.4370(5) 0.3890(3) 0.0563(12) Uani 1 1 d . . . H6G H 1.1324 1.5195 0.3620 0.068 Uiso 1 1 calc R . . C7G C 1.1903(7) 1.3225(5) 0.3552(3) 0.0692(14) Uani 1 1 d . . . H7G H 1.1508 1.3279 0.3056 0.083 Uiso 1 1 calc R . . O8G O 1.2324(7) 1.9088(5) 0.5890(3) 0.1164(18) Uani 1 1 d . . . N9G N 1.2259(7) 1.7961(6) 0.5607(3) 0.0794(14) Uani 1 1 d . . . C10G C 1.2802(7) 1.6739(9) 0.6022(3) 0.090(2) Uani 1 1 d . . . H10G H 1.3169 1.6703 0.6523 0.108 Uiso 1 1 calc R . . C11G C 1.2832(6) 1.5539(7) 0.5732(3) 0.0686(14) Uani 1 1 d . . . H11G H 1.3196 1.4706 0.6037 0.082 Uiso 1 1 calc R . . C12G C 1.2312(5) 1.5575(5) 0.4973(2) 0.0495(11) Uani 1 1 d . . . C13G C 1.1731(7) 1.6848(5) 0.4583(3) 0.0630(13) Uani 1 1 d . . . H13G H 1.1334 1.6915 0.4087 0.076 Uiso 1 1 calc R . . C14G C 1.1712(8) 1.8005(6) 0.4889(3) 0.0787(17) Uani 1 1 d . . . H14G H 1.1314 1.8841 0.4599 0.094 Uiso 1 1 calc R . . N11 N 0.4564(5) 0.5750(4) 0.2449(2) 0.0565(10) Uani 1 1 d . . . O14 O 0.5198(5) 0.4567(4) 0.2397(2) 0.0842(12) Uani 1 1 d . . . O12 O 0.4925(7) 0.6353(4) 0.2960(3) 0.1139(17) Uani 1 1 d . . . O13 O 0.3424(6) 0.6266(4) 0.2029(2) 0.0847(12) Uani 1 1 d . . . O1W O 0.5164(5) 0.8849(4) 0.3503(2) 0.0760(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0463(4) 0.0351(3) 0.0407(3) -0.0050(2) -0.0096(2) 0.0038(2) O2 0.0458(17) 0.0405(17) 0.085(2) -0.0026(16) -0.0117(15) 0.0071(13) O3 0.0414(16) 0.075(2) 0.065(2) -0.0082(17) -0.0096(14) 0.0066(15) O4 0.069(2) 0.055(2) 0.062(2) -0.0259(16) -0.0138(16) 0.0037(16) O5 0.079(2) 0.0460(17) 0.0387(16) -0.0097(14) -0.0174(14) -0.0081(15) O6 0.075(2) 0.0513(19) 0.0419(17) -0.0038(14) -0.0144(14) -0.0063(16) O1 0.071(2) 0.0379(16) 0.0473(17) 0.0060(13) 0.0020(14) 0.0215(15) N2 0.0485(19) 0.0318(18) 0.0436(19) -0.0008(15) 0.0014(15) 0.0092(15) C3 0.068(3) 0.043(2) 0.042(2) -0.007(2) -0.013(2) 0.005(2) C4 0.061(3) 0.036(2) 0.045(2) -0.0111(18) -0.011(2) 0.0081(19) C5 0.035(2) 0.030(2) 0.041(2) -0.0030(17) -0.0035(16) 0.0021(15) C6 0.065(3) 0.035(2) 0.040(2) -0.0098(18) -0.0137(19) 0.0143(19) O7 0.119(3) 0.0361(18) 0.078(2) -0.0079(16) -0.025(2) -0.0178(19) C7 0.070(3) 0.033(2) 0.042(2) -0.0104(18) -0.004(2) 0.010(2) O8 0.0573(18) 0.0286(15) 0.0619(18) -0.0049(13) -0.0150(14) 0.0116(13) N8 0.058(2) 0.042(2) 0.050(2) -0.0053(18) -0.0141(17) -0.0082(17) N9 0.0427(18) 0.0266(17) 0.051(2) -0.0052(15) -0.0093(15) 0.0010(14) C10 0.068(3) 0.033(2) 0.053(3) -0.019(2) -0.013(2) 0.010(2) C11 0.064(3) 0.037(2) 0.040(2) -0.0091(18) -0.0152(19) 0.0059(19) C12 0.036(2) 0.033(2) 0.044(2) -0.0093(17) -0.0050(16) -0.0021(16) C13 0.064(3) 0.033(2) 0.049(2) -0.0126(19) -0.015(2) 0.0096(19) C14 0.067(3) 0.038(2) 0.042(2) -0.0088(19) -0.018(2) 0.006(2) O1G 0.090(3) 0.068(3) 0.257(6) -0.090(4) -0.083(4) 0.024(2) N2G 0.059(3) 0.044(2) 0.148(5) -0.036(3) -0.039(3) 0.008(2) C3G 0.093(4) 0.044(3) 0.153(6) -0.004(4) -0.075(4) 0.002(3) C4G 0.082(4) 0.052(3) 0.090(4) 0.010(3) -0.045(3) -0.014(3) C5G 0.040(2) 0.049(3) 0.056(3) -0.004(2) -0.0096(19) -0.0076(19) C6G 0.068(3) 0.041(3) 0.058(3) -0.001(2) -0.014(2) -0.003(2) C7G 0.075(3) 0.055(3) 0.086(4) -0.024(3) -0.025(3) -0.001(3) O8G 0.154(4) 0.114(4) 0.099(3) -0.072(3) 0.040(3) -0.060(3) N9G 0.089(3) 0.097(4) 0.061(3) -0.039(3) 0.017(2) -0.039(3) C10G 0.069(4) 0.161(7) 0.052(3) -0.045(4) -0.007(3) -0.022(4) C11G 0.056(3) 0.095(4) 0.058(3) -0.019(3) -0.012(2) -0.002(3) C12G 0.045(2) 0.062(3) 0.043(2) -0.009(2) -0.0044(18) -0.012(2) C13G 0.095(4) 0.052(3) 0.042(2) -0.007(2) -0.005(2) -0.014(3) C14G 0.122(5) 0.057(3) 0.057(3) -0.014(3) 0.007(3) -0.021(3) N11 0.057(2) 0.050(2) 0.066(3) -0.016(2) -0.0153(19) 0.0067(19) O14 0.092(3) 0.062(2) 0.106(3) -0.036(2) -0.033(2) 0.031(2) O12 0.137(4) 0.076(3) 0.156(4) -0.062(3) -0.091(3) 0.034(3) O13 0.125(3) 0.055(2) 0.086(3) -0.0300(19) -0.056(2) 0.032(2) O1W 0.069(2) 0.083(3) 0.072(2) -0.0092(19) -0.0063(17) 0.0108(19) _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 O1 2.025(3) . ? Co1 O4 2.040(3) . ? Co1 O3 2.082(3) . ? Co1 O2 2.090(3) . ? Co1 O6 2.173(3) . ? Co1 O5 2.217(3) . ? O5 N8 1.255(4) . ? O6 N8 1.262(4) . ? O1 N2 1.332(4) . ? N2 C3 1.339(5) . ? N2 C7 1.340(5) . ? C3 C4 1.372(6) . ? C4 C5 1.394(6) . ? C5 C6 1.390(6) . ? C5 C12 1.484(5) . ? C6 C7 1.359(5) . ? O7 N8 1.226(5) . ? O8 N9 1.330(4) . ? N9 C14 1.333(5) . ? N9 C10 1.337(5) . ? C10 C11 1.371(6) . ? C11 C12 1.403(6) . ? C12 C13 1.381(6) . ? C13 C14 1.369(6) . ? O1G N2G 1.319(6) . ? N2G C3G 1.348(8) . ? N2G C7G 1.355(6) . ? C3G C4G 1.331(8) . ? C4G C5G 1.385(6) . ? C5G C6G 1.383(6) . ? C5G C12G 1.470(6) . ? C6G C7G 1.367(7) . ? O8G N9G 1.309(6) . ? N9G C14G 1.343(7) . ? N9G C10G 1.344(8) . ? C10G C11G 1.375(9) . ? C11G C12G 1.402(6) . ? C12G C13G 1.376(7) . ? C13G C14G 1.351(7) . ? N11 O12 1.224(5) . ? N11 O13 1.228(5) . ? N11 O14 1.254(5) . ? 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 O1 Co1 O4 105.21(13) . . ? O1 Co1 O3 92.20(12) . . ? O4 Co1 O3 86.01(13) . . ? O1 Co1 O2 88.10(12) . . ? O4 Co1 O2 89.76(13) . . ? O3 Co1 O2 175.69(13) . . ? O1 Co1 O6 95.09(12) . . ? O4 Co1 O6 159.69(12) . . ? O3 Co1 O6 93.98(13) . . ? O2 Co1 O6 90.27(12) . . ? O1 Co1 O5 152.83(12) . . ? O4 Co1 O5 101.49(12) . . ? O3 Co1 O5 94.58(13) . . ? O2 Co1 O5 87.07(12) . . ? O6 Co1 O5 58.23(10) . . ? N8 O5 Co1 91.8(2) . . ? N8 O6 Co1 93.7(2) . . ? N2 O1 Co1 125.2(2) . . ? O1 N2 C3 121.2(3) . . ? O1 N2 C7 118.5(3) . . ? C3 N2 C7 120.2(3) . . ? N2 C3 C4 120.9(4) . . ? C3 C4 C5 120.4(4) . . ? C6 C5 C4 116.4(3) . . ? C6 C5 C12 122.0(3) . . ? C4 C5 C12 121.6(3) . . ? C7 C6 C5 121.3(4) . . ? N2 C7 C6 120.7(4) . . ? O7 N8 O5 123.0(4) . . ? O7 N8 O6 120.8(4) . . ? O5 N8 O6 116.1(3) . . ? O8 N9 C14 120.6(3) . . ? O8 N9 C10 118.9(3) . . ? C14 N9 C10 120.5(3) . . ? N9 C10 C11 121.0(4) . . ? C10 C11 C12 120.4(4) . . ? C13 C12 C11 115.9(4) . . ? C13 C12 C5 122.0(3) . . ? C11 C12 C5 122.0(4) . . ? C14 C13 C12 122.0(4) . . ? N9 C14 C13 120.2(4) . . ? O1G N2G C3G 122.7(5) . . ? O1G N2G C7G 118.4(5) . . ? C3G N2G C7G 118.9(5) . . ? C4G C3G N2G 121.5(5) . . ? C3G C4G C5G 122.1(5) . . ? C6G C5G C4G 115.7(4) . . ? C6G C5G C12G 121.2(4) . . ? C4G C5G C12G 123.1(4) . . ? C7G C6G C5G 121.5(5) . . ? N2G C7G C6G 120.2(5) . . ? O8G N9G C14G 121.1(6) . . ? O8G N9G C10G 120.2(6) . . ? C14G N9G C10G 118.7(5) . . ? N9G C10G C11G 122.1(5) . . ? C10G C11G C12G 119.8(5) . . ? C13G C12G C11G 115.5(5) . . ? C13G C12G C5G 122.7(4) . . ? C11G C12G C5G 121.8(5) . . ? C14G C13G C12G 123.0(5) . . ? N9G C14G C13G 120.8(6) . . ? O12 N11 O13 118.6(4) . . ? O12 N11 O14 121.9(4) . . ? O13 N11 O14 119.1(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.84 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.529 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.094 #===END data_4_LT _database_code_depnum_ccdc_archive 'CCDC 279574' _audit_creation_method SHELXL-97 _chemical_name_systematic '[Co(H2O)3(bpdo)(NO3)] NO3 . bpdo . H2O' _chemical_name_common '(Co(H2O)3(bpdo)(NO3)) NO3 . bpdo . H2O' _chemical_melting_point ? _chemical_formula_moiety '(Co 3(H2 O) (C10 H8 N2 O2) (N O3)), N O3, C10 H8 N2 O2, H2 O' _chemical_formula_sum 'C20 H24 Co N6 O14' _chemical_formula_weight 631.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.129(2) _cell_length_b 12.907(3) _cell_length_c 17.896(4) _cell_angle_alpha 77.49(3) _cell_angle_beta 70.25(3) _cell_angle_gamma 76.28(3) _cell_volume 2532.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour Orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1300 _exptl_absorpt_coefficient_mu 0.762 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8942 _exptl_absorpt_correction_T_max 0.9415 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44753 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.13 _reflns_number_total 11119 _reflns_number_gt 6777 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+1.2634P] 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 11118 _refine_ls_number_parameters 805 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0896 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1085 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 Co1A Co 0.83970(3) 0.81403(3) 0.28475(2) 0.01365(10) Uani 1 1 d . . . O2A O 0.68178(16) 0.92023(15) 0.28578(12) 0.0191(4) Uani 1 1 d . . . H21A H 0.627(3) 0.896(3) 0.281(2) 0.044(11) Uiso 1 1 d . . . H22A H 0.651(3) 0.968(3) 0.326(2) 0.062(12) Uiso 1 1 d . . . O3A O 1.00473(17) 0.71882(16) 0.27757(14) 0.0205(4) Uani 1 1 d . . . H31A H 1.020(4) 0.673(3) 0.316(3) 0.071(14) Uiso 1 1 d . . . H32A H 1.032(3) 0.696(3) 0.240(2) 0.027(10) Uiso 1 1 d . . . O4A O 0.93107(19) 0.92805(17) 0.20848(12) 0.0210(4) Uani 1 1 d . . . H41A H 0.902(3) 0.984(3) 0.184(2) 0.043(11) Uiso 1 1 d . . . H42A H 0.998(4) 0.911(3) 0.176(2) 0.064(13) Uiso 1 1 d . . . O5A O 0.80113(15) 0.73085(13) 0.20226(10) 0.0186(4) Uani 1 1 d . . . O6A O 0.74767(16) 0.67755(14) 0.33023(10) 0.0195(4) Uani 1 1 d . . . N8A N 0.74757(19) 0.66707(16) 0.26107(13) 0.0167(5) Uani 1 1 d . . . O7A O 0.69710(17) 0.60102(14) 0.25239(11) 0.0261(5) Uani 1 1 d . . . O1A O 0.82017(15) 0.84263(14) 0.39585(10) 0.0198(4) Uani 1 1 d . . . N2A N 0.91120(17) 0.84693(16) 0.42081(12) 0.0143(5) Uani 1 1 d . . . C3A C 0.9954(2) 0.9053(2) 0.37429(16) 0.0175(6) Uani 1 1 d . . . H3A H 0.9938 0.9386 0.3217 0.021 Uiso 1 1 calc R . . C4A C 1.0831(2) 0.9168(2) 0.40244(15) 0.0171(6) Uani 1 1 d . . . H4A H 1.1418 0.9581 0.3692 0.021 Uiso 1 1 calc R . . C5A C 1.0871(2) 0.86840(19) 0.47976(15) 0.0130(5) Uani 1 1 d . . . C6A C 1.0004(2) 0.8061(2) 0.52457(15) 0.0173(6) Uani 1 1 d . . . H6A H 1.0012 0.7701 0.5767 0.021 Uiso 1 1 calc R . . C7A C 0.9139(2) 0.7962(2) 0.49442(16) 0.0191(6) Uani 1 1 d . . . H7A H 0.8556 0.7533 0.5257 0.023 Uiso 1 1 calc R . . O8A O 1.42219(15) 0.93650(14) 0.60680(10) 0.0180(4) Uani 1 1 d . . . N9A N 1.34371(17) 0.91805(16) 0.57653(12) 0.0135(5) Uani 1 1 d . . . C10A C 1.3452(2) 0.9634(2) 0.50098(15) 0.0188(6) Uani 1 1 d . . . H10A H 1.4029 1.0070 0.4700 0.023 Uiso 1 1 calc R . . C11A C 1.2641(2) 0.9472(2) 0.46817(16) 0.0169(6) Uani 1 1 d . . . H11A H 1.2669 0.9791 0.4146 0.020 Uiso 1 1 calc R . . C12A C 1.1778(2) 0.88426(19) 0.51285(15) 0.0133(5) Uani 1 1 d . . . C13A C 1.1799(2) 0.8381(2) 0.59081(15) 0.0175(6) Uani 1 1 d . . . H13A H 1.1234 0.7940 0.6230 0.021 Uiso 1 1 calc R . . C14A C 1.2626(2) 0.8558(2) 0.62148(16) 0.0187(6) Uani 1 1 d . . . H14A H 1.2626 0.8241 0.6746 0.022 Uiso 1 1 calc R . . O1B O 0.85297(18) 1.10935(15) 0.12122(14) 0.0356(5) Uani 1 1 d . . . N2B N 0.9303(2) 1.17665(18) 0.09232(15) 0.0264(6) Uani 1 1 d . . . C3B C 0.9439(3) 1.2341(2) 0.01740(18) 0.0273(7) Uani 1 1 d . . . H3B H 0.8988 1.2255 -0.0144 0.033 Uiso 1 1 calc R . . C4B C 1.0225(2) 1.3040(2) -0.01188(17) 0.0239(6) Uani 1 1 d . . . H4B H 1.0312 1.3439 -0.0642 0.029 Uiso 1 1 calc R . . C5B C 1.0902(2) 1.3180(2) 0.03320(16) 0.0185(6) Uani 1 1 d . . . C6B C 1.0765(2) 1.2551(2) 0.10851(16) 0.0208(6) Uani 1 1 d . . . H6B H 1.1233 1.2602 0.1403 0.025 Uiso 1 1 calc R . . C7B C 0.9966(3) 1.1860(2) 0.13733(17) 0.0247(6) Uani 1 1 d . . . H7B H 0.9876 1.1443 0.1891 0.030 Uiso 1 1 calc R . . O8B O 1.40971(19) 1.60666(17) -0.07751(12) 0.0355(5) Uani 1 1 d . . . N9B N 1.3338(2) 1.53766(18) -0.05271(14) 0.0259(6) Uani 1 1 d . . . C10B C 1.2601(3) 1.5378(2) -0.09386(17) 0.0287(7) Uani 1 1 d . . . H10B H 1.2625 1.5872 -0.1419 0.034 Uiso 1 1 calc R . . C11B C 1.1806(2) 1.4673(2) -0.06773(17) 0.0251(6) Uani 1 1 d . . . H11B H 1.1296 1.4686 -0.0983 0.030 Uiso 1 1 calc R . . C12B C 1.1739(2) 1.3942(2) 0.00304(16) 0.0192(6) Uani 1 1 d . . . C13B C 1.2531(2) 1.3971(2) 0.04392(16) 0.0233(6) Uani 1 1 d . . . H13B H 1.2521 1.3493 0.0925 0.028 Uiso 1 1 calc R . . C14B C 1.3318(3) 1.4674(2) 0.01545(17) 0.0265(7) Uani 1 1 d . . . H14B H 1.3855 1.4667 0.0439 0.032 Uiso 1 1 calc R . . O1W O 1.11137(19) 0.62226(16) 0.14653(12) 0.0245(5) Uani 1 1 d . . . H11W H 1.176(4) 0.611(3) 0.150(2) 0.062(14) Uiso 1 1 d . . . H12W H 1.090(5) 0.546(4) 0.159(3) 0.13(2) Uiso 1 1 d . . . N11 N 0.92943(19) 0.38556(17) 0.24860(13) 0.0195(5) Uani 1 1 d . . . O12 O 0.96822(18) 0.46084(16) 0.19725(13) 0.0357(5) Uani 1 1 d . . . O13 O 0.98788(18) 0.33623(16) 0.29605(12) 0.0307(5) Uani 1 1 d . . . O14 O 0.83719(16) 0.35560(15) 0.25199(13) 0.0293(5) Uani 1 1 d . . . Co1C Co 0.33439(3) 1.30817(3) 0.28924(2) 0.01401(10) Uani 1 1 d . . . O2C O 0.17575(17) 1.41596(16) 0.29254(12) 0.0209(4) Uani 1 1 d . . . H21C H 0.150(3) 1.462(3) 0.330(2) 0.051(11) Uiso 1 1 d . . . H22C H 0.125(3) 1.393(2) 0.2851(18) 0.028(9) Uiso 1 1 d . . . O3C O 0.49974(18) 1.21257(17) 0.27848(14) 0.0242(5) Uani 1 1 d . . . H31C H 0.536(4) 1.189(3) 0.231(3) 0.073(14) Uiso 1 1 d . . . H32C H 0.513(2) 1.172(2) 0.3096(17) 0.008(8) Uiso 1 1 d . . . O4C O 0.4238(2) 1.42347(17) 0.21369(13) 0.0212(4) Uani 1 1 d . . . H41C H 0.474(3) 1.404(3) 0.180(2) 0.038(12) Uiso 1 1 d . . . H42C H 0.381(3) 1.486(3) 0.201(2) 0.053(12) Uiso 1 1 d . . . O5C O 0.29337(15) 1.22917(13) 0.20659(10) 0.0184(4) Uani 1 1 d . . . O6C O 0.23659(16) 1.17574(14) 0.33435(10) 0.0202(4) Uani 1 1 d . . . O7C O 0.17717(17) 1.10889(14) 0.25550(11) 0.0252(4) Uani 1 1 d . . . N8C N 0.23412(19) 1.16878(16) 0.26499(13) 0.0176(5) Uani 1 1 d . . . O1C O 0.31823(15) 1.33775(14) 0.39898(10) 0.0199(4) Uani 1 1 d . . . N2C N 0.40902(17) 1.34393(16) 0.42320(12) 0.0146(5) Uani 1 1 d . . . C3C C 0.4949(2) 1.3988(2) 0.37516(16) 0.0185(6) Uani 1 1 d . . . H3C H 0.4949 1.4286 0.3218 0.022 Uiso 1 1 calc R . . C4C C 0.5831(2) 1.4120(2) 0.40276(16) 0.0177(6) Uani 1 1 d . . . H4C H 0.6432 1.4510 0.3682 0.021 Uiso 1 1 calc R . . C5C C 0.5849(2) 1.36892(19) 0.48094(14) 0.0124(5) Uani 1 1 d . . . C6C C 0.4955(2) 1.3101(2) 0.52808(16) 0.0177(6) Uani 1 1 d . . . H6C H 0.4942 1.2783 0.5814 0.021 Uiso 1 1 calc R . . C7C C 0.4094(2) 1.2978(2) 0.49823(15) 0.0180(6) Uani 1 1 d . . . H7C H 0.3501 1.2567 0.5307 0.022 Uiso 1 1 calc R . . O8C O 0.92386(15) 1.43381(14) 0.60601(11) 0.0182(4) Uani 1 1 d . . . N9C N 0.84333(18) 1.41789(16) 0.57623(13) 0.0143(5) Uani 1 1 d . . . C10C C 0.8451(2) 1.4626(2) 0.50042(15) 0.0189(6) Uani 1 1 d . . . H10C H 0.9037 1.5050 0.4690 0.023 Uiso 1 1 calc R . . C11C C 0.7632(2) 1.4476(2) 0.46828(16) 0.0187(6) Uani 1 1 d . . . H11C H 0.7662 1.4792 0.4147 0.022 Uiso 1 1 calc R . . C12C C 0.6750(2) 1.38604(18) 0.51371(15) 0.0135(5) Uani 1 1 d . . . C13C C 0.6767(2) 1.3418(2) 0.59186(15) 0.0172(6) Uani 1 1 d . . . H13C H 0.6186 1.2997 0.6249 0.021 Uiso 1 1 calc R . . C14C C 0.7603(2) 1.3580(2) 0.62180(16) 0.0180(6) Uani 1 1 d . . . H14C H 0.7598 1.3268 0.6751 0.022 Uiso 1 1 calc R . . O1D O 0.32198(17) 1.61706(15) 0.17004(14) 0.0362(6) Uani 1 1 d . . . N2D N 0.4036(2) 1.67817(17) 0.12770(15) 0.0254(6) Uani 1 1 d . . . C3D C 0.3983(3) 1.7373(2) 0.05708(19) 0.0273(7) Uani 1 1 d . . . H3D H 0.3377 1.7331 0.0359 0.033 Uiso 1 1 calc R . . C4D C 0.4789(3) 1.8039(2) 0.01496(18) 0.0261(7) Uani 1 1 d . . . H4D H 0.4740 1.8442 -0.0353 0.031 Uiso 1 1 calc R . . C5D C 0.5681(2) 1.8133(2) 0.04486(16) 0.0179(6) Uani 1 1 d . . . C6D C 0.5731(2) 1.7479(2) 0.11738(16) 0.0191(6) Uani 1 1 d . . . H6D H 0.6341 1.7490 0.1391 0.023 Uiso 1 1 calc R . . C7D C 0.4910(2) 1.6820(2) 0.15757(18) 0.0233(6) Uani 1 1 d . . . H7D H 0.4956 1.6386 0.2070 0.028 Uiso 1 1 calc R . . O8D O 0.86267(18) 2.11810(15) -0.09984(13) 0.0358(5) Uani 1 1 d . . . N9D N 0.7988(2) 2.04039(18) -0.06861(14) 0.0277(6) Uani 1 1 d . . . C10D C 0.7337(3) 2.0163(2) -0.10869(18) 0.0282(7) Uani 1 1 d . . . H10D H 0.7389 2.0515 -0.1619 0.034 Uiso 1 1 calc R . . C11D C 0.6605(2) 1.9422(2) -0.07375(16) 0.0229(6) Uani 1 1 d . . . H11D H 0.6152 1.9265 -0.1027 0.027 Uiso 1 1 calc R . . C12D C 0.6518(2) 1.8893(2) 0.00449(15) 0.0181(6) Uani 1 1 d . . . C13D C 0.7225(3) 1.9130(2) 0.04273(17) 0.0248(6) Uani 1 1 d . . . H13D H 0.7205 1.8771 0.0953 0.030 Uiso 1 1 calc R . . C14D C 0.7954(3) 1.9873(2) 0.00596(17) 0.0276(7) Uani 1 1 d . . . H14D H 0.8440 2.0018 0.0330 0.033 Uiso 1 1 calc R . . N21 N 0.42930(19) 0.88526(17) 0.25960(14) 0.0206(5) Uani 1 1 d . . . O22 O 0.4550(2) 0.97021(17) 0.21717(17) 0.0567(8) Uani 1 1 d . . . O23 O 0.50353(16) 0.82454(14) 0.29277(11) 0.0237(4) Uani 1 1 d . . . O24 O 0.33434(16) 0.85633(16) 0.26845(12) 0.0298(5) Uani 1 1 d . . . O2WA O 0.6082(3) 1.1242(5) 0.1479(3) 0.0245(16) Uani 0.642(13) 1 d P A 1 O2WB O 0.6313(5) 1.1852(8) 0.1245(4) 0.018(2) Uani 0.358(13) 1 d P A 2 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 Co1A 0.01274(19) 0.0163(2) 0.0130(2) -0.00132(14) -0.00561(15) -0.00279(14) O2A 0.0143(10) 0.0210(11) 0.0254(12) -0.0067(8) -0.0104(9) 0.0001(8) O3A 0.0188(11) 0.0234(12) 0.0170(12) -0.0032(10) -0.0059(9) 0.0012(8) O4A 0.0169(11) 0.0215(11) 0.0207(11) 0.0036(9) -0.0035(9) -0.0055(9) O5A 0.0233(10) 0.0187(10) 0.0144(10) 0.0011(7) -0.0058(8) -0.0078(8) O6A 0.0255(10) 0.0235(10) 0.0112(10) 0.0000(7) -0.0067(8) -0.0085(8) N8A 0.0192(12) 0.0151(11) 0.0149(12) 0.0001(9) -0.0065(10) -0.0017(9) O7A 0.0348(12) 0.0201(10) 0.0294(12) -0.0024(8) -0.0120(9) -0.0138(9) O1A 0.0121(9) 0.0337(11) 0.0190(10) -0.0077(8) -0.0080(8) -0.0055(8) N2A 0.0102(11) 0.0206(12) 0.0144(12) -0.0066(9) -0.0048(9) -0.0017(9) C3A 0.0179(14) 0.0182(14) 0.0162(14) 0.0021(10) -0.0060(11) -0.0060(11) C4A 0.0172(14) 0.0209(14) 0.0149(14) -0.0011(11) -0.0050(11) -0.0074(11) C5A 0.0118(13) 0.0122(13) 0.0154(14) -0.0021(10) -0.0055(11) -0.0007(10) C6A 0.0170(14) 0.0228(14) 0.0123(14) 0.0008(10) -0.0050(11) -0.0063(11) C7A 0.0156(14) 0.0278(15) 0.0161(14) -0.0017(11) -0.0044(11) -0.0101(11) O8A 0.0164(9) 0.0220(10) 0.0215(10) -0.0029(8) -0.0113(8) -0.0066(7) N9A 0.0112(11) 0.0150(11) 0.0172(12) -0.0043(9) -0.0075(9) -0.0016(8) C10A 0.0180(14) 0.0212(15) 0.0181(15) 0.0019(11) -0.0069(12) -0.0075(11) C11A 0.0169(14) 0.0187(14) 0.0168(14) 0.0018(11) -0.0080(11) -0.0057(11) C12A 0.0117(13) 0.0141(13) 0.0144(14) -0.0024(10) -0.0050(11) -0.0011(10) C13A 0.0191(14) 0.0179(14) 0.0186(15) -0.0002(11) -0.0079(12) -0.0082(11) C14A 0.0205(14) 0.0190(14) 0.0170(14) 0.0012(11) -0.0073(12) -0.0056(11) O1B 0.0322(12) 0.0228(11) 0.0557(15) 0.0076(10) -0.0223(11) -0.0110(9) N2B 0.0265(13) 0.0189(13) 0.0385(16) 0.0006(11) -0.0164(12) -0.0074(10) C3B 0.0314(17) 0.0238(16) 0.0331(18) 0.0005(13) -0.0216(14) -0.0037(13) C4B 0.0302(16) 0.0200(15) 0.0260(16) -0.0009(12) -0.0180(13) -0.0011(12) C5B 0.0196(14) 0.0166(14) 0.0192(15) -0.0046(11) -0.0091(12) 0.0038(11) C6B 0.0239(15) 0.0208(15) 0.0210(15) -0.0038(11) -0.0111(12) -0.0031(12) C7B 0.0304(16) 0.0200(15) 0.0251(16) -0.0013(12) -0.0124(13) -0.0032(12) O8B 0.0374(13) 0.0401(13) 0.0273(12) -0.0050(9) 0.0034(10) -0.0231(10) N9B 0.0268(13) 0.0257(13) 0.0217(13) -0.0066(10) 0.0007(11) -0.0069(10) C10B 0.0296(17) 0.0243(16) 0.0202(16) 0.0049(12) -0.0019(13) 0.0016(13) C11B 0.0220(15) 0.0279(16) 0.0210(16) 0.0007(12) -0.0084(12) 0.0028(12) C12B 0.0194(14) 0.0168(14) 0.0178(15) -0.0050(11) -0.0035(12) 0.0029(11) C13B 0.0261(16) 0.0275(16) 0.0160(15) -0.0024(11) -0.0041(12) -0.0082(12) C14B 0.0293(17) 0.0338(17) 0.0178(15) -0.0083(12) -0.0040(13) -0.0090(13) O1W 0.0231(12) 0.0265(12) 0.0263(12) -0.0015(9) -0.0119(10) -0.0048(9) N11 0.0181(12) 0.0169(12) 0.0243(13) -0.0031(10) -0.0071(10) -0.0037(9) O12 0.0346(12) 0.0308(12) 0.0478(14) 0.0185(10) -0.0261(11) -0.0191(10) O13 0.0340(12) 0.0397(12) 0.0268(12) 0.0129(9) -0.0214(10) -0.0207(10) O14 0.0173(10) 0.0302(12) 0.0444(13) 0.0022(9) -0.0147(10) -0.0105(9) Co1C 0.01421(19) 0.0161(2) 0.01280(19) -0.00149(14) -0.00603(15) -0.00245(14) O2C 0.0155(10) 0.0215(11) 0.0312(12) -0.0087(9) -0.0131(9) -0.0008(8) O3C 0.0217(11) 0.0254(12) 0.0187(12) 0.0012(10) -0.0072(10) 0.0061(9) O4C 0.0198(11) 0.0209(12) 0.0199(12) 0.0009(9) -0.0046(10) -0.0036(9) O5C 0.0250(10) 0.0176(10) 0.0118(9) 0.0028(7) -0.0042(8) -0.0091(8) O6C 0.0284(11) 0.0214(10) 0.0123(10) 0.0002(7) -0.0073(8) -0.0076(8) O7C 0.0366(12) 0.0217(10) 0.0245(11) -0.0024(8) -0.0117(9) -0.0160(9) N8C 0.0228(12) 0.0127(11) 0.0170(13) -0.0015(9) -0.0064(10) -0.0029(9) O1C 0.0116(9) 0.0361(11) 0.0169(10) -0.0076(8) -0.0069(8) -0.0064(8) N2C 0.0115(11) 0.0209(12) 0.0148(12) -0.0060(9) -0.0055(9) -0.0040(9) C3C 0.0201(14) 0.0227(15) 0.0151(14) -0.0006(11) -0.0080(12) -0.0065(11) C4C 0.0158(14) 0.0204(14) 0.0188(15) -0.0003(11) -0.0067(11) -0.0071(11) C5C 0.0110(12) 0.0140(13) 0.0126(13) -0.0044(10) -0.0036(10) -0.0006(10) C6C 0.0161(14) 0.0251(15) 0.0138(14) 0.0001(11) -0.0070(11) -0.0061(11) C7C 0.0147(13) 0.0272(15) 0.0127(14) -0.0016(11) -0.0022(11) -0.0088(11) O8C 0.0138(9) 0.0239(10) 0.0230(10) -0.0041(8) -0.0116(8) -0.0054(7) N9C 0.0124(11) 0.0140(11) 0.0195(12) -0.0031(9) -0.0079(9) -0.0029(9) C10C 0.0164(14) 0.0249(15) 0.0182(15) 0.0015(11) -0.0070(12) -0.0106(11) C11C 0.0166(14) 0.0244(15) 0.0150(14) -0.0005(11) -0.0051(11) -0.0052(11) C12C 0.0144(13) 0.0097(13) 0.0162(14) -0.0038(10) -0.0045(11) -0.0004(10) C13C 0.0164(14) 0.0204(14) 0.0154(14) 0.0034(11) -0.0065(11) -0.0078(11) C14C 0.0212(14) 0.0173(14) 0.0172(14) 0.0013(11) -0.0095(12) -0.0050(11) O1D 0.0236(11) 0.0208(11) 0.0671(16) 0.0046(10) -0.0199(11) -0.0105(9) N2D 0.0189(12) 0.0139(12) 0.0462(16) -0.0014(11) -0.0153(12) -0.0029(9) C3D 0.0273(16) 0.0194(15) 0.045(2) -0.0033(13) -0.0256(15) -0.0023(12) C4D 0.0328(17) 0.0181(15) 0.0348(18) -0.0017(12) -0.0237(14) -0.0005(12) C5D 0.0209(14) 0.0141(14) 0.0198(15) -0.0072(11) -0.0082(12) 0.0021(11) C6D 0.0190(14) 0.0203(15) 0.0215(15) -0.0050(11) -0.0087(12) -0.0041(11) C7D 0.0195(15) 0.0208(15) 0.0312(17) -0.0017(12) -0.0109(13) -0.0038(11) O8D 0.0335(12) 0.0240(11) 0.0388(13) -0.0047(9) 0.0091(10) -0.0138(9) N9D 0.0297(14) 0.0158(12) 0.0245(14) -0.0041(10) 0.0093(11) -0.0040(10) C10D 0.0310(17) 0.0252(16) 0.0207(16) -0.0041(12) -0.0033(13) 0.0035(13) C11D 0.0245(15) 0.0224(15) 0.0178(15) -0.0033(11) -0.0051(12) 0.0016(12) C12D 0.0208(14) 0.0136(13) 0.0176(14) -0.0060(11) -0.0050(12) 0.0032(11) C13D 0.0323(17) 0.0250(16) 0.0196(15) -0.0002(12) -0.0088(13) -0.0113(13) C14D 0.0316(17) 0.0285(17) 0.0249(17) -0.0046(13) -0.0062(13) -0.0119(13) N21 0.0164(12) 0.0203(13) 0.0257(13) 0.0000(10) -0.0086(10) -0.0041(10) O22 0.0523(16) 0.0325(13) 0.099(2) 0.0363(13) -0.0560(15) -0.0264(12) O23 0.0216(10) 0.0268(11) 0.0254(11) 0.0066(8) -0.0145(9) -0.0079(8) O24 0.0149(10) 0.0360(12) 0.0388(13) 0.0068(9) -0.0119(9) -0.0108(9) O2WA 0.0242(19) 0.031(4) 0.016(2) -0.005(2) -0.0055(16) -0.0009(18) O2WB 0.020(3) 0.020(5) 0.013(3) 0.003(3) -0.002(2) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1A O1A 2.0258(18) . ? Co1A O4A 2.034(2) . ? Co1A O3A 2.064(2) . ? Co1A O2A 2.0709(19) . ? Co1A O6A 2.1701(19) . ? Co1A O5A 2.2232(18) . ? O5A N8A 1.274(3) . ? O6A N8A 1.274(3) . ? N8A O7A 1.223(3) . ? O1A N2A 1.340(2) . ? N2A C7A 1.346(3) . ? N2A C3A 1.350(3) . ? C3A C4A 1.369(3) . ? C4A C5A 1.401(3) . ? C5A C6A 1.395(3) . ? C5A C12A 1.485(3) . ? C6A C7A 1.373(4) . ? O8A N9A 1.330(2) . ? N9A C10A 1.348(3) . ? N9A C14A 1.349(3) . ? C10A C11A 1.378(3) . ? C11A C12A 1.397(3) . ? C12A C13A 1.400(3) . ? C13A C14A 1.376(3) . ? O1B N2B 1.329(3) . ? N2B C7B 1.355(3) . ? N2B C3B 1.361(4) . ? C3B C4B 1.365(4) . ? C4B C5B 1.393(4) . ? C5B C6B 1.394(4) . ? C5B C12B 1.471(4) . ? C6B C7B 1.369(4) . ? O8B N9B 1.334(3) . ? N9B C10B 1.336(4) . ? N9B C14B 1.350(4) . ? C10B C11B 1.379(4) . ? C11B C12B 1.397(4) . ? C12B C13B 1.401(4) . ? C13B C14B 1.370(4) . ? N11 O12 1.244(3) . ? N11 O14 1.247(3) . ? N11 O13 1.260(3) . ? Co1C O1C 2.0175(18) . ? Co1C O4C 2.031(2) . ? Co1C O3C 2.061(2) . ? Co1C O2C 2.081(2) . ? Co1C O6C 2.1674(19) . ? Co1C O5C 2.2061(18) . ? O5C N8C 1.273(3) . ? O6C N8C 1.275(3) . ? O7C N8C 1.221(3) . ? O1C N2C 1.336(2) . ? N2C C3C 1.344(3) . ? N2C C7C 1.347(3) . ? C3C C4C 1.377(3) . ? C4C C5C 1.395(3) . ? C5C C6C 1.400(4) . ? C5C C12C 1.480(3) . ? C6C C7C 1.375(3) . ? O8C N9C 1.332(3) . ? N9C C14C 1.349(3) . ? N9C C10C 1.350(3) . ? C10C C11C 1.371(3) . ? C11C C12C 1.405(4) . ? C12C C13C 1.396(3) . ? C13C C14C 1.369(3) . ? O1D N2D 1.334(3) . ? N2D C3D 1.341(4) . ? N2D C7D 1.353(3) . ? C3D C4D 1.372(4) . ? C4D C5D 1.398(4) . ? C5D C6D 1.398(4) . ? C5D C12D 1.478(4) . ? C6D C7D 1.373(4) . ? O8D N9D 1.323(3) . ? N9D C10D 1.353(4) . ? N9D C14D 1.353(4) . ? C10D C11D 1.365(4) . ? C11D C12D 1.399(4) . ? C12D C13D 1.381(4) . ? C13D C14D 1.368(4) . ? N21 O22 1.232(3) . ? N21 O24 1.243(3) . ? N21 O23 1.266(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A Co1A O4A 104.63(8) . . ? O1A Co1A O3A 91.69(9) . . ? O4A Co1A O3A 85.74(9) . . ? O1A Co1A O2A 89.25(8) . . ? O4A Co1A O2A 89.29(9) . . ? O3A Co1A O2A 175.02(8) . . ? O1A Co1A O6A 93.58(7) . . ? O4A Co1A O6A 161.78(8) . . ? O3A Co1A O6A 93.24(8) . . ? O2A Co1A O6A 91.57(8) . . ? O1A Co1A O5A 152.04(7) . . ? O4A Co1A O5A 103.02(7) . . ? O3A Co1A O5A 94.45(8) . . ? O2A Co1A O5A 86.98(8) . . ? O6A Co1A O5A 58.88(7) . . ? N8A O5A Co1A 91.35(13) . . ? N8A O6A Co1A 93.80(14) . . ? O7A N8A O5A 122.5(2) . . ? O7A N8A O6A 121.6(2) . . ? O5A N8A O6A 115.9(2) . . ? N2A O1A Co1A 123.71(14) . . ? O1A N2A C7A 118.7(2) . . ? O1A N2A C3A 120.4(2) . . ? C7A N2A C3A 120.9(2) . . ? N2A C3A C4A 120.4(2) . . ? C3A C4A C5A 120.8(2) . . ? C6A C5A C4A 116.7(2) . . ? C6A C5A C12A 121.7(2) . . ? C4A C5A C12A 121.6(2) . . ? C7A C6A C5A 120.9(2) . . ? N2A C7A C6A 120.3(2) . . ? O8A N9A C10A 119.2(2) . . ? O8A N9A C14A 120.2(2) . . ? C10A N9A C14A 120.6(2) . . ? N9A C10A C11A 120.7(2) . . ? C10A C11A C12A 120.6(2) . . ? C11A C12A C13A 116.8(2) . . ? C11A C12A C5A 121.7(2) . . ? C13A C12A C5A 121.5(2) . . ? C14A C13A C12A 120.9(2) . . ? N9A C14A C13A 120.4(2) . . ? O1B N2B C7B 119.5(2) . . ? O1B N2B C3B 119.9(2) . . ? C7B N2B C3B 120.5(2) . . ? N2B C3B C4B 119.9(3) . . ? C3B C4B C5B 121.4(3) . . ? C4B C5B C6B 116.9(3) . . ? C4B C5B C12B 122.2(2) . . ? C6B C5B C12B 120.9(2) . . ? C7B C6B C5B 120.9(3) . . ? N2B C7B C6B 120.3(3) . . ? O8B N9B C10B 121.1(2) . . ? O8B N9B C14B 118.9(2) . . ? C10B N9B C14B 120.0(2) . . ? N9B C10B C11B 121.1(3) . . ? C10B C11B C12B 121.0(3) . . ? C11B C12B C13B 115.7(3) . . ? C11B C12B C5B 122.7(3) . . ? C13B C12B C5B 121.5(2) . . ? C14B C13B C12B 121.5(3) . . ? N9B C14B C13B 120.6(3) . . ? O12 N11 O14 121.6(2) . . ? O12 N11 O13 118.7(2) . . ? O14 N11 O13 119.7(2) . . ? O1C Co1C O4C 103.27(8) . . ? O1C Co1C O3C 92.76(9) . . ? O4C Co1C O3C 85.85(10) . . ? O1C Co1C O2C 88.62(8) . . ? O4C Co1C O2C 88.72(9) . . ? O3C Co1C O2C 174.57(9) . . ? O1C Co1C O6C 94.77(7) . . ? O4C Co1C O6C 161.86(8) . . ? O3C Co1C O6C 95.28(8) . . ? O2C Co1C O6C 89.83(8) . . ? O1C Co1C O5C 153.49(7) . . ? O4C Co1C O5C 102.75(8) . . ? O3C Co1C O5C 94.12(8) . . ? O2C Co1C O5C 86.93(8) . . ? O6C Co1C O5C 59.12(7) . . ? N8C O5C Co1C 91.55(13) . . ? N8C O6C Co1C 93.28(14) . . ? O7C N8C O5C 122.4(2) . . ? O7C N8C O6C 121.9(2) . . ? O5C N8C O6C 115.7(2) . . ? N2C O1C Co1C 124.67(14) . . ? O1C N2C C3C 120.8(2) . . ? O1C N2C C7C 118.3(2) . . ? C3C N2C C7C 120.8(2) . . ? N2C C3C C4C 120.5(2) . . ? C3C C4C C5C 120.7(2) . . ? C4C C5C C6C 116.8(2) . . ? C4C C5C C12C 122.1(2) . . ? C6C C5C C12C 121.1(2) . . ? C7C C6C C5C 120.9(2) . . ? N2C C7C C6C 120.2(2) . . ? O8C N9C C14C 120.1(2) . . ? O8C N9C C10C 119.6(2) . . ? C14C N9C C10C 120.3(2) . . ? N9C C10C C11C 120.8(2) . . ? C10C C11C C12C 120.8(2) . . ? C13C C12C C11C 116.3(2) . . ? C13C C12C C5C 121.6(2) . . ? C11C C12C C5C 122.1(2) . . ? C14C C13C C12C 121.3(2) . . ? N9C C14C C13C 120.5(2) . . ? O1D N2D C3D 120.8(2) . . ? O1D N2D C7D 119.3(2) . . ? C3D N2D C7D 119.9(2) . . ? N2D C3D C4D 121.0(3) . . ? C3D C4D C5D 121.0(3) . . ? C4D C5D C6D 116.2(3) . . ? C4D C5D C12D 123.0(2) . . ? C6D C5D C12D 120.7(2) . . ? C7D C6D C5D 120.9(3) . . ? N2D C7D C6D 120.8(3) . . ? O8D N9D C10D 121.1(2) . . ? O8D N9D C14D 119.1(3) . . ? C10D N9D C14D 119.8(2) . . ? N9D C10D C11D 120.9(3) . . ? C10D C11D C12D 120.4(3) . . ? C13D C12D C11D 117.3(3) . . ? C13D C12D C5D 121.7(2) . . ? C11D C12D C5D 121.1(3) . . ? C14D C13D C12D 121.0(3) . . ? N9D C14D C13D 120.6(3) . . ? O22 N21 O24 121.7(2) . . ? O22 N21 O23 118.8(2) . . ? O24 N21 O23 119.4(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.13 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.765 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.072 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 279575' _audit_creation_method SHELXL-97 _chemical_name_systematic '[Co(H2O)5(bpdo)]SO4 . 2H2O' _chemical_name_common '(Co(H2O)5(bpdo))SO4 . 2H2O' _chemical_melting_point ? _chemical_formula_moiety '(Co 5(H2 O) C10 H8 N2 O2), S O4, 2(H2 O)' _chemical_formula_sum 'C10 H22 Co N2 O13 S' _chemical_formula_weight 469.29 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' S S 0.1246 0.1234 '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 'P 21/n' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.122(1) _cell_length_b 25.319(5) _cell_length_c 10.241(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.14(3) _cell_angle_gamma 90.00 _cell_volume 1843.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour Orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 1.113 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8420 _exptl_absorpt_correction_T_max 0.8780 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33963 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 26.71 _reflns_number_total 3883 _reflns_number_gt 3257 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+3.0887P] 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 SHELXL _refine_ls_extinction_coef 0.0017(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3883 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0932 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _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 0.17557(5) 0.146633(13) 0.97363(3) 0.01214(12) Uani 1 1 d . . . O2 O -0.0410(3) 0.17638(8) 0.8517(2) 0.0179(4) Uani 1 1 d . . . H2A H -0.021(6) 0.1919(17) 0.789(4) 0.045(13) Uiso 1 1 d . . . H2B H -0.131(6) 0.1898(15) 0.884(4) 0.034(11) Uiso 1 1 d . . . O3 O 0.3814(3) 0.17077(8) 0.8488(2) 0.0149(4) Uani 1 1 d . . . H3A H 0.361(5) 0.1865(15) 0.789(4) 0.029(11) Uiso 1 1 d . . . H3B H 0.481(6) 0.1851(15) 0.889(4) 0.041(11) Uiso 1 1 d . . . O4 O 0.3954(3) 0.11756(8) 1.0901(2) 0.0181(4) Uani 1 1 d . . . H4A H 0.485(6) 0.1048(17) 1.055(4) 0.051(13) Uiso 1 1 d . . . H4B H 0.429(6) 0.1286(17) 1.157(4) 0.046(13) Uiso 1 1 d . . . O5 O -0.0162(3) 0.11582(8) 1.0994(2) 0.0159(4) Uani 1 1 d . . . H5A H 0.286(6) 0.2351(16) 1.092(4) 0.044(12) Uiso 1 1 d . . . H5B H 0.102(5) 0.2350(14) 1.089(3) 0.022(9) Uiso 1 1 d . . . O6 O 0.1893(3) 0.21639(8) 1.0836(2) 0.0223(5) Uani 1 1 d . . . H6A H -0.060(6) 0.1366(17) 1.154(4) 0.044(12) Uiso 1 1 d . . . H6B H -0.106(5) 0.1039(14) 1.066(3) 0.026(10) Uiso 1 1 d . . . O1 O 0.1522(3) 0.07075(7) 0.88793(17) 0.0170(4) Uani 1 1 d . . . N2 N 0.1866(3) 0.05397(9) 0.7692(2) 0.0136(5) Uani 1 1 d . . . C3 C 0.1549(4) 0.08506(10) 0.6631(3) 0.0154(5) Uani 1 1 d . . . H3 H 0.1143 0.1205 0.6735 0.019 Uiso 1 1 calc R . . C4 C 0.1811(4) 0.06559(10) 0.5400(3) 0.0143(5) Uani 1 1 d . . . H4 H 0.1600 0.0881 0.4664 0.017 Uiso 1 1 calc R . . C5 C 0.2381(4) 0.01357(10) 0.5206(2) 0.0132(5) Uani 1 1 d . . . C6 C 0.2741(4) -0.01675(10) 0.6335(3) 0.0151(5) Uani 1 1 d . . . H6 H 0.3170 -0.0521 0.6258 0.018 Uiso 1 1 calc R . . C7 C 0.2486(4) 0.00380(10) 0.7553(3) 0.0159(5) Uani 1 1 d . . . H7 H 0.2746 -0.0174 0.8307 0.019 Uiso 1 1 calc R . . O8 O 0.3153(3) -0.06689(7) 0.01839(17) 0.0163(4) Uani 1 1 d . . . N9 N 0.2978(3) -0.04808(9) 0.1383(2) 0.0137(5) Uani 1 1 d . . . C10 C 0.2358(4) 0.00171(11) 0.1532(3) 0.0164(6) Uani 1 1 d . . . H10 H 0.2052 0.0228 0.0784 0.020 Uiso 1 1 calc R . . C11 C 0.2168(4) 0.02207(10) 0.2760(3) 0.0163(6) Uani 1 1 d . . . H11 H 0.1733 0.0573 0.2851 0.020 Uiso 1 1 calc R . . C12 C 0.2601(4) -0.00804(10) 0.3879(2) 0.0127(5) Uani 1 1 d . . . C13 C 0.3225(4) -0.05960(10) 0.3676(3) 0.0155(5) Uani 1 1 d . . . H13 H 0.3529 -0.0817 0.4407 0.019 Uiso 1 1 calc R . . C14 C 0.3405(4) -0.07872(10) 0.2433(3) 0.0158(5) Uani 1 1 d . . . H14 H 0.3834 -0.1138 0.2313 0.019 Uiso 1 1 calc R . . S1 S 0.18094(9) 0.23107(3) 0.54421(6) 0.01320(16) Uani 1 1 d . . . O1S O 0.3542(3) 0.23031(7) 0.63177(18) 0.0179(4) Uani 1 1 d . . . O2S O 0.0160(3) 0.22601(8) 0.62325(19) 0.0212(4) Uani 1 1 d . . . O3S O 0.1724(3) 0.28190(8) 0.47404(19) 0.0187(4) Uani 1 1 d . . . O4S O 0.1871(3) 0.18699(8) 0.4516(2) 0.0234(5) Uani 1 1 d . . . O1W O 0.5056(3) 0.13853(8) 0.3484(2) 0.0213(4) Uani 1 1 d . . . H11W H 0.428(6) 0.1566(15) 0.382(4) 0.031(10) Uiso 1 1 d . . . H12W H 0.604(7) 0.1572(18) 0.338(4) 0.057(14) Uiso 1 1 d . . . O2W O 0.8582(3) 0.17900(9) 0.2950(2) 0.0205(4) Uani 1 1 d . . . H21W H 0.851(6) 0.2064(19) 0.252(4) 0.056(14) Uiso 1 1 d . . . H22W H 0.958(6) 0.1824(16) 0.341(4) 0.049(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01314(19) 0.01238(19) 0.01089(19) -0.00099(13) 0.00079(13) 0.00029(14) O2 0.0181(11) 0.0207(10) 0.0152(10) 0.0024(9) 0.0032(8) 0.0055(8) O3 0.0160(10) 0.0170(10) 0.0118(10) 0.0020(8) 0.0003(8) -0.0008(8) O4 0.0174(11) 0.0230(11) 0.0138(10) -0.0037(9) 0.0000(9) 0.0043(9) O5 0.0161(10) 0.0175(10) 0.0141(10) -0.0023(8) 0.0022(8) -0.0023(8) O6 0.0154(11) 0.0185(10) 0.0331(12) -0.0089(9) 0.0034(9) -0.0004(9) O1 0.0261(11) 0.0162(9) 0.0090(9) -0.0033(7) 0.0036(8) -0.0012(8) N2 0.0140(11) 0.0163(11) 0.0105(10) -0.0030(9) 0.0010(8) -0.0020(9) C3 0.0185(14) 0.0126(12) 0.0152(13) -0.0001(10) 0.0004(11) 0.0010(10) C4 0.0173(13) 0.0141(12) 0.0114(13) -0.0003(10) -0.0009(10) -0.0004(10) C5 0.0114(12) 0.0157(13) 0.0124(13) 0.0000(10) 0.0000(10) -0.0022(10) C6 0.0178(14) 0.0143(13) 0.0133(13) -0.0013(10) 0.0014(10) 0.0000(10) C7 0.0210(14) 0.0138(12) 0.0128(13) 0.0018(10) 0.0002(11) -0.0005(11) O8 0.0195(10) 0.0210(10) 0.0087(9) -0.0056(7) 0.0022(7) 0.0015(8) N9 0.0132(11) 0.0174(11) 0.0107(10) -0.0035(9) 0.0011(8) -0.0008(9) C10 0.0201(14) 0.0157(13) 0.0134(13) 0.0004(10) 0.0005(11) 0.0022(11) C11 0.0183(14) 0.0140(13) 0.0166(13) -0.0017(10) 0.0004(11) 0.0018(10) C12 0.0129(13) 0.0128(12) 0.0126(13) -0.0013(10) 0.0019(10) -0.0018(10) C13 0.0182(14) 0.0147(13) 0.0136(13) 0.0015(10) 0.0010(10) 0.0004(11) C14 0.0173(13) 0.0135(12) 0.0167(14) -0.0004(10) 0.0013(11) 0.0025(10) S1 0.0117(3) 0.0151(3) 0.0128(3) 0.0023(2) 0.0003(2) -0.0001(2) O1S 0.0135(9) 0.0224(10) 0.0173(10) 0.0053(8) -0.0038(8) -0.0020(8) O2S 0.0145(10) 0.0291(11) 0.0206(10) 0.0095(8) 0.0055(8) 0.0021(8) O3S 0.0151(10) 0.0196(10) 0.0215(10) 0.0087(8) 0.0013(8) 0.0012(8) O4S 0.0226(11) 0.0216(10) 0.0255(11) -0.0074(8) -0.0024(9) 0.0029(8) O1W 0.0205(11) 0.0227(11) 0.0210(11) -0.0040(9) 0.0034(9) 0.0008(9) O2W 0.0205(11) 0.0225(11) 0.0182(11) -0.0028(9) -0.0015(9) -0.0006(9) _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 O4 2.052(2) . ? Co1 O2 2.072(2) . ? Co1 O5 2.080(2) . ? Co1 O3 2.088(2) . ? Co1 O6 2.094(2) . ? Co1 O1 2.1151(19) . ? O1 N2 1.324(3) . ? N2 C3 1.351(3) . ? N2 C7 1.355(3) . ? C3 C4 1.376(4) . ? C4 C5 1.396(4) . ? C5 C6 1.400(4) . ? C5 C12 1.481(4) . ? C6 C7 1.372(4) . ? O8 N9 1.329(3) . ? N9 C10 1.347(3) . ? N9 C14 1.347(3) . ? C10 C11 1.373(4) . ? C11 C12 1.397(4) . ? C12 C13 1.398(4) . ? C13 C14 1.374(4) . ? S1 O4S 1.467(2) . ? S1 O2S 1.468(2) . ? S1 O3S 1.4737(19) . ? S1 O1S 1.4852(19) . ? 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 O4 Co1 O2 178.31(9) . . ? O4 Co1 O5 90.66(8) . . ? O2 Co1 O5 90.98(9) . . ? O4 Co1 O3 85.51(9) . . ? O2 Co1 O3 92.82(9) . . ? O5 Co1 O3 174.60(8) . . ? O4 Co1 O6 88.75(9) . . ? O2 Co1 O6 91.65(9) . . ? O5 Co1 O6 89.78(9) . . ? O3 Co1 O6 93.94(9) . . ? O4 Co1 O1 87.45(8) . . ? O2 Co1 O1 92.36(8) . . ? O5 Co1 O1 82.92(8) . . ? O3 Co1 O1 93.09(7) . . ? O6 Co1 O1 171.73(8) . . ? N2 O1 Co1 131.17(15) . . ? O1 N2 C3 121.4(2) . . ? O1 N2 C7 118.4(2) . . ? C3 N2 C7 120.2(2) . . ? N2 C3 C4 120.2(2) . . ? C3 C4 C5 121.6(2) . . ? C4 C5 C6 116.2(2) . . ? C4 C5 C12 121.7(2) . . ? C6 C5 C12 122.1(2) . . ? C7 C6 C5 121.0(2) . . ? N2 C7 C6 120.7(2) . . ? O8 N9 C10 119.2(2) . . ? O8 N9 C14 120.2(2) . . ? C10 N9 C14 120.6(2) . . ? N9 C10 C11 120.3(2) . . ? C10 C11 C12 121.2(2) . . ? C11 C12 C13 116.4(2) . . ? C11 C12 C5 121.4(2) . . ? C13 C12 C5 122.1(2) . . ? C14 C13 C12 120.9(2) . . ? N9 C14 C13 120.5(2) . . ? O4S S1 O2S 110.07(12) . . ? O4S S1 O3S 110.57(12) . . ? O2S S1 O3S 109.40(11) . . ? O4S S1 O1S 109.10(12) . . ? O2S S1 O1S 109.23(11) . . ? O3S S1 O1S 108.44(11) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.71 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.848 _refine_diff_density_min -0.477 _refine_diff_density_rms 0.083