#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/46/2014603.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2014603 loop_ _publ_author_name 'Yu-Mei Dai' 'En Tang' 'Zhao-Ji Li' 'Yuan-Gen Yao' _publ_section_title Poly[[diaquacobalt(II)]-\m-4,4'-bipyridine-\k^2^N:N'-\m-p-phenylenebis(oxyacetato)-\k^2^O:O'] _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m61 _journal_page_last m63 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '[Co (C10 H8 O6) (C10 H8 N2) (H2 O)2]' _chemical_formula_moiety 'C20 H20 Co N2 O8' _chemical_formula_sum 'C20 H20 Co N2 O8' _chemical_formula_weight 475.31 _chemical_name_systematic ; Poly[[diaquacobalt(II)]-\m-4,4'-bipyridine-\k^2^N:N'-\m-p- phenylenebis(oxyacetato)-\k^2^O:O'] ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 106.100(10) _cell_angle_beta 96.910(10) _cell_angle_gamma 97.400(10) _cell_formula_units_Z 1 _cell_length_a 5.7600(10) _cell_length_b 8.1770(10) _cell_length_c 10.639(2) _cell_measurement_reflns_used 1535 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.06 _cell_measurement_theta_min 2.02 _cell_volume 470.98(14) _computing_cell_refinement 'SMART and SAINT (Siemens, 1994)' _computing_data_collection 'SMART (Siemens, 1996)' _computing_data_reduction 'SANT and? XPREP in SHELXTL (Siemens, 1994)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution SHELXTL _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type 'Siemens SMART CCD area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 2498 _diffrn_reflns_theta_full 25.06 _diffrn_reflns_theta_max 25.06 _diffrn_reflns_theta_min 2.02 _diffrn_standards_decay_% none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_number none _exptl_absorpt_coefficient_mu 0.966 _exptl_absorpt_correction_T_max 0.748 _exptl_absorpt_correction_T_min 0.650 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 245 _exptl_crystal_size_max .60 _exptl_crystal_size_mid .38 _exptl_crystal_size_min .30 _refine_diff_density_max 0.612 _refine_diff_density_min -0.825 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 156 _refine_ls_number_reflns 1664 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.110 _refine_ls_R_factor_gt 0.0723 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.049P)^2^+3.5833P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1670 _refine_ls_wR_factor_ref 0.1830 _reflns_number_gt 1409 _reflns_number_total 1663 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file av1215.cif _[local]_cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2014603 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Co1 0.0000 0.0000 0.0000 0.0258(4) Uani d S 1 . . Co O1W 0.3257(8) 0.1436(6) -0.0176(4) 0.0340(10) Uani d D 1 . . O H1WB 0.256(13) 0.213(8) -0.043(8) 0.051 Uiso d D 1 . . H H1WA 0.424(11) 0.112(10) -0.066(6) 0.051 Uiso d D 1 . . H O1 0.5229(8) -0.2380(6) 0.2600(4) 0.0373(11) Uani d . 1 . . O O2 -0.0798(8) -0.3480(6) 0.1046(5) 0.0439(12) Uani d . 1 . . O O3 0.2021(7) -0.1340(5) 0.0994(4) 0.0289(10) Uani d . 1 . . O N1 0.0041(9) 0.1961(6) 0.1866(5) 0.0288(11) Uani d . 1 . . N C1 0.6967(12) 0.0057(10) 0.4390(7) 0.0377(16) Uani d . 1 . . C H1 0.827(12) 0.013(9) 0.390(7) 0.035(18) Uiso d . 1 . . H C2 0.4983(11) -0.1217(9) 0.3782(6) 0.0333(14) Uani d . 1 . . C C3 0.3004(12) -0.1247(9) 0.4394(6) 0.0354(15) Uani d . 1 . . C H3 0.148(11) -0.219(8) 0.388(6) 0.025(15) Uiso d . 1 . . H C4 0.3146(12) -0.3576(9) 0.1871(7) 0.0364(15) Uani d . 1 . . C H4A 0.2449 -0.4144 0.2458 0.044 Uiso calc R 1 . . H H4B 0.3599 -0.4455 0.1168 0.044 Uiso calc R 1 . . H C5 0.1284(11) -0.2722(8) 0.1262(6) 0.0272(13) Uani d . 1 . . C C6 0.1777(11) 0.2226(8) 0.2897(6) 0.0311(14) Uani d . 1 . . C H6 0.3010 0.1597 0.2782 0.037 Uiso calc R 1 . . H C7 0.1815(11) 0.3394(8) 0.4123(6) 0.0318(14) Uani d . 1 . . C H7 0.3054 0.3526 0.4809 0.038 Uiso calc R 1 . . H C8 0.0019(10) 0.4370(7) 0.4339(5) 0.0259(13) Uani d . 1 . . C C9 -0.1754(12) 0.4119(9) 0.3260(6) 0.0366(16) Uani d . 1 . . C H9 -0.2991 0.4749 0.3339 0.044 Uiso calc R 1 . . H C10 -0.1655(11) 0.2915(9) 0.2062(6) 0.0375(16) Uani d . 1 . . C H10 -0.2855 0.2768 0.1352 0.045 Uiso calc R 1 . . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co1 0.0285(7) 0.0272(6) 0.0192(6) 0.0064(5) 0.0042(4) 0.0020(5) O1W 0.031(3) 0.042(3) 0.031(2) 0.008(2) 0.0082(19) 0.012(2) O1 0.032(2) 0.047(3) 0.031(2) 0.010(2) 0.0062(19) 0.006(2) O2 0.032(3) 0.042(3) 0.061(3) 0.005(2) 0.011(2) 0.020(2) O3 0.028(2) 0.034(2) 0.023(2) 0.0085(18) 0.0004(17) 0.0072(18) N1 0.024(3) 0.029(3) 0.027(3) 0.003(2) 0.002(2) -0.002(2) C1 0.030(4) 0.055(4) 0.034(4) 0.010(3) 0.011(3) 0.018(3) C2 0.030(3) 0.039(4) 0.037(4) 0.013(3) 0.007(3) 0.019(3) C3 0.032(4) 0.044(4) 0.029(3) 0.004(3) 0.004(3) 0.011(3) C4 0.039(4) 0.036(4) 0.036(4) 0.015(3) 0.006(3) 0.010(3) C5 0.031(3) 0.029(3) 0.021(3) 0.010(3) 0.006(2) 0.003(2) C6 0.036(4) 0.029(3) 0.025(3) 0.010(3) 0.004(3) 0.000(2) C7 0.035(4) 0.035(3) 0.019(3) 0.012(3) -0.005(2) -0.001(2) C8 0.030(3) 0.026(3) 0.019(3) 0.002(2) 0.001(2) 0.004(2) C9 0.035(4) 0.049(4) 0.023(3) 0.022(3) 0.000(3) 0.001(3) C10 0.028(3) 0.049(4) 0.025(3) 0.008(3) -0.005(3) -0.002(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 O3 2 2.086(4) yes Co1 O3 . 2.086(4) no Co1 O1W . 2.138(5) yes Co1 O1W 2 2.138(5) no Co1 N1 2 2.174(5) yes Co1 N1 . 2.174(5) no O1W H1WB . 0.82(7) no O1W H1WA . 0.83(6) no O1 C2 . 1.386(8) no O1 C4 . 1.432(8) no O2 C5 . 1.240(7) no O3 C5 . 1.274(7) no N1 C10 . 1.327(8) no N1 C6 . 1.341(8) no C1 C3 2_656 1.383(10) no C1 C2 . 1.396(10) no C1 H1 . 0.97(7) no C2 C3 . 1.380(9) no C3 C1 2_656 1.383(10) no C3 H3 . 1.07(6) no C4 C5 . 1.528(8) no C4 H4A . 0.9700 no C4 H4B . 0.9700 no C6 C7 . 1.382(8) no C6 H6 . 0.9300 no C7 C8 . 1.388(8) no C7 H7 . 0.9300 no C8 C9 . 1.392(8) no C8 C8 2_566 1.499(11) no C9 C10 . 1.390(9) no C9 H9 . 0.9300 no C10 H10 . 0.9300 no 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O3 Co1 O3 2 . 180.0(3) no O3 Co1 O1W 2 . 92.23(17) yes O3 Co1 O1W . . 87.77(17) no O3 Co1 O1W 2 2 87.77(17) no O3 Co1 O1W . 2 92.23(17) no O1W Co1 O1W . 2 180.0(2) no O3 Co1 N1 2 2 90.18(17) yes O3 Co1 N1 . 2 89.82(17) no O1W Co1 N1 . 2 91.88(18) yes O1W Co1 N1 2 2 88.12(18) no O3 Co1 N1 2 . 89.82(17) no O3 Co1 N1 . . 90.18(17) no O1W Co1 N1 . . 88.12(18) no O1W Co1 N1 2 . 91.88(18) no N1 Co1 N1 2 . 180.00(19) no Co1 O1W H1WB . . 92(6) no Co1 O1W H1WA . . 129(6) no H1WB O1W H1WA . . 110(8) no C2 O1 C4 . . 116.7(5) no C5 O3 Co1 . . 126.7(4) no C10 N1 C6 . . 116.6(5) no C10 N1 Co1 . . 122.5(4) no C6 N1 Co1 . . 120.8(4) no C3 C1 C2 2_656 . 121.1(6) no C3 C1 H1 2_656 . 121(4) no C2 C1 H1 . . 117(4) no C3 C2 O1 . . 125.7(6) no C3 C2 C1 . . 119.0(6) no O1 C2 C1 . . 115.2(6) no C2 C3 C1 . 2_656 119.9(6) no C2 C3 H3 . . 117(3) no C1 C3 H3 2_656 . 123(3) no O1 C4 C5 . . 113.1(5) no O1 C4 H4A . . 109.0 no C5 C4 H4A . . 109.0 no O1 C4 H4B . . 109.0 no C5 C4 H4B . . 109.0 no H4A C4 H4B . . 107.8 no O2 C5 O3 . . 126.6(6) no O2 C5 C4 . . 116.2(6) no O3 C5 C4 . . 117.2(5) no N1 C6 C7 . . 122.9(6) no N1 C6 H6 . . 118.5 no C7 C6 H6 . . 118.5 no C6 C7 C8 . . 120.6(5) no C6 C7 H7 . . 119.7 no C8 C7 H7 . . 119.7 no C7 C8 C9 . . 116.4(5) no C7 C8 C8 . 2_566 122.1(6) no C9 C8 C8 . 2_566 121.5(7) no C10 C9 C8 . . 119.2(6) no C10 C9 H9 . . 120.4 no C8 C9 H9 . . 120.4 no N1 C10 C9 . . 124.2(6) no N1 C10 H10 . . 117.9 no C9 C10 H10 . . 117.9 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O1W H1WB O2 2 0.83(6) 1.79(7) 2.609(7) 174(8) O1W H1WB O3 2 0.83(6) 2.59(7) 3.045(6) 116(7) O1W H1WA O3 2_655 0.82(7) 2.22(4) 2.958(6) 149(7) O1W H1WA O1 2_655 0.82(7) 2.58(7) 3.078(6) 120(7) _journal_paper_doi 10.1107/S0108270104031397