#------------------------------------------------------------------------------ #$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/43/2204384.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_2204384 loop_ _publ_author_name 'Shan Gao' 'Zhu-Yan Zhang' 'Li-Hua Huo' 'Hui Zhao' 'Jing-Gui Zhao' _publ_section_title ; 'Tetraaquabis[(2-oxo-4H-pyridin-1-yl)acetate]cobalt(II)' ; _journal_issue 10 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first m1422 _journal_page_last m1424 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Co (C7 H6 N O)2 (H2 O)4]' _chemical_formula_moiety 'C14 H20 Co N2 O10' _chemical_formula_sum 'C14 H20 Co N2 O10' _chemical_formula_weight 435.25 _chemical_name_systematic ; Tetraaquabis[(2-oxo-4H-pyridin-1-yl)acetate]cobalt(II) ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 113.83(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 10.527(2) _cell_length_b 7.0943(14) _cell_length_c 13.007(3) _cell_measurement_reflns_used 6681 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 3.3 _cell_volume 888.6(4) _computing_cell_refinement RAPID-AUTO _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_data_reduction 'CrystalStructure (Rigaku/MSC , 2002)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 10 _diffrn_measured_fraction_theta_full 1.00 _diffrn_measured_fraction_theta_max 1.00 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\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 0.024 _diffrn_reflns_av_sigmaI/netI 0.017 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 7469 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 3.2 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.024 _exptl_absorpt_correction_T_max 0.837 _exptl_absorpt_correction_T_min 0.709 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_crystal_colour Pink _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Prism _exptl_crystal_F_000 450 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.58 _refine_diff_density_min -0.31 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.06 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 136 _refine_ls_number_reflns 2031 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.06 _refine_ls_R_factor_all 0.047 _refine_ls_R_factor_gt 0.039 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0512P)^2^+0.7445P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.096 _refine_ls_wR_factor_ref 0.100 _reflns_number_gt 1776 _reflns_number_total 2031 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file sj6005.cif _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' 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 ; _cod_database_code 2204384 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' 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_type_symbol Co1 0.0000 0.0000 0.5000 0.02566(14) Uani d S 1 Co O1W 0.0321(2) 0.1517(3) 0.64431(15) 0.0531(5) Uani d D 1 O H1W1 -0.0567(11) 0.143(6) 0.621(3) 0.080 Uiso d D 1 H H1W2 0.064(3) 0.108(6) 0.7123(14) 0.080 Uiso d D 1 H O2W 0.10012(16) -0.2412(2) 0.59896(14) 0.0337(4) Uani d D 1 O H2W1 0.147(2) -0.304(3) 0.570(2) 0.051 Uiso d D 1 H H2W2 0.041(2) -0.315(3) 0.607(2) 0.051 Uiso d D 1 H O1 0.25580(17) 0.5484(3) 0.51970(14) 0.0382(4) Uani d . 1 O O2 0.08666(19) 0.5036(2) 0.34996(14) 0.0401(4) Uani d . 1 O O3 0.17912(17) 0.1043(3) 0.49781(17) 0.0520(5) Uani d . 1 O N1 0.37898(18) 0.2174(3) 0.50381(15) 0.0294(4) Uani d . 1 N C1 0.3079(2) 0.1110(3) 0.5514(2) 0.0339(5) Uani d . 1 C C2 0.3882(3) 0.0203(4) 0.6543(2) 0.0416(6) Uani d . 1 C H2 0.3446 -0.0531 0.6896 0.050 Uiso calc R 1 H C3 0.5284(3) 0.0395(4) 0.7017(2) 0.0478(7) Uani d . 1 C H3 0.5797 -0.0191 0.7699 0.057 Uiso calc R 1 H C4 0.5965(3) 0.1466(4) 0.6488(2) 0.0471(7) Uani d . 1 C H4 0.6927 0.1587 0.6810 0.057 Uiso calc R 1 H C5 0.5197(2) 0.2322(3) 0.5501(2) 0.0377(5) Uani d . 1 C H5 0.5638 0.3020 0.5135 0.045 Uiso calc R 1 H C6 0.2931(2) 0.3196(3) 0.40150(19) 0.0346(5) Uani d . 1 C H6A 0.2329 0.2316 0.3462 0.042 Uiso calc R 1 H H6B 0.3523 0.3797 0.3702 0.042 Uiso calc R 1 H C7 0.2045(2) 0.4698(3) 0.42696(19) 0.0306(5) Uani d . 1 C 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 0.0250(2) 0.0261(2) 0.0260(2) -0.00082(15) 0.01043(15) 0.00091(16) O1W 0.0816(14) 0.0411(10) 0.0300(9) 0.0150(10) 0.0157(9) 0.0007(8) O2W 0.0330(8) 0.0328(8) 0.0373(9) 0.0016(7) 0.0162(7) 0.0038(7) O1 0.0370(9) 0.0405(9) 0.0354(9) -0.0001(7) 0.0129(7) -0.0088(7) O2 0.0455(9) 0.0362(9) 0.0319(8) 0.0074(7) 0.0087(7) -0.0001(7) O3 0.0285(8) 0.0576(12) 0.0673(13) -0.0039(8) 0.0167(8) 0.0219(11) N1 0.0281(8) 0.0280(9) 0.0332(9) -0.0021(7) 0.0136(7) -0.0024(8) C1 0.0313(11) 0.0309(11) 0.0410(12) -0.0016(9) 0.0162(9) 0.0016(10) C2 0.0496(14) 0.0381(13) 0.0388(13) 0.0035(11) 0.0193(11) 0.0044(10) C3 0.0499(15) 0.0435(14) 0.0359(13) 0.0082(12) 0.0029(11) -0.0027(11) C4 0.0274(11) 0.0447(14) 0.0565(16) 0.0000(10) 0.0039(11) -0.0155(13) C5 0.0314(11) 0.0328(12) 0.0529(14) -0.0055(9) 0.0214(10) -0.0117(11) C6 0.0420(12) 0.0320(11) 0.0321(11) 0.0006(10) 0.0173(10) -0.0003(9) C7 0.0358(11) 0.0266(10) 0.0329(11) -0.0023(8) 0.0176(9) 0.0024(9) 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 O1W . . 90.63(10) yes O3 Co1 O1W . 3_556 89.37(10) yes O3 Co1 O2W . . 93.73(7) yes O3 Co1 O2W . 3_556 86.27(7) yes O1W Co1 O2W . . 90.57(7) yes O1W Co1 O2W . 3_556 89.43(7) yes N1 C6 C7 . . 110.66(19) yes O3 Co1 O3 3_556 . 180.0 no O3 Co1 O1W 3_556 3_556 90.63(10) no O3 Co1 O1W 3_556 . 89.37(10) no O1W Co1 O1W 3_556 . 180.0 no O3 Co1 O2W 3_556 . 86.27(7) no O1W Co1 O2W 3_556 . 89.43(7) no O3 Co1 O2W 3_556 3_556 93.73(7) no O1W Co1 O2W 3_556 3_556 90.57(7) no O2W Co1 O2W . 3_556 180.0 no Co1 O1W H1W1 . . 84(3) no Co1 O1W H1W2 . . 126(3) no H1W1 O1W H1W2 . . 104.5(15) no Co1 O2W H2W1 . . 112(2) no Co1 O2W H2W2 . . 111(2) no H2W1 O2W H2W2 . . 108.3(16) no C1 O3 Co1 . . 143.85(17) no C5 N1 C1 . . 122.5(2) no C5 N1 C6 . . 121.8(2) no C1 N1 C6 . . 115.68(18) no O3 C1 N1 . . 115.8(2) no O3 C1 C2 . . 127.6(2) no N1 C1 C2 . . 116.7(2) no C3 C2 C1 . . 120.6(3) no C3 C2 H2 . . 119.7 no C1 C2 H2 . . 119.7 no C2 C3 C4 . . 120.7(3) no C2 C3 H3 . . 119.7 no C4 C3 H3 . . 119.7 no C5 C4 C3 . . 118.7(2) no C5 C4 H4 . . 120.6 no C3 C4 H4 . . 120.6 no C4 C5 N1 . . 120.8(2) no C4 C5 H5 . . 119.6 no N1 C5 H5 . . 119.6 no N1 C6 H6A . . 109.5 no C7 C6 H6A . . 109.5 no N1 C6 H6B . . 109.5 no C7 C6 H6B . . 109.5 no H6A C6 H6B . . 108.1 no O1 C7 O2 . . 126.1(2) no O1 C7 C6 . . 117.3(2) no O2 C7 C6 . . 116.6(2) no 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 O1W . 2.0694(19) yes Co1 O2W . 2.1447(17) yes Co1 O3 . 2.0364(17) yes O3 C1 . 1.250(3) yes C2 C3 . 1.356(4) yes C4 C5 . 1.353(4) yes O1 C7 . 1.238(3) yes O2 C7 . 1.263(3) yes Co1 O1W 3_556 2.0694(19) no Co1 O2W 3_556 2.1447(17) no Co1 O3 3_556 2.0364(17) no O1W H1W1 . 0.86(3) no O1W H1W2 . 0.86(3) no O2W H2W1 . 0.86(3) no O2W H2W2 . 0.85(3) no N1 C5 . 1.359(3) no N1 C1 . 1.374(3) no N1 C6 . 1.463(3) no C1 C2 . 1.416(3) no C2 H2 . 0.9300 no C3 C4 . 1.401(4) no C3 H3 . 0.9300 no C4 H4 . 0.9300 no C5 H5 . 0.9300 no C6 C7 . 1.538(3) no C6 H6A . 0.9700 no C6 H6B . 0.9700 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 _geom_hbond_publ_flag O1W H1W1 O3 3_556 0.86(3) 2.35(4) 2.887(3) 121(3) yes O1W H1W2 O2 4_566 0.86(3) 1.88(3) 2.731(3) 166(3) yes O2W H2W1 O1 1_545 0.86(3) 1.85(3) 2.709(2) 175(3) yes O2W H2W2 O2 3_556 0.85(3) 2.13(3) 2.971(3) 172(3) yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion _geom_torsion_publ_flag O1W Co1 O3 C1 3_556 -118.1(3) no O1W Co1 O3 C1 . 61.9(3) no O2W Co1 O3 C1 . -28.7(3) no O2W Co1 O3 C1 3_556 151.3(3) no Co1 O3 C1 N1 . -178.1(2) no Co1 O3 C1 C2 . 2.7(5) no C5 N1 C1 O3 . -177.5(2) no C6 N1 C1 O3 . 4.5(3) no C5 N1 C1 C2 . 1.8(3) no C6 N1 C1 C2 . -176.2(2) no O3 C1 C2 C3 . 179.1(3) no N1 C1 C2 C3 . -0.1(4) no C1 C2 C3 C4 . -1.1(4) no C2 C3 C4 C5 . 0.7(4) no C3 C4 C5 N1 . 1.1(4) no C1 N1 C5 C4 . -2.4(4) no C6 N1 C5 C4 . 175.5(2) no C5 N1 C6 C7 . -113.1(2) no C1 N1 C6 C7 . 64.9(3) no N1 C6 C7 O1 . 33.8(3) no N1 C6 C7 O2 . -147.4(2) no