#------------------------------------------------------------------------------ #$Date: 2016-02-20 03:06:23 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/23/2202383.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_2202383 loop_ _publ_author_name 'Yang, Shi-Yao' 'Long, La-Sheng' 'Huang, Rong-Bin' 'Zheng, Lan-Sun' 'Ng, Seik Weng' _publ_section_title ; catena-Poly[[[tetraaquacobalt(II)]-\m-pyrazine] phthalate] ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m961 _journal_page_last m963 _journal_paper_doi 10.1107/S1600536803021573 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Co (C4 H4 N2) (H2 O)4] (C8 H4 O4)' _chemical_formula_moiety 'C4 H12 Co N2 O4 2+, C8 H4 O4 2-' _chemical_formula_sum 'C12 H16 Co N2 O8' _chemical_formula_weight 375.20 _chemical_name_systematic ; catena-Poly[[[tetraaquacobalt(II)]-\m-pyrazine] phthalate] ; _space_group_IT_number 71 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-I 2 2' _symmetry_space_group_name_H-M 'I m m m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 7.1791(5) _cell_length_b 9.4033(6) _cell_length_c 10.2886(7) _cell_measurement_reflns_used 2933 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 28.4 _cell_measurement_theta_min 2.9 _cell_volume 694.55(8) _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_collection 'SMART (Bruker, 2001)' _computing_data_reduction SAINT _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'difference Fourier synthesis, with Co at (1/2, 1/2, 1/2)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measurement_device_type 'Bruker APEX area-detector' _diffrn_measurement_method '\f and \w' _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 0.053 _diffrn_reflns_av_sigmaI/netI 0.037 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 2970 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 2.9 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.28 _exptl_absorpt_correction_T_max 0.708 _exptl_absorpt_correction_T_min 0.437 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour Orange _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Prism _exptl_crystal_F_000 386 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.27 _refine_diff_density_max 1.67 _refine_diff_density_min -1.59 _refine_ls_extinction_coef 0.05(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.23 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 47 _refine_ls_number_reflns 480 _refine_ls_number_restraints 8 _refine_ls_restrained_S_all 1.30 _refine_ls_R_factor_all 0.097 _refine_ls_R_factor_gt 0.096 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.1108P)^2^+25.7589P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.297 _refine_ls_wR_factor_ref 0.297 _reflns_number_gt 472 _reflns_number_total 480 _reflns_threshold_expression I>2\s(I) _cod_data_source_file bt6353.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' 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 'Orthorhombic' changed to 'orthorhombic' 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 2202383 _cod_database_fobs_code 2202383 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' '-x, y, z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Co1 0.5000 0.5000 0.5000 0.0180(10) Uani d S 1 . . Co O1w 0.5000 0.6520(10) 0.6442(9) 0.035(2) Uani d S 1 . . O O1 0.216(2) 0.6180(10) 0.8260(10) 0.038(3) Uani d P 0.50 . . O N1 0.193(2) 0.5000 0.5000 0.026(3) Uani d S 1 . . N C1 0.0000 0.5000 0.9321(5) 0.043(5) Uani d SD 1 . . C C2 -0.1660(10) 0.5000 0.8598(7) 0.046(4) Uani d SD 1 . . C C3 -0.336(2) 0.5000 0.9316(5) 0.052(9) Uani d SPD 0.50 . . C C4 0.095(2) 0.3810(10) 0.5000 0.033(3) Uani d S 1 . . C H1w 0.4014 0.6486 0.6844 0.042 Uiso calc R 1 . . H H2 -0.1648 0.5000 0.7694 0.056 Uiso calc SPR 0.50 . . H H3 -0.4491 0.5000 0.8872 0.062 Uiso calc SPR 0.50 . . H H4 0.1580 0.2947 0.5000 0.040 Uiso calc SR 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 0.013(2) 0.020(2) 0.022(2) 0.000 0.000 0.000 O1w 0.037(5) 0.034(5) 0.033(5) 0.000 0.000 -0.007(4) O1 0.027(7) 0.036(7) 0.051(8) 0.003(5) 0.021(6) -0.001(6) N1 0.016(6) 0.032(7) 0.030(7) 0.000 0.000 0.000 C1 0.08(2) 0.018(8) 0.030(10) 0.000 0.000 0.000 C2 0.070(10) 0.035(7) 0.032(7) 0.000 -0.018(7) 0.000 C3 0.08(2) 0.04(2) 0.04(2) 0.000 -0.01(2) 0.000 C4 0.027(7) 0.022(6) 0.052(8) 0.001(5) 0.000 0.000 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 O1w Co1 O1w . 2_665 88.0(6) yes O1w Co1 O1w . 9_666 180.00(10) yes O1w Co1 O1w . 10_556 92.0(6) yes O1w Co1 N1 . . 90.00(10) yes O1w Co1 N1 . 9_666 90.00(10) yes O1w Co1 O1w 2_665 9_666 92.0(6) no O1w Co1 O1w 2_665 10_556 180.00(10) no O1w Co1 N1 2_665 . 90.00(10) no O1w Co1 N1 2_665 9_666 90.00(10) no O1w Co1 O1w 9_666 10_556 88.0(6) yes O1w Co1 N1 9_666 . 90.00(10) yes O1w Co1 N1 9_666 9_666 90.00(10) yes O1w Co1 N1 10_556 . 90.00(10) no O1w Co1 N1 10_556 9_666 90.00(10) no N1 Co1 N1 . 9_666 180.00(10) yes C4 N1 C4 . 3_566 116(2) no C4 N1 Co1 . . 122.2(7) no C4 N1 Co1 3_566 . 122.2(7) no C1 C1 C2 9_567 2_565 122.0(4) no C1 C1 C2 9_567 . 122.0(4) no C2 C1 C2 2_565 . 116.0(8) no C1 C2 C3 . . 116.9(7) no C3 C3 C2 10_557 . 121.1(4) no N1 C4 C4 . 11 122.2(7) no Co1 O1w H1w . . 109.5 no C1 C2 H2 . . 121.6 no C3 C2 H2 . . 121.6 no C3 C3 H3 10_557 . 119.4 no C2 C3 H3 . . 119.4 no N1 C4 H4 . . 118.9 no C4 C4 H4 11 . 118.9 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 . 2.062(9) yes Co1 O1w 2_665 2.062(9) no Co1 O1w 9_666 2.062(9) no Co1 O1w 10_556 2.062(9) no Co1 N1 . 2.200(10) yes Co1 N1 9_666 2.200(10) no O1 C2 2_565 1.210(10) no N1 C4 . 1.320(10) no N1 C4 3_566 1.320(10) no C1 C1 9_567 1.400(10) no C1 C2 2_565 1.404(9) no C1 C2 . 1.404(9) no C2 C3 . 1.430(10) no C3 C3 10_557 1.410(10) no C4 C4 11 1.37(3) no O1w H1w . 0.82 no C2 H2 . 0.93 no C3 H3 . 0.93 no C4 H4 . 0.93 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1w H1w O1 0.82 2.00 2.790(10) 162 no 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_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O1w Co1 N1 C4 9_666 . 46.0(3) no O1w Co1 N1 C4 . . -134.0(3) no O1w Co1 N1 C4 2_665 . -46.0(3) no O1w Co1 N1 C4 10_556 . 134.0(3) no N1 Co1 N1 C4 9_666 . 180.0 no O1w Co1 N1 C4 9_666 3_566 -134.0(3) no O1w Co1 N1 C4 . 3_566 46.0(3) no O1w Co1 N1 C4 2_665 3_566 134.0(3) no O1w Co1 N1 C4 10_556 3_566 -46.0(3) no N1 Co1 N1 C4 9_666 3_566 0.0 no C1 C1 C2 C3 9_567 . 0.00(10) no C2 C1 C2 C3 2_565 . 180.00(10) no C1 C2 C3 C3 . 10_557 0.00(10) no C4 N1 C4 C4 3_566 11 0.0 no Co1 N1 C4 C4 . 11 180.0 no