#------------------------------------------------------------------------------ #$Date: 2011-01-02 20:00:31 +0000 (Sun, 02 Jan 2011) $ #$Revision: 5310 $ #$URL: svn://www.crystallography.net/cod/cif/2/2214447.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_2214447 loop_ _publ_author_name 'Liu, Yen-Hsiang' 'Ding, Miao-Tzu' _publ_section_title ; Poly[[tetraaqua(\m~6~-benzene-1,2,4,5-tetracarboxylato)dicobalt(II)] dihydrate] ; _journal_coeditor_code XU2263 _journal_issue 7 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first m1828 _journal_page_last m1829 _journal_volume 63 _journal_year 2007 _chemical_formula_iupac '[Co2 (C10 H2 O8) (H2 O)4], 2H2 O' _chemical_formula_moiety 'C5 H5 Co O6, H2 O' _chemical_formula_sum 'C5 H7 Co O7' _chemical_formula_weight 238.04 _chemical_name_systematic ; Poly[[tetraaqua(\m~6~-benzene-1,2,4,5-tetracarboxylato)dicobalt(II)] dihydrate] ; _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90.342(8) _cell_angle_beta 109.848(7) _cell_angle_gamma 93.161(7) _cell_formula_units_Z 2 _cell_length_a 6.9362(7) _cell_length_b 7.4559(6) _cell_length_c 8.2797(7) _cell_measurement_reflns_used 34 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 12.82 _cell_measurement_theta_min 5.58 _cell_volume 402.00(6) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Bruker, 1991)' _computing_data_reduction XSCANS _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997) and PLATON (Spek, 2003)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.97 _diffrn_measured_fraction_theta_max 0.97 _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.028 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 2314 _diffrn_reflns_theta_full 28.0 _diffrn_reflns_theta_max 28.0 _diffrn_reflns_theta_min 2.6 _diffrn_standards_decay_% 1.0 _diffrn_standards_interval_count 24 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.139 _exptl_absorpt_correction_T_max 0.811 _exptl_absorpt_correction_T_min 0.685 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.966 _exptl_crystal_density_method 'not measured' _exptl_crystal_description column _exptl_crystal_F_000 240 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.588 _refine_diff_density_min -0.774 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 131 _refine_ls_number_reflns 1883 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.047 _refine_ls_R_factor_gt 0.038 _refine_ls_shift/su_max 0.00 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+0.4406P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.103 _reflns_number_gt 1570 _reflns_number_total 1883 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file xu2263.cif _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 ; _cod_database_code 2214447 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _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 Co Co1 0 0 0.5 0.01624(16) Uani d S 1 Co Co2 0.5 0.5 0.5 0.01426(16) Uani d S 1 O O1 0.1694(3) 0.2325(3) 0.6119(3) 0.0223(4) Uani d . 1 O O2 0.4875(3) 0.3576(3) 0.7123(3) 0.0227(4) Uani d . 1 O O3 0.2645(3) -0.1283(3) 0.5378(3) 0.0268(5) Uani d . 1 O O4 0.5570(3) -0.2620(3) 0.6499(2) 0.0175(4) Uani d . 1 O O21 0.0391(4) 0.0928(4) 0.2669(3) 0.0342(6) Uani d . 1 H H21A 0.151 0.1538 0.2826 0.051 Uiso d R 1 H H21B -0.0337 0.0886 0.1656 0.051 Uiso d R 1 O O22 0.1793(3) 0.5155(3) 0.3953(3) 0.0265(5) Uani d . 1 H H22A 0.1224 0.6092 0.404 0.04 Uiso d R 1 H H22B 0.1421 0.4397 0.4559 0.04 Uiso d R 1 O O31A -0.0980(8) 0.2254(8) -0.0766(7) 0.0469(18) Uani d P 0.527(8) O O31B -0.1415(13) 0.4510(14) 0.0178(11) 0.089(4) Uani d P 0.473(8) C C1 0.3523(4) 0.2411(4) 0.7155(3) 0.0155(5) Uani d . 1 C C2 0.4193(4) 0.1081(4) 0.8574(3) 0.0150(5) Uani d . 1 C C3 0.4640(4) -0.0677(4) 0.8333(3) 0.0136(5) Uani d . 1 C C4 0.4246(4) -0.1563(4) 0.6596(3) 0.0145(5) Uani d . 1 C C5 0.4549(4) 0.1741(4) 1.0238(3) 0.0163(5) Uani d . 1 H H5A 0.4241 0.2912 1.0399 0.02 Uiso calc R 1 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 0.0143(3) 0.0151(3) 0.0165(3) 0.00031(19) 0.0018(2) -0.00175(19) Co2 0.0178(3) 0.0117(3) 0.0122(2) -0.00056(19) 0.00392(19) -0.00044(18) O1 0.0210(10) 0.0161(10) 0.0224(10) -0.0007(8) -0.0018(8) 0.0031(8) O2 0.0236(11) 0.0234(11) 0.0181(9) -0.0065(8) 0.0042(8) 0.0048(8) O3 0.0238(11) 0.0343(13) 0.0170(10) 0.0117(9) -0.0015(8) -0.0091(9) O4 0.0177(9) 0.0163(9) 0.0170(9) 0.0033(7) 0.0035(8) -0.0042(7) O21 0.0222(11) 0.0541(16) 0.0214(11) -0.0087(11) 0.0028(9) 0.0053(10) O22 0.0219(10) 0.0225(11) 0.0346(12) 0.0025(9) 0.0088(9) -0.0006(9) O31A 0.038(3) 0.059(4) 0.040(3) -0.001(3) 0.009(2) 0.004(3) O31B 0.068(6) 0.092(7) 0.067(5) -0.026(5) -0.023(4) 0.007(5) C1 0.0210(13) 0.0127(12) 0.0120(11) 0.0002(10) 0.0048(10) -0.0032(9) C2 0.0143(12) 0.0158(12) 0.0127(11) -0.0026(10) 0.0025(10) -0.0019(9) C3 0.0140(12) 0.0147(12) 0.0107(11) -0.0023(9) 0.0032(9) -0.0035(9) C4 0.0174(12) 0.0129(12) 0.0130(11) -0.0008(10) 0.0052(10) -0.0026(9) C5 0.0201(13) 0.0131(12) 0.0158(12) 0.0007(10) 0.0062(10) -0.0018(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 '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 O3 Co1 O3 2_556 . 180.00(12) O3 Co1 O1 2_556 . 89.65(9) O3 Co1 O1 . . 90.35(9) O3 Co1 O1 2_556 2_556 90.35(9) O3 Co1 O1 . 2_556 89.65(9) O1 Co1 O1 . 2_556 180 O3 Co1 O21 2_556 . 94.40(10) O3 Co1 O21 . . 85.60(10) O1 Co1 O21 . . 85.35(9) O1 Co1 O21 2_556 . 94.65(9) O3 Co1 O21 2_556 2_556 85.60(10) O3 Co1 O21 . 2_556 94.40(10) O1 Co1 O21 . 2_556 94.65(9) O1 Co1 O21 2_556 2_556 85.35(9) O21 Co1 O21 . 2_556 180.0000(10) O2 Co2 O2 2_666 . 180.0000(10) O2 Co2 O4 2_666 1_565 91.12(8) O2 Co2 O4 . 1_565 88.88(8) O2 Co2 O4 2_666 2_656 88.88(8) O2 Co2 O4 . 2_656 91.12(8) O4 Co2 O4 1_565 2_656 180 O2 Co2 O22 2_666 . 86.24(9) O2 Co2 O22 . . 93.76(9) O4 Co2 O22 1_565 . 96.15(8) O4 Co2 O22 2_656 . 83.85(8) O2 Co2 O22 2_666 2_666 93.76(9) O2 Co2 O22 . 2_666 86.24(9) O4 Co2 O22 1_565 2_666 83.85(8) O4 Co2 O22 2_656 2_666 96.15(8) O22 Co2 O22 . 2_666 180.0000(10) C1 O1 Co1 . . 125.58(19) C1 O2 Co2 . . 126.83(18) C4 O3 Co1 . . 137.74(18) C4 O4 Co2 . 1_545 126.45(17) Co1 O21 H21A . . 113.9 Co1 O21 H21B . . 134.3 H21A O21 H21B . . 111.6 Co2 O22 H22A . . 121.8 Co2 O22 H22B . . 99.9 H22A O22 H22B . . 105.4 O2 C1 O1 . . 124.3(3) O2 C1 C2 . . 115.2(2) O1 C1 C2 . . 120.4(2) C3 C2 C5 . . 119.3(2) C3 C2 C1 . . 124.0(2) C5 C2 C1 . . 116.4(2) C2 C3 C5 . 2_657 119.4(2) C2 C3 C4 . . 124.2(2) C5 C3 C4 2_657 . 116.4(2) O3 C4 O4 . . 123.9(2) O3 C4 C3 . . 119.9(2) O4 C4 C3 . . 116.1(2) C2 C5 C3 . 2_657 121.4(2) C2 C5 H5A . . 119.3 C3 C5 H5A 2_657 . 119.3 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 O1 . 2.065(2) y Co1 O1 2_556 2.065(2) ? Co1 O3 2_556 2.046(2) ? Co1 O3 . 2.046(2) y Co1 O21 . 2.151(2) y Co1 O21 2_556 2.151(2) ? Co2 O2 2_666 2.083(2) ? Co2 O2 . 2.083(2) y Co2 O4 1_565 2.0996(19) y Co2 O4 2_656 2.0996(19) ? Co2 O22 . 2.105(2) y Co2 O22 2_666 2.105(2) ? O1 C1 . 1.265(3) ? O2 C1 . 1.250(3) ? O3 C4 . 1.250(3) ? O4 C4 . 1.264(3) ? O4 Co2 1_545 2.0996(19) ? O21 H21A . 0.8472 ? O21 H21B . 0.8188 ? O22 H22A . 0.8359 ? O22 H22B . 0.8447 ? C1 C2 . 1.508(4) ? C2 C3 . 1.392(4) ? C2 C5 . 1.395(3) ? C3 C5 2_657 1.398(4) ? C3 C4 . 1.511(3) ? C5 C3 2_657 1.398(4) ? C5 H5A . 0.93 ? 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 O21 H21A O4 2_656 0.85 2.03 2.864(3) 169 O21 H21B O31A . 0.82 2.17 2.876(6) 144 O22 H22A O3 1_565 0.84 2.25 2.848(3) 129 O22 H22B O1 . 0.84 1.99 2.790(3) 157