#------------------------------------------------------------------------------ #$Date: 2025-08-19 11:43:10 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301803 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/67/2206762.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_2206762 loop_ _publ_author_name 'Dong-Dong Lin' 'Duan-Jun Xu' _publ_section_title ; Redetermination of diaquabis(vanillinato-\k^2^O,O')cobalt(II) ; _journal_coeditor_code NG6181 _journal_issue 9 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m1821 _journal_page_last m1822 _journal_paper_doi 10.1107/S1600536805026085 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '[Co (C8 H7 O3)2 (H2 O)2]' _chemical_formula_moiety 'C16 H18 Co O8' _chemical_formula_sum 'C16 H18 Co O8' _chemical_formula_weight 397.23 _chemical_name_systematic ; diaquabis(vanillinato-\k^2^O,O')cobalt(II) ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 107.249(12) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 22.270(2) _cell_length_b 10.4487(12) _cell_length_c 7.7771(9) _cell_measurement_reflns_used 6807 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 26.0 _cell_measurement_theta_min 3.2 _cell_volume 1728.3(3) _computing_cell_refinement PROCESS-AUTO _computing_data_collection 'PROCESS-AUTO (Rigaku, 1998)' _computing_data_reduction 'CrystalStructure (Rigaku/MSC, 2002)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'averaging the coordinates of the published Cc structure (Xiao et al., 2002)' _diffrn_ambient_temperature 295(2) _diffrn_detector_area_resol_mean 10.00 _diffrn_measured_fraction_theta_full 1.00 _diffrn_measured_fraction_theta_max 1.00 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \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 0.024 _diffrn_reflns_av_sigmaI/netI 0.016 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 7677 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 1.9 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.033 _exptl_absorpt_correction_T_max 0.738 _exptl_absorpt_correction_T_min 0.672 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 820 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.29 _refine_diff_density_min -0.24 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 115 _refine_ls_number_reflns 1973 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.087 _refine_ls_R_factor_all 0.036 _refine_ls_R_factor_gt 0.032 _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^)+(0.0446P)^2^+1.1767P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.082 _refine_ls_wR_factor_ref 0.084 _reflns_number_gt 1798 _reflns_number_total 1973 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ng6181.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2206762 _cod_database_fobs_code 2206762 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' '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_type_symbol Co 0.5000 0.15843(3) 0.2500 0.03372(12) Uani d S 1 Co O1 0.82098(6) 0.41801(17) 0.7983(2) 0.0611(4) Uani d . 1 O O2 0.43973(6) 0.02273(13) 0.2910(2) 0.0496(3) Uani d . 1 O H2A 0.4035 0.0479 0.2937 0.074 Uiso d R 1 H H2B 0.4518 -0.0479 0.3541 0.074 Uiso d R 1 H O3 0.57272(6) 0.30852(14) 0.24496(17) 0.0452(3) Uani d . 1 O O4 0.54453(6) 0.19436(12) 0.50848(16) 0.0377(3) Uani d . 1 O C3 0.61787(8) 0.31481(16) 0.4107(2) 0.0349(4) Uani d . 1 C C1 0.71767(8) 0.36917(18) 0.6190(3) 0.0401(4) Uani d . 1 C C2 0.67556(9) 0.37263(17) 0.4449(2) 0.0385(4) Uani d . 1 C H2 0.6866 0.4140 0.3529 0.046 Uiso calc R 1 H C4 0.59947(8) 0.25106(16) 0.5472(2) 0.0343(4) Uani d . 1 C C5 0.64209(9) 0.25060(19) 0.7208(2) 0.0417(4) Uani d . 1 C H5 0.6311 0.2108 0.8142 0.050 Uiso calc R 1 H C6 0.70003(9) 0.30838(19) 0.7547(3) 0.0439(4) Uani d . 1 C H6 0.7278 0.3065 0.8707 0.053 Uiso calc R 1 H C7 0.78041(9) 0.4211(2) 0.6527(3) 0.0498(5) Uani d . 1 C H7 0.7905 0.4593 0.5569 0.060 Uiso calc R 1 H C8 0.58407(14) 0.3723(3) 0.0982(3) 0.0782(9) Uani d . 1 C H8A 0.5488 0.3606 -0.0071 0.117 Uiso calc R 1 H H8B 0.6212 0.3379 0.0769 0.117 Uiso calc R 1 H H8C 0.5900 0.4620 0.1248 0.117 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 Co 0.02859(18) 0.03306(19) 0.03686(19) 0.000 0.00565(13) 0.000 O1 0.0355(7) 0.0744(11) 0.0694(10) -0.0115(7) 0.0094(7) -0.0162(8) O2 0.0303(6) 0.0434(7) 0.0730(9) 0.0000(5) 0.0119(6) 0.0151(7) O3 0.0464(7) 0.0498(8) 0.0351(6) -0.0143(6) 0.0053(5) 0.0055(6) O4 0.0330(6) 0.0411(7) 0.0382(6) -0.0069(5) 0.0093(5) 0.0029(5) C3 0.0368(9) 0.0315(8) 0.0348(8) -0.0026(7) 0.0082(7) -0.0018(6) C1 0.0348(9) 0.0369(9) 0.0477(10) -0.0048(7) 0.0110(7) -0.0074(7) C2 0.0403(9) 0.0363(9) 0.0410(9) -0.0064(7) 0.0153(7) -0.0018(7) C4 0.0337(8) 0.0305(8) 0.0387(8) -0.0022(6) 0.0111(7) -0.0022(7) C5 0.0446(10) 0.0440(10) 0.0353(9) -0.0085(8) 0.0099(7) 0.0006(7) C6 0.0392(10) 0.0467(10) 0.0401(9) -0.0049(8) 0.0029(8) -0.0024(8) C7 0.0392(10) 0.0513(11) 0.0602(12) -0.0086(9) 0.0170(9) -0.0106(10) C8 0.0832(18) 0.101(2) 0.0418(12) -0.0365(16) 0.0056(11) 0.0200(13) 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.0000 '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 O2 Co O2 . 2_655 92.02(8) y O2 Co O3 . . 172.33(5) y O2 Co O3 . 2_655 88.37(6) y O2 Co O3 2_655 . 88.37(6) ? O2 Co O4 . . 97.28(5) y O3 Co O3 . 2_655 92.27(8) y O3 Co O4 . . 75.09(5) ? O4 Co O4 . 2_655 158.32(8) y O4 Co O2 . 2_655 97.74(6) ? O4 Co O2 2_655 2_655 97.28(5) ? O4 Co O2 2_655 . 97.74(6) ? O4 Co O3 2_655 . 89.81(5) ? O4 Co O3 . 2_655 89.81(5) ? O4 Co O3 2_655 2_655 75.09(5) ? O2 Co O3 2_655 2_655 172.33(5) ? Co O2 H2A . . 117.3 ? Co O2 H2B . . 124.2 ? H2A O2 H2B . . 112.1 ? C3 O3 C8 . . 118.55(16) ? C3 O3 Co . . 110.08(10) ? C8 O3 Co . . 130.07(13) ? C4 O4 Co . . 117.87(11) ? C2 C3 O3 . . 125.61(16) ? C2 C3 C4 . . 121.69(16) ? O3 C3 C4 . . 112.68(15) ? C6 C1 C2 . . 119.26(17) ? C6 C1 C7 . . 120.70(18) ? C2 C1 C7 . . 119.91(18) ? C3 C2 C1 . . 119.74(17) ? C3 C2 H2 . . 120.1 ? C1 C2 H2 . . 120.1 ? O4 C4 C5 . . 122.62(16) ? O4 C4 C3 . . 119.93(15) ? C5 C4 C3 . . 117.45(16) ? C6 C5 C4 . . 120.74(17) ? C6 C5 H5 . . 119.6 ? C4 C5 H5 . . 119.6 ? C5 C6 C1 . . 121.12(17) ? C5 C6 H6 . . 119.4 ? C1 C6 H6 . . 119.4 ? O1 C7 C1 . . 124.5(2) ? O1 C7 H7 . . 117.7 ? C1 C7 H7 . . 117.7 ? O3 C8 H8A . . 109.5 ? O3 C8 H8B . . 109.5 ? H8A C8 H8B . . 109.5 ? O3 C8 H8C . . 109.5 ? H8A C8 H8C . . 109.5 ? H8B C8 H8C . . 109.5 ? 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 Co O2 2_655 2.0415(13) ? Co O2 . 2.0415(13) y Co O3 . 2.2631(13) y Co O3 2_655 2.2631(13) ? Co O4 . 1.9958(12) y Co O4 2_655 1.9958(12) ? O1 C7 . 1.222(3) y O2 H2A . 0.8555 ? O2 H2B . 0.8826 ? O3 C3 . 1.382(2) y O3 C8 . 1.408(3) y O4 C4 . 1.311(2) y C3 C2 . 1.372(2) ? C3 C4 . 1.413(2) ? C1 C6 . 1.384(3) ? C1 C2 . 1.400(3) ? C1 C7 . 1.448(3) ? C2 H2 . 0.9300 ? C4 C5 . 1.401(2) ? C5 C6 . 1.377(3) ? C5 H5 . 0.9300 ? C6 H6 . 0.9300 ? C7 H7 . 0.9300 ? C8 H8A . 0.9600 ? C8 H8B . 0.9600 ? C8 H8C . 0.9600 ? 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 O2 H2A O1 8_455 0.85 1.88 2.733(2) 173 y O2 H2B O4 5_656 0.88 1.85 2.7158(19) 165 y loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 168308876