#------------------------------------------------------------------------------ #$Date: 2025-08-19 11:43:10 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301803 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/35/2203528.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_2203528 loop_ _publ_author_name 'Shan Gao' 'Zhu-Yan Zhang' 'Li-Hua Huo' 'Hui Zhao' 'Jing-Gui Zhao' _publ_section_title ; Hexaaquazinc(II) bis[(4-oxo-4H-pyridin-1-yl)acetate] dihydrate ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m444 _journal_page_last m446 _journal_paper_doi 10.1107/S1600536804006257 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Zn (H2 O)6] (C7 H6 N O3)2, 2H2 O' _chemical_formula_moiety 'H12 O6 Zn, 2(C7 H6 N O3), 2(H2 O)' _chemical_formula_sum 'C14 H28 N2 O14 Zn' _chemical_formula_weight 513.75 _chemical_name_systematic 'Hexaaquazinc(II) bis[(4-oxo-4H-pyridine-1-yl)acetate] dihydrate' _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 98.62(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 12.427(3) _cell_length_b 12.833(3) _cell_length_c 6.7816(14) _cell_measurement_reflns_used 8214 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.47 _cell_measurement_theta_min 3.23 _cell_volume 1069.3(4) _computing_cell_refinement RAPID-AUTO _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_data_reduction 'CrystalStructure (Rigaku/MSC, 2002)' _computing_molecular_graphics SHELXL97 _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 10.000 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0149 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 9929 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_min 3.17 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.222 _exptl_absorpt_correction_T_max 0.8100 _exptl_absorpt_correction_T_min 0.7032 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 536 _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.281 _refine_diff_density_min -0.422 _refine_ls_extinction_coef 0.040(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 1.048 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 158 _refine_ls_number_reflns 2447 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.052 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0272 _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^)+(0.0454P)^2^+0.3156P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0734 _refine_ls_wR_factor_ref 0.0752 _reflns_number_gt 2251 _reflns_number_total 2447 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ww6176.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2203528 _cod_database_fobs_code 2203528 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 Zn1 0.5000 0.0000 0.0000 0.02890(10) Uani d S 1 Zn O1 0.75756(9) 0.29091(8) -0.4060(2) 0.0375(3) Uani d . 1 O O2 0.60245(8) 0.19901(8) -0.4560(2) 0.0354(2) Uani d . 1 O O3 1.21414(9) 0.11950(10) -0.3263(2) 0.0449(3) Uani d . 1 O O1W 0.47143(9) 0.06870(10) 0.2677(2) 0.0433(3) Uani d D 1 O H8A 0.4103 0.0944 0.2524 0.065 Uiso calc RD 1 H O2W 0.66740(10) 0.01781(9) 0.0737(2) 0.0408(3) Uani d D 1 O H9A 0.6828 0.0799 0.0742 0.061 Uiso calc RD 1 H O3W 0.51419(9) -0.14356(8) 0.1426(2) 0.0350(2) Uani d D 1 O H10A 0.4761 -0.1865 0.0749 0.053 Uiso calc RD 1 H O4W 0.28170(10) 0.16620(10) 0.3088(3) 0.0620(4) Uani d D 1 O N1 0.88320(10) 0.11397(9) -0.3593(2) 0.0317(3) Uani d . 1 N C1 0.70450(10) 0.20850(10) -0.4166(2) 0.0283(3) Uani d . 1 C C2 0.76430(10) 0.10520(10) -0.3776(2) 0.0348(3) Uani d . 1 C H2A 0.7459 0.0752 -0.2558 0.042 Uiso calc R 1 H H2B 0.7390 0.0576 -0.4858 0.042 Uiso calc R 1 H C3 0.94810(10) 0.10490(10) -0.1808(2) 0.0383(3) Uani d . 1 C H3 0.9162 0.0962 -0.0662 0.046 Uiso calc R 1 H C4 1.05840(10) 0.10800(10) -0.1642(2) 0.0395(3) Uani d . 1 C H4 1.1003 0.1015 -0.0391 0.047 Uiso calc R 1 H C5 1.11090(10) 0.12090(10) -0.3353(2) 0.0336(3) Uani d . 1 C C6 1.03910(10) 0.13560(10) -0.5178(2) 0.0362(3) Uani d . 1 C H6 1.0679 0.1481 -0.6345 0.043 Uiso calc R 1 H C7 0.92970(10) 0.13160(10) -0.5243(2) 0.0359(3) Uani d . 1 C H7 0.8851 0.1413 -0.6458 0.043 Uiso calc R 1 H H8B 0.5179(9) 0.099(2) 0.344(3) 0.054 Uiso d D 1 H H10B 0.494(2) -0.138(2) 0.256(2) 0.054 Uiso d D 1 H H9B 0.703(2) -0.0220(10) 0.145(3) 0.054 Uiso d D 1 H H11B 0.279(2) 0.153(2) 0.428(2) 0.054 Uiso d D 1 H H11A 0.281(2) 0.2297(8) 0.289(3) 0.054 Uiso d D 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 Zn1 0.0262(2) 0.0256(2) 0.0335(2) -0.00223(8) -0.00002(9) 0.00012(8) O1 0.0326(5) 0.0273(5) 0.0502(6) 0.0011(4) -0.0010(5) -0.0018(4) O2 0.0272(5) 0.0347(5) 0.0429(6) 0.0022(4) 0.0013(4) 0.0011(4) O3 0.0287(5) 0.0483(7) 0.0562(7) 0.0043(5) 0.0011(5) 0.0080(5) O1W 0.0366(6) 0.0505(7) 0.0413(6) 0.0013(5) 0.0008(5) -0.0153(5) O2W 0.0284(6) 0.0314(5) 0.0584(8) -0.0045(4) -0.0074(5) 0.0080(5) O3W 0.0373(5) 0.0300(5) 0.0370(5) -0.0041(4) 0.0033(4) 0.0025(4) O4W 0.0655(9) 0.0510(8) 0.0760(10) 0.0135(7) 0.0330(8) 0.0096(7) N1 0.0288(6) 0.0282(6) 0.0377(6) 0.0061(5) 0.0034(5) 0.0031(5) C1 0.0285(6) 0.0292(6) 0.0266(6) 0.0038(5) 0.0026(5) -0.0008(5) C2 0.0301(7) 0.0282(7) 0.0464(8) 0.0024(6) 0.0063(6) 0.0029(6) C3 0.0404(8) 0.0416(8) 0.0329(7) 0.0065(7) 0.0059(6) 0.0019(6) C4 0.0377(8) 0.0452(9) 0.0333(8) 0.0060(7) -0.0018(6) 0.0006(6) C5 0.0308(7) 0.0255(6) 0.0432(8) 0.0034(5) 0.0014(6) 0.0020(6) C6 0.0346(7) 0.0369(8) 0.0374(8) 0.0032(7) 0.0063(6) 0.0071(6) C7 0.0345(7) 0.0377(8) 0.0340(7) 0.0061(6) 0.0003(6) 0.0066(6) 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' Zn Zn 0.2839 1.4301 '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 O3W Zn1 O3W 3_655 . 180.00(7) no O3W Zn1 O2W 3_655 3_655 88.48(5) no O3W Zn1 O2W . 3_655 91.52(5) yes O3W Zn1 O2W 3_655 . 91.52(5) no O3W Zn1 O2W . . 88.48(5) yes O2W Zn1 O2W 3_655 . 180.00(6) no O3W Zn1 O1W 3_655 3_655 89.07(5) no O3W Zn1 O1W . 3_655 90.93(5) no O2W Zn1 O1W 3_655 3_655 92.22(6) no O2W Zn1 O1W . 3_655 87.78(6) yes O3W Zn1 O1W 3_655 . 90.93(5) yes O3W Zn1 O1W . . 89.07(5) yes O2W Zn1 O1W 3_655 . 87.78(6) no O2W Zn1 O1W . . 92.22(6) yes O1W Zn1 O1W 3_655 . 180.00(6) no Zn1 O1W H8A . . 109.5 no Zn1 O1W H8B . . 124.0(10) no H8A O1W H8B . . 116.2 no Zn1 O2W H9A . . 109.5 no Zn1 O2W H9B . . 122(2) no H9A O2W H9B . . 120.8 no Zn1 O3W H10A . . 109.5 no Zn1 O3W H10B . . 109(2) no H10A O3W H10B . . 109.7 no H11B O4W H11A . . 111.0(10) no C7 N1 C3 . . 118.80(10) no C7 N1 C2 . . 119.40(10) no C3 N1 C2 . . 121.80(10) no O1 C1 O2 . . 127.00(10) no O1 C1 C2 . . 119.30(10) no O2 C1 C2 . . 113.70(10) no N1 C2 C1 . . 114.00(10) yes N1 C2 H2A . . 108.8 no C1 C2 H2A . . 108.8 no N1 C2 H2B . . 108.8 no C1 C2 H2B . . 108.8 no H2A C2 H2B . . 107.7 no N1 C3 C4 . . 122.00(10) no N1 C3 H3 . . 119.0 no C4 C3 H3 . . 119.0 no C3 C4 C5 . . 121.0(2) no C3 C4 H4 . . 119.5 no C5 C4 H4 . . 119.5 no O3 C5 C4 . . 122.6(2) no O3 C5 C6 . . 122.5(2) no C4 C5 C6 . . 114.90(10) no C7 C6 C5 . . 121.1(2) no C7 C6 H6 . . 119.4 no C5 C6 H6 . . 119.4 no N1 C7 C6 . . 122.00(10) no N1 C7 H7 . . 119.0 no C6 C7 H7 . . 119.0 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 Zn1 O3W 3_655 2.0760(10) no Zn1 O3W . 2.0760(10) yes Zn1 O2W 3_655 2.0770(10) no Zn1 O2W . 2.0770(10) yes Zn1 O1W 3_655 2.0960(10) no Zn1 O1W . 2.0960(10) yes O1 C1 . 1.242(2) yes O2 C1 . 1.262(2) yes O3 C5 . 1.276(2) yes O1W H8A . 0.8200 no O1W H8B . 0.82(2) no O2W H9A . 0.8200 no O2W H9B . 0.80(2) no O3W H10A . 0.8200 no O3W H10B . 0.84(2) no O4W H11B . 0.84(2) no O4W H11A . 0.83(2) no N1 C7 . 1.353(2) no N1 C3 . 1.355(2) no N1 C2 . 1.468(2) no C1 C2 . 1.524(2) no C2 H2A . 0.9700 no C2 H2B . 0.9700 no C3 C4 . 1.359(2) yes C3 H3 . 0.9300 no C4 C5 . 1.423(2) no C4 H4 . 0.9300 no C5 C6 . 1.425(2) no C6 C7 . 1.356(2) yes C6 H6 . 0.9300 no C7 H7 . 0.9300 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 H8A O4W . 0.82 1.93 2.720(2) 161 yes O1W H8B O2 1_556 0.82(2) 2.040(10) 2.836(2) 166(2) yes O2W H9A O1 4_566 0.82 1.89 2.694(2) 164 yes O2W H9B O3 3_755 0.80(2) 1.940(10) 2.730(2) 177(2) yes O3W H10A O2 2_644 0.82 1.88 2.690(2) 170 yes O3W H10B O2 3_655 0.84(2) 2.090(10) 2.837(2) 147.0(10) yes O4W H11B O3 1_456 0.84(2) 2.000(10) 2.794(2) 159(2) yes O4W H11A O3 4_466 0.83(2) 2.200(10) 2.980(2) 157(2) 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 _geom_torsion_publ_flag C7 N1 C2 C1 -73.1(2) no C3 N1 C2 C1 106.9(2) no O1 C1 C2 N1 -8.5(2) no O2 C1 C2 N1 171.90(10) no C7 N1 C3 C4 -3.2(2) no C2 N1 C3 C4 176.8(2) no N1 C3 C4 C5 0.0(3) no C3 C4 C5 O3 -176.8(2) no C3 C4 C5 C6 3.2(2) no O3 C5 C6 C7 176.70(10) no C4 C5 C6 C7 -3.2(2) no C3 N1 C7 C6 3.2(2) no C2 N1 C7 C6 -176.80(10) no C5 C6 C7 N1 0.2(2) no loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 168308731