#------------------------------------------------------------------------------ #$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $ #$Revision: 176798 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/23/66/2236698.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_2236698 loop_ _publ_author_name 'Jin, Shouwen' 'Huang, Yanfei' 'Wei, Shuaishuai' 'Zhou, Yong' 'Zhou, Yingping' _publ_section_title ; Poly[diammonium [(\m~4~-butane-1,2,3,4-tetracarboxylato)zincate] tetrahydrate] ; _journal_coeditor_code WM2679 _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m1268 _journal_page_last m1269 _journal_paper_doi 10.1107/S1600536812038883 _journal_volume 68 _journal_year 2012 _chemical_formula_iupac '(N H4)2 [Zn (C8 H6 O8)], 4H2 O' _chemical_formula_moiety '2(H4 N +), C8 H6 O8 Zn 2-, 4(H2 O)' _chemical_formula_sum 'C8 H22 N2 O12 Zn' _chemical_formula_weight 403.65 _chemical_name_systematic ; Poly[diammonium [(\m~4~-butane-1,2,3,4-tetracarboxylato)zincate] tetrahydrate] ; _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 111.761(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 14.1153(12) _cell_length_b 8.8505(8) _cell_length_c 13.5704(11) _cell_measurement_reflns_used 2092 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 27.613 _cell_measurement_theta_min 2.777 _cell_volume 1574.5(2) _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_collection 'SMART (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'publCIF (Westrip, 2010)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker SMART 1K CCD area-detector' _diffrn_measurement_method 'phi and omega 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 0.0894 _diffrn_reflns_av_sigmaI/netI 0.0646 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 3841 _diffrn_reflns_theta_full 25.01 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_min 2.78 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.625 _exptl_absorpt_correction_T_max 0.823 _exptl_absorpt_correction_T_min 0.697 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2002)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 840 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _refine_diff_density_max 1.526 _refine_diff_density_min -1.300 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 105 _refine_ls_number_reflns 1386 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.018 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0587 _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^)+(0.1135P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1483 _refine_ls_wR_factor_ref 0.1556 _reflns_number_gt 1167 _reflns_number_total 1386 _reflns_threshold_expression I>2sigma(I) _cod_data_source_file wm2679.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2236698 _cod_database_fobs_code 2236698 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_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 _atom_site_symmetry_multiplicity Zn Zn1 0.5000 0.50029(6) 0.7500 0.0196(3) Uani d S 1 2 N N1 0.6212(3) 0.8163(4) 0.5030(3) 0.0379(9) Uani d . 1 1 H H1C 0.5861 0.8480 0.5427 0.045 Uiso d R 1 1 H H1D 0.6836 0.8588 0.5287 0.045 Uiso d R 1 1 H H1A 0.5884 0.8440 0.4350 0.045 Uiso d R 1 1 H H1B 0.6269 0.7150 0.5062 0.045 Uiso d R 1 1 O O1 0.41853(19) 0.6486(3) 0.6404(2) 0.0291(7) Uani d . 1 1 O O2 0.3143(2) 0.4535(4) 0.5878(2) 0.0340(7) Uani d . 1 1 O O3 0.3480(3) 0.4657(4) 0.3648(3) 0.0413(8) Uani d . 1 1 O O4 0.44049(18) 0.6425(3) 0.32532(19) 0.0262(6) Uani d . 1 1 O O5 0.5186(2) 0.9191(4) 0.6280(3) 0.0516(9) Uani d . 1 1 H H5C 0.4923 0.8395 0.6420 0.062 Uiso d R 1 1 H H5D 0.5526 0.9635 0.6859 0.062 Uiso d R 1 1 O O6 0.6370(2) 0.0991(3) 0.7995(2) 0.0470(8) Uani d . 1 1 H H6C 0.7008 0.0871 0.8163 0.056 Uiso d R 1 1 H H6D 0.6189 0.1787 0.7622 0.056 Uiso d R 1 1 C C1 0.3369(3) 0.5846(4) 0.5744(3) 0.0210(8) Uani d . 1 1 C C2 0.3742(3) 0.5970(5) 0.3645(3) 0.0244(9) Uani d . 1 1 C C3 0.2700(3) 0.6794(4) 0.4801(3) 0.0203(8) Uani d . 1 1 H H3 0.2111 0.6180 0.4378 0.024 Uiso calc R 1 1 C C4 0.3286(3) 0.7247(4) 0.4090(3) 0.0254(9) Uani d . 1 1 H H4A 0.2827 0.7823 0.3496 0.030 Uiso calc R 1 1 H H4B 0.3836 0.7918 0.4494 0.030 Uiso calc R 1 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 Zn1 0.0194(4) 0.0239(5) 0.0197(5) 0.000 0.0122(3) 0.000 N1 0.039(2) 0.039(2) 0.042(2) -0.0020(16) 0.0213(18) -0.0064(16) O1 0.0260(14) 0.0341(16) 0.0247(15) 0.0003(12) 0.0064(12) 0.0014(12) O2 0.0367(17) 0.0293(16) 0.0373(18) 0.0002(14) 0.0152(14) 0.0075(14) O3 0.053(2) 0.0317(17) 0.056(2) -0.0036(16) 0.0396(18) -0.0033(15) O4 0.0259(13) 0.0337(15) 0.0268(14) 0.0008(12) 0.0187(12) -0.0014(11) O5 0.061(2) 0.055(2) 0.053(2) -0.0072(18) 0.0373(18) -0.0061(17) O6 0.0522(18) 0.0453(19) 0.0493(19) 0.0042(16) 0.0257(16) 0.0129(16) C1 0.0232(18) 0.028(2) 0.0190(18) 0.0074(16) 0.0157(16) -0.0022(15) C2 0.0236(18) 0.035(2) 0.0190(19) 0.0058(17) 0.0126(16) -0.0008(16) C3 0.0197(17) 0.026(2) 0.0183(18) 0.0006(15) 0.0108(15) -0.0012(14) C4 0.0267(19) 0.031(2) 0.025(2) 0.0040(17) 0.0170(17) 0.0035(16) 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 O4 Zn1 O4 5_666 6_566 101.42(14) O4 Zn1 O1 5_666 2_656 124.21(10) O4 Zn1 O1 6_566 2_656 105.67(10) O4 Zn1 O1 5_666 . 105.67(10) O4 Zn1 O1 6_566 . 124.21(10) O1 Zn1 O1 2_656 . 97.83(15) H1C N1 H1D . . 108.3 H1C N1 H1A . . 109.9 H1D N1 H1A . . 109.9 H1C N1 H1B . . 109.9 H1D N1 H1B . . 109.9 H1A N1 H1B . . 108.9 C1 O1 Zn1 . . 110.2(2) C2 O4 Zn1 . 5_666 121.1(2) H5C O5 H5D . . 108.7 H6C O6 H6D . . 108.6 O2 C1 O1 . . 121.4(3) O2 C1 C3 . . 121.7(3) O1 C1 C3 . . 116.9(3) O3 C2 O4 . . 124.1(3) O3 C2 C4 . . 122.0(4) O4 C2 C4 . . 113.9(3) C1 C3 C4 . . 111.0(3) C1 C3 C3 . 7_566 110.1(3) C4 C3 C3 . 7_566 110.9(4) C1 C3 H3 . . 108.2 C4 C3 H3 . . 108.2 C3 C3 H3 7_566 . 108.2 C2 C4 C3 . . 117.2(3) C2 C4 H4A . . 108.0 C3 C4 H4A . . 108.0 C2 C4 H4B . . 108.0 C3 C4 H4B . . 108.0 H4A C4 H4B . . 107.2 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Zn1 O4 5_666 1.996(2) Zn1 O4 6_566 1.996(2) Zn1 O1 2_656 1.998(3) Zn1 O1 . 1.998(3) N1 H1C . 0.9000 N1 H1D . 0.9001 N1 H1A . 0.9001 N1 H1B . 0.9000 O1 C1 . 1.298(4) O2 C1 . 1.234(5) O3 C2 . 1.220(5) O4 C2 . 1.300(4) O4 Zn1 5_666 1.996(2) O5 H5C . 0.8499 O5 H5D . 0.8500 O6 H6C . 0.8500 O6 H6D . 0.8500 C1 C3 . 1.529(5) C2 C4 . 1.531(5) C3 C4 . 1.540(5) C3 C3 7_566 1.548(7) C3 H3 . 0.9800 C4 H4A . 0.9700 C4 H4B . 0.9700 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 O6 H6D O4 5_666 0.85 1.97 2.814(4) 172.8 O6 H6C O3 8_556 0.85 1.99 2.833(5) 173.1 O5 H5D O6 1_565 0.85 1.97 2.805(5) 167.5 O5 H5C O1 . 0.85 1.98 2.816(4) 167.4 N1 H1B O2 5_666 0.90 2.31 2.981(5) 131.4 N1 H1B O3 5_666 0.90 2.30 3.009(5) 135.7 N1 H1A O5 5_676 0.90 2.54 3.153(5) 125.8 N1 H1A O6 6_565 0.90 2.24 2.948(5) 134.7 N1 H1D O2 3 0.90 1.91 2.810(5) 177.5 N1 H1C O5 . 0.90 1.86 2.761(5) 177.4 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 O4 Zn1 O1 C1 5_666 . 71.4(2) O4 Zn1 O1 C1 6_566 . -44.7(3) O1 Zn1 O1 C1 2_656 . -159.7(3) Zn1 O1 C1 O2 . . 5.1(4) Zn1 O1 C1 C3 . . -175.4(2) Zn1 O4 C2 O3 5_666 . 4.7(5) Zn1 O4 C2 C4 5_666 . -173.9(2) O2 C1 C3 C4 . . -118.4(4) O1 C1 C3 C4 . . 62.1(4) O2 C1 C3 C3 . 7_566 118.4(4) O1 C1 C3 C3 . 7_566 -61.2(4) O3 C2 C4 C3 . . 15.6(5) O4 C2 C4 C3 . . -165.7(3) C1 C3 C4 C2 . . 56.4(4) C3 C3 C4 C2 7_566 . 179.2(3)