#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2204457.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_2204457 loop_ _publ_author_name 'Deng, Bing' 'Liu, Zhao-Di' 'Liu, Xiu-Ying' 'Tan, Min-Yu' 'Zhu, Hai-Liang' _publ_section_title ; Diaquabis(3-hydroxynaphthalene-2-carboxylato-\kO)zinc(II) ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m1568 _journal_page_last m1569 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Zn (C11 H7 O3)2 (H2 O)2]' _chemical_formula_moiety 'C22 H18 O8 Zn' _chemical_formula_sum 'C22 H18 O8 Zn' _chemical_formula_weight 475.73 _chemical_name_systematic ; Diaquabis(3-hydroxynaphthalene-2-carboxylato-\kO)zinc(II) ; _space_group_IT_number 5 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'C 2y' _symmetry_space_group_name_H-M 'C 1 2 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 95.06(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 15.597(9) _cell_length_b 5.509(4) _cell_length_c 12.648(7) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 15.0 _cell_measurement_theta_min 7.5 _cell_volume 1082.5(12) _computing_cell_refinement SHELXTL-Plus _computing_data_collection 'SHELXTL-Plus (Siemens, 1990)' _computing_data_reduction SHELXTL-Plus _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997b)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997a)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997a)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Siemens R3m' _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 0.0891 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 1227 _diffrn_reflns_theta_full 26.01 _diffrn_reflns_theta_max 26.01 _diffrn_reflns_theta_min 2.62 _diffrn_standards_decay_% none _diffrn_standards_interval_count 200 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 1.180 _exptl_absorpt_correction_T_max 0.8157 _exptl_absorpt_correction_T_min 0.5791 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 488 _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.411 _refine_diff_density_min -0.541 _refine_ls_abs_structure_details 'Flack (1983), no Friedel pairs' _refine_ls_abs_structure_Flack 0.00(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 141 _refine_ls_number_reflns 1180 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.016 _refine_ls_R_factor_all 0.0840 _refine_ls_R_factor_gt 0.0569 _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^)+(0.0945P)^2^+0.6786P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1399 _refine_ls_wR_factor_ref 0.1577 _reflns_number_gt 879 _reflns_number_total 1180 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ci6447.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'C 2' _cod_database_code 2204457 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' 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 1.0000 -0.00352(19) 0.0000 0.0620(5) Uani d S 1 Zn O1W 0.9212(4) -0.2331(12) -0.0830(5) 0.0801(19) Uani d . 1 O H1W 0.9342 -0.3585 -0.1131 0.120 Uiso d R 1 H H2W 0.8658 -0.2215 -0.0841 0.120 Uiso d R 1 H O1 1.0213(3) 0.3351(12) 0.1460(5) 0.0741(17) Uani d . 1 O O2 0.9037(4) 0.1548(12) 0.0702(5) 0.0720(16) Uani d . 1 O O3 0.7527(3) 0.3442(14) 0.0815(4) 0.0767(18) Uani d . 1 O H3 0.7893 0.2520 0.0616 0.115 Uiso calc R 1 H C1 0.9181(5) 0.6652(18) 0.2578(7) 0.065(2) Uani d . 1 C H1 0.9772 0.6603 0.2762 0.078 Uiso calc R 1 H C2 0.8826(4) 0.503(3) 0.1831(5) 0.0533(15) Uani d . 1 C C3 0.7912(4) 0.507(3) 0.1561(5) 0.0587(16) Uani d . 1 C C4 0.7391(5) 0.6730(18) 0.2027(7) 0.067(2) Uani d . 1 C H4 0.6800 0.6741 0.1850 0.081 Uiso calc R 1 H C5 0.7258(6) 1.020(3) 0.3275(6) 0.079(3) Uani d . 1 C H5 0.6666 1.0252 0.3103 0.095 Uiso calc R 1 H C6 0.7643(8) 1.186(2) 0.4010(7) 0.091(3) Uani d . 1 C H6 0.7307 1.3025 0.4309 0.110 Uiso calc R 1 H C7 0.8549(8) 1.177(2) 0.4304(8) 0.094(3) Uani d . 1 C H7 0.8796 1.2834 0.4817 0.112 Uiso calc R 1 H C8 0.9051(7) 1.014(4) 0.3833(7) 0.089(3) Uani d . 1 C H8 0.9644 1.0142 0.4001 0.107 Uiso calc R 1 H C9 0.8677(6) 0.8405(18) 0.3081(7) 0.066(2) Uani d . 1 C C10 0.7774(6) 0.8408(18) 0.2778(6) 0.065(2) Uani d . 1 C C11 0.9396(5) 0.3217(16) 0.1319(6) 0.0578(19) Uani d . 1 C 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 0.0516(7) 0.0452(7) 0.0903(9) 0.000 0.0115(5) 0.000 O1W 0.056(3) 0.062(4) 0.122(5) 0.002(3) 0.000(3) -0.035(4) O1 0.054(3) 0.059(4) 0.109(5) 0.007(3) 0.012(3) 0.008(4) O2 0.073(3) 0.051(3) 0.095(4) 0.001(3) 0.020(3) -0.012(4) O3 0.058(3) 0.077(4) 0.094(4) 0.007(3) 0.003(3) -0.029(4) C1 0.060(4) 0.064(6) 0.070(5) -0.005(5) 0.000(4) 0.007(5) C2 0.055(3) 0.049(3) 0.056(4) 0.007(9) 0.006(3) 0.008(7) C3 0.062(4) 0.049(4) 0.065(4) 0.007(8) 0.006(3) -0.003(8) C4 0.063(5) 0.061(5) 0.077(5) 0.003(5) 0.003(4) -0.001(5) C5 0.101(6) 0.066(7) 0.072(5) 0.027(9) 0.013(4) -0.010(8) C6 0.142(10) 0.060(7) 0.074(6) 0.012(8) 0.024(6) -0.004(6) C7 0.138(10) 0.064(6) 0.081(7) -0.011(8) 0.020(7) -0.011(6) C8 0.112(7) 0.076(6) 0.079(5) -0.010(12) 0.008(5) -0.025(9) C9 0.081(6) 0.051(5) 0.067(5) -0.006(5) 0.008(4) -0.005(5) C10 0.082(6) 0.054(5) 0.058(5) 0.009(5) 0.006(4) 0.001(5) C11 0.064(5) 0.041(4) 0.070(5) 0.004(4) 0.009(4) 0.008(4) 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' 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 O1W Zn1 O1W . 2_755 101.3(4) y O1W Zn1 O2 . 2_755 119.5(2) y O1W Zn1 O2 2_755 2_755 93.3(2) ? O1W Zn1 O2 . . 93.3(2) y O1W Zn1 O2 2_755 . 119.5(2) ? O2 Zn1 O2 2_755 . 128.6(4) y Zn1 O1W H1W . . 127.6 ? Zn1 O1W H2W . . 121.9 ? H1W O1W H2W . . 109.9 ? C11 O2 Zn1 . . 105.9(5) ? C3 O3 H3 . . 109.5 ? C2 C1 C9 . . 122.6(8) ? C2 C1 H1 . . 118.7 ? C9 C1 H1 . . 118.7 ? C1 C2 C3 . . 118.8(11) ? C1 C2 C11 . . 120.2(6) ? C3 C2 C11 . . 121.0(11) ? C4 C3 O3 . . 118.4(6) ? C4 C3 C2 . . 121.0(11) ? O3 C3 C2 . . 120.6(10) ? C3 C4 C10 . . 119.1(8) ? C3 C4 H4 . . 120.5 ? C10 C4 H4 . . 120.5 ? C6 C5 C10 . . 120.7(9) ? C6 C5 H5 . . 119.7 ? C10 C5 H5 . . 119.7 ? C5 C6 C7 . . 120.5(10) ? C5 C6 H6 . . 119.7 ? C7 C6 H6 . . 119.7 ? C8 C7 C6 . . 120.0(10) ? C8 C7 H7 . . 120.0 ? C6 C7 H7 . . 120.0 ? C7 C8 C9 . . 120.9(10) ? C7 C8 H8 . . 119.6 ? C9 C8 H8 . . 119.6 ? C10 C9 C1 . . 116.8(8) ? C10 C9 C8 . . 120.8(9) ? C1 C9 C8 . . 122.4(9) ? C4 C10 C9 . . 121.8(8) ? C4 C10 C5 . . 121.1(9) ? C9 C10 C5 . . 117.1(9) ? O1 C11 O2 . . 119.8(8) ? O1 C11 C2 . . 121.2(8) ? O2 C11 C2 . . 118.9(7) ? 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 O1W . 1.996(6) y Zn1 O1W 2_755 1.996(6) ? Zn1 O2 2_755 2.010(6) ? Zn1 O2 . 2.010(6) y O1W H1W . 0.82 ? O1W H2W . 0.87 ? O1 C11 . 1.273(9) ? O2 C11 . 1.300(10) ? O3 C3 . 1.399(14) ? O3 H3 . 0.82 ? C1 C2 . 1.382(15) ? C1 C9 . 1.430(13) ? C1 H1 . 0.93 ? C2 C3 . 1.436(9) ? C2 C11 . 1.518(15) ? C3 C4 . 1.389(14) ? C4 C10 . 1.418(12) ? C4 H4 . 0.93 ? C5 C6 . 1.400(17) ? C5 C10 . 1.452(15) ? C5 H5 . 0.93 ? C6 C7 . 1.429(14) ? C6 H6 . 0.93 ? C7 C8 . 1.367(18) ? C7 H7 . 0.93 ? C8 C9 . 1.434(17) ? C8 H8 . 0.93 ? C9 C10 . 1.426(13) ? 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 O1W H1W O1 2_745 0.82 1.89 2.688(9) 165 O1W H2W O3 4_645 0.87 1.89 2.747(8) 173 O3 H3 O2 . 0.82 1.86 2.591(8) 148 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 O1W Zn1 O2 C11 . -179.8(5) O1W Zn1 O2 C11 2_755 75.1(6) O2 Zn1 O2 C11 2_755 -47.3(5) C9 C1 C2 C3 . -1.1(15) C9 C1 C2 C11 . 179.6(8) C1 C2 C3 C4 . 0.9(16) C11 C2 C3 C4 . -179.9(10) C1 C2 C3 O3 . -179.4(10) C11 C2 C3 O3 . -0.2(16) O3 C3 C4 C10 . -179.4(9) C2 C3 C4 C10 . 0.3(16) C10 C5 C6 C7 . -1.6(18) C5 C6 C7 C8 . 2.9(18) C6 C7 C8 C9 . -3.2(19) C2 C1 C9 C10 . 0.2(13) C2 C1 C9 C8 . -178.1(11) C7 C8 C9 C10 . 2.3(19) C7 C8 C9 C1 . -179.5(10) C3 C4 C10 C9 . -1.2(14) C3 C4 C10 C5 . 179.0(10) C1 C9 C10 C4 . 1.0(13) C8 C9 C10 C4 . 179.3(11) C1 C9 C10 C5 . -179.3(9) C8 C9 C10 C5 . -0.9(16) C6 C5 C10 C4 . -179.6(10) C6 C5 C10 C9 . 0.6(16) Zn1 O2 C11 O1 . -7.8(9) Zn1 O2 C11 C2 . 170.1(7) C1 C2 C11 O1 . -9.1(14) C3 C2 C11 O1 . 171.7(10) C1 C2 C11 O2 . 173.0(8) C3 C2 C11 O2 . -6.2(14)