data_2203247 loop_ _publ_author_name 'Xu, Hongbin' 'Liang, Yucang' 'Su, Zhongmin' 'Zhao, Yahui' 'Shao, Kuizhan' 'Zhang, Hengjun' 'Yue, Shumei' _publ_section_title ; Tetraaqua(2,2'-bipyridine)zinc(II) terephthalate ; _journal_issue 2 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first m142 _journal_page_last m144 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Zn (C10 H8 N2) (H2 O)4] (C8 H4 O4)' _chemical_formula_moiety 'C10 H16 N2 O4 Zn 2+, C8 H4 O4 2-' _chemical_formula_sum 'C18 H20 N2 O8 Zn' _chemical_formula_weight 457.73 _chemical_name_common 'C18 H20 N2 O8 Zn' _chemical_name_systematic ; Tetraaqua(2,2'-bipyridine)zinc(II) terephthalate ; _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _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 102.40(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.641(2) _cell_length_b 23.508(5) _cell_length_c 11.134(2) _cell_measurement_reflns_used 13997 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 1.73 _cell_volume 1953.5(7) _computing_cell_refinement PROCESS-AUTO _computing_data_collection 'PROCESS-AUTO (Rigaku, 1998)' _computing_data_reduction 'RAPID-AUTO (Rigaku, 1998)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXTL/PC (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 10.00 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 0.0542 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 4476 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_min 1.73 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.306 _exptl_absorpt_correction_T_max 0.737 _exptl_absorpt_correction_T_min 0.540 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 944 _exptl_crystal_size_max 0.406 _exptl_crystal_size_mid 0.376 _exptl_crystal_size_min 0.234 _refine_diff_density_max 2.245 _refine_diff_density_min -0.575 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 286 _refine_ls_number_reflns 4476 _refine_ls_number_restraints 8 _refine_ls_restrained_S_all 1.103 _refine_ls_R_factor_all 0.0775 _refine_ls_R_factor_gt 0.0598 _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^)(0.1219P)^2^.4398P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1944 _refine_ls_wR_factor_ref 0.2015 _reflns_number_gt 3222 _reflns_number_total 4476 _reflns_threshold_expression I>2\s(I) 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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Zn1 0.71111(6) 0.63942(2) 0.77627(4) 0.02283(19) Uani d . 1 . . Zn O8W 0.4267(5) 0.63496(17) 0.7618(3) 0.0398(8) Uani d D 1 . . O O4 -0.1296(4) 0.69475(15) 1.4610(3) 0.0348(8) Uani d . 1 . . O O7W 0.9920(5) 0.64433(19) 0.7876(3) 0.0433(9) Uani d D 1 . . O O6W 0.7243(5) 0.70105(15) 0.9069(3) 0.0387(8) Uani d D 1 . . O O2 0.2964(5) 0.66631(18) 0.9635(3) 0.0408(9) Uani d . 1 . . O N1 0.7397(5) 0.57087(15) 0.9059(4) 0.0301(8) Uani d . 1 . . N O5W 0.6744(5) 0.69313(14) 0.6297(3) 0.0326(7) Uani d D 1 . . O O3 0.1231(5) 0.66285(18) 1.5811(3) 0.0432(9) Uani d . 1 . . O C10 0.7093(9) 0.5640(2) 0.5447(5) 0.0451(13) Uani d . 1 . . C H20A 0.6891 0.5982 0.5022 0.080 Uiso calc R 1 . . H N2 0.7144(5) 0.56418(16) 0.6649(3) 0.0312(8) Uani d . 1 . . N O1 0.5448(4) 0.69988(14) 1.0846(3) 0.0349(7) Uani d . 1 . . O C17 0.3118(6) 0.6841(2) 1.3916(4) 0.0306(10) Uani d . 1 . . C H36A 0.3810 0.6833 1.4713 0.080 Uiso calc R 1 . . H C20 0.0341(6) 0.68061(17) 1.4817(4) 0.0254(9) Uani d . 1 . . C C19 0.3831(6) 0.68417(18) 1.0655(4) 0.0264(9) Uani d . 1 . . C C15 0.0218(6) 0.6857(2) 1.2528(4) 0.0320(10) Uani d . 1 . . C H32A -0.1025 0.6872 1.2393 0.080 Uiso calc R 1 . . H C16 0.1238(6) 0.68378(17) 1.3723(4) 0.0233(8) Uani d . 1 . . C C11 0.7480(6) 0.51835(19) 0.8605(4) 0.0308(9) Uani d . 1 . . C C12 0.7442(6) 0.51529(19) 0.7271(4) 0.0303(9) Uani d . 1 . . C C1 0.7436(8) 0.5767(2) 1.0266(5) 0.0415(12) Uani d . 1 . . C H11A 0.7367 0.6132 1.0578 0.080 Uiso calc R 1 . . H C13 0.2912(6) 0.68542(17) 1.1718(4) 0.0239(8) Uani d . 1 . . C C18 0.3945(6) 0.6857(2) 1.2920(4) 0.0305(10) Uani d . 1 . . C H35A 0.5189 0.6869 1.3052 0.080 Uiso calc R 1 . . H C14 0.1054(6) 0.6855(2) 1.1535(4) 0.0325(10) Uani d . 1 . . C H33A 0.0362 0.6854 1.0739 0.080 Uiso calc R 1 . . H C4 0.7599(9) 0.4708(2) 0.9366(5) 0.0475(14) Uani d . 1 . . C H14A 0.7657 0.4345 0.9042 0.080 Uiso calc R 1 . . H C7 0.7695(9) 0.4650(2) 0.6667(6) 0.0489(14) Uani d . 1 . . C H17A 0.7906 0.4311 0.7107 0.080 Uiso calc R 1 . . H C9 0.7327(10) 0.5151(3) 0.4792(6) 0.0587(17) Uani d . 1 . . C H19A 0.7276 0.5164 0.3951 0.080 Uiso calc R 1 . . H C2 0.7575(10) 0.5310(3) 1.1070(6) 0.0578(16) Uani d . 1 . . C H12A 0.7627 0.5364 1.1904 0.080 Uiso calc R 1 . . H C8 0.7634(10) 0.4653(3) 0.5431(6) 0.0594(17) Uani d . 1 . . C H18A 0.7801 0.4317 0.5027 0.080 Uiso calc R 1 . . H C3 0.7632(10) 0.4774(3) 1.0586(6) 0.0606(18) Uani d . 1 . . C H13A 0.7693 0.4457 1.1091 0.080 Uiso calc R 1 . . H H7 1.066(9) 0.654(3) 0.852(4) 0.080 Uiso d D 1 . . H H6 0.668(9) 0.700(4) 0.965(5) 0.080 Uiso d D 1 . . H H5 0.749(8) 0.696(3) 0.583(6) 0.080 Uiso d D 1 . . H H4 0.375(11) 0.644(3) 0.690(3) 0.080 Uiso d D 1 . . H H3 1.050(10) 0.650(3) 0.732(6) 0.080 Uiso d D 1 . . H H2 0.377(10) 0.647(3) 0.818(5) 0.080 Uiso d D 1 . . H H1 0.783(9) 0.7315(19) 0.911(7) 0.080 Uiso d D 1 . . H H11 0.626(10) 0.7256(16) 0.620(7) 0.080 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 0.0272(3) 0.0227(3) 0.0203(3) 0.00129(19) 0.00877(18) 0.00109(18) O8W 0.0292(17) 0.061(2) 0.0305(17) 0.0017(16) 0.0096(14) -0.0010(17) O4 0.0336(17) 0.0439(19) 0.0315(17) 0.0144(15) 0.0171(14) 0.0109(14) O7W 0.0254(17) 0.078(3) 0.0287(18) -0.0013(17) 0.0097(14) 0.0018(18) O6W 0.051(2) 0.0325(17) 0.0410(19) -0.0118(16) 0.0294(17) -0.0148(15) O2 0.0386(18) 0.067(2) 0.0198(16) -0.0089(18) 0.0138(13) -0.0075(15) N1 0.034(2) 0.0264(18) 0.033(2) 0.0020(16) 0.0123(16) 0.0050(15) O5W 0.0381(18) 0.0323(17) 0.0327(17) 0.0093(14) 0.0196(14) 0.0103(14) O3 0.0387(19) 0.068(2) 0.0251(17) 0.0103(18) 0.0117(14) 0.0077(16) C10 0.072(4) 0.037(3) 0.029(2) -0.001(3) 0.017(2) -0.002(2) N2 0.040(2) 0.0257(18) 0.0298(19) 0.0007(16) 0.0127(16) -0.0012(15) O1 0.0339(17) 0.0378(17) 0.0377(18) -0.0122(15) 0.0184(14) -0.0107(15) C17 0.030(2) 0.039(2) 0.024(2) -0.0044(19) 0.0088(17) -0.0036(18) C20 0.034(2) 0.026(2) 0.0220(19) 0.0027(17) 0.0184(17) 0.0006(16) C19 0.032(2) 0.024(2) 0.026(2) -0.0020(17) 0.0120(17) -0.0002(16) C15 0.027(2) 0.045(3) 0.025(2) 0.0048(19) 0.0067(17) 0.0020(19) C16 0.026(2) 0.027(2) 0.0202(18) 0.0029(16) 0.0119(15) 0.0014(15) C11 0.033(2) 0.026(2) 0.034(2) 0.0010(18) 0.0070(18) 0.0047(18) C12 0.031(2) 0.024(2) 0.035(2) 0.0008(17) 0.0072(18) -0.0034(18) C1 0.054(3) 0.042(3) 0.031(2) 0.005(2) 0.016(2) 0.007(2) C13 0.029(2) 0.026(2) 0.0186(18) -0.0033(16) 0.0105(15) -0.0002(16) C18 0.025(2) 0.041(3) 0.028(2) -0.0049(19) 0.0113(17) -0.0036(18) C14 0.032(2) 0.044(3) 0.022(2) 0.003(2) 0.0067(17) 0.0002(18) C4 0.066(4) 0.027(2) 0.050(3) 0.004(2) 0.014(3) 0.008(2) C7 0.067(4) 0.027(2) 0.054(3) 0.005(2) 0.016(3) -0.008(2) C9 0.091(5) 0.050(4) 0.040(3) -0.003(3) 0.026(3) -0.012(3) C2 0.079(5) 0.058(4) 0.038(3) 0.007(3) 0.018(3) 0.016(3) C8 0.090(5) 0.041(3) 0.052(3) 0.008(3) 0.024(3) -0.018(3) C3 0.094(5) 0.045(3) 0.043(3) 0.001(3) 0.014(3) 0.022(3) 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 O5W Zn1 O6W . . 96.22(15) yes O5W Zn1 O7W . . 88.71(14) yes O6W Zn1 O7W . . 91.41(15) yes O5W Zn1 N1 . . 169.56(15) yes O6W Zn1 N1 . . 94.11(15) yes O7W Zn1 N1 . . 92.60(15) yes O5W Zn1 O8W . . 90.41(14) yes O6W Zn1 O8W . . 88.98(15) yes O7W Zn1 O8W . . 179.07(14) yes N1 Zn1 O8W . . 88.21(15) yes O5W Zn1 N2 . . 93.67(14) yes O6W Zn1 N2 . . 169.89(15) yes O7W Zn1 N2 . . 86.70(16) yes N1 Zn1 N2 . . 76.08(15) yes O8W Zn1 N2 . . 93.06(15) yes Zn1 O8W H4 . . 109(6) ? Zn1 O8W H2 . . 123(6) ? H4 O8W H2 . . 116(8) ? Zn1 O7W H7 . . 123(6) ? Zn1 O7W H3 . . 130(6) ? H7 O7W H3 . . 103(8) ? Zn1 O6W H6 . . 124(6) ? Zn1 O6W H1 . . 126(6) ? H6 O6W H1 . . 110(8) ? C11 N1 C1 . . 118.6(4) ? C11 N1 Zn1 . . 116.4(3) ? C1 N1 Zn1 . . 125.0(3) ? Zn1 O5W H5 . . 123(5) ? Zn1 O5W H11 . . 130(5) ? H5 O5W H11 . . 100(7) ? N2 C10 C9 . . 123.4(5) ? N2 C10 H20A . . 118.3 ? C9 C10 H20A . . 118.3 ? C10 N2 C12 . . 118.9(4) ? C10 N2 Zn1 . . 125.3(3) ? C12 N2 Zn1 . . 115.3(3) ? C18 C17 C16 . . 120.2(4) ? C18 C17 H36A . . 119.9 ? C16 C17 H36A . . 119.9 ? O3 C20 O4 . . 125.6(4) ? O3 C20 C16 . . 118.4(4) ? O4 C20 C16 . . 116.0(4) ? O2 C19 O1 . . 123.8(4) ? O2 C19 C13 . . 118.3(4) ? O1 C19 C13 . . 117.9(4) ? C14 C15 C16 . . 120.1(4) ? C14 C15 H32A . . 119.9 ? C16 C15 H32A . . 119.9 ? C15 C16 C17 . . 119.3(4) ? C15 C16 C20 . . 120.7(4) ? C17 C16 C20 . . 119.9(4) ? N1 C11 C4 . . 120.7(5) ? N1 C11 C12 . . 115.5(4) ? C4 C11 C12 . . 123.7(4) ? N2 C12 C7 . . 120.4(5) ? N2 C12 C11 . . 116.3(4) ? C7 C12 C11 . . 123.3(4) ? N1 C1 C2 . . 123.2(5) ? N1 C1 H11A . . 118.4 ? C2 C1 H11A . . 118.4 ? C14 C13 C18 . . 119.2(4) ? C14 C13 C19 . . 121.4(4) ? C18 C13 C19 . . 119.4(4) ? C17 C18 C13 . . 120.2(4) ? C17 C18 H35A . . 119.9 ? C13 C18 H35A . . 119.9 ? C13 C14 C15 . . 120.8(4) ? C13 C14 H33A . . 119.6 ? C15 C14 H33A . . 119.6 ? C3 C4 C11 . . 119.9(5) ? C3 C4 H14A . . 120.0 ? C11 C4 H14A . . 120.0 ? C8 C7 C12 . . 120.1(5) ? C8 C7 H17A . . 119.9 ? C12 C7 H17A . . 119.9 ? C8 C9 C10 . . 117.5(5) ? C8 C9 H19A . . 121.2 ? C10 C9 H19A . . 121.2 ? C3 C2 C1 . . 117.5(6) ? C3 C2 H12A . . 121.3 ? C1 C2 H12A . . 121.3 ? C9 C8 C7 . . 119.7(5) ? C9 C8 H18A . . 120.2 ? C7 C8 H18A . . 120.2 ? C4 C3 C2 . . 120.1(5) ? C4 C3 H13A . . 120.0 ? C2 C3 H13A . . 120.0 ? 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 O5W . 2.034(3) yes Zn1 O6W . 2.040(3) yes Zn1 O7W . 2.126(4) yes Zn1 N1 . 2.143(4) yes Zn1 O8W . 2.147(4) yes Zn1 N2 . 2.164(4) yes O8W H4 . 0.84(2) ? O8W H2 . 0.85(2) ? O4 C20 . 1.266(5) ? O7W H7 . 0.84(2) ? O7W H3 . 0.85(2) ? O6W H6 . 0.85(2) ? O6W H1 . 0.84(2) ? O2 C19 . 1.257(5) ? N1 C11 . 1.341(6) ? N1 C1 . 1.345(6) ? O5W H5 . 0.85(2) ? O5W H11 . 0.84(2) ? O3 C20 . 1.240(5) ? C10 N2 . 1.330(6) ? C10 C9 . 1.392(8) ? C10 H20A . 0.9300 ? N2 C12 . 1.336(6) ? O1 C19 . 1.263(6) ? C17 C18 . 1.390(6) ? C17 C16 . 1.406(6) ? C17 H36A . 0.9300 ? C20 C16 . 1.523(5) ? C19 C13 . 1.501(6) ? C15 C14 . 1.391(6) ? C15 C16 . 1.391(6) ? C15 H32A . 0.9300 ? C11 C4 . 1.395(7) ? C11 C12 . 1.481(7) ? C12 C7 . 1.394(7) ? C1 C2 . 1.387(7) ? C1 H11A . 0.9300 ? C13 C14 . 1.390(6) ? C13 C18 . 1.400(6) ? C18 H35A . 0.9300 ? C14 H33A . 0.9300 ? C4 C3 . 1.361(9) ? C4 H14A . 0.9300 ? C7 C8 . 1.368(9) ? C7 H17A . 0.9300 ? C9 C8 . 1.364(9) ? C9 H19A . 0.9300 ? C2 C3 . 1.375(9) ? C2 H12A . 0.9300 ? C8 H18A . 0.9300 ? C3 H13A . 0.9300 ? 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 O7W H7 O2 1_655 0.84(2) 1.95(4) 2.749(5) 159(8) O6W H6 O1 . 0.85(2) 1.78(2) 2.638(5) 178(9) O5W H5 O4 1_654 0.85(2) 1.80(3) 2.643(4) 167(8) O8W H4 O3 1_554 0.84(2) 2.09(6) 2.803(5) 142(8) O7W H3 O3 1_654 0.85(2) 1.90(3) 2.732(5) 166(8) O8W H2 O2 . 0.85(2) 1.90(2) 2.745(5) 170(8) O6W H1 O4 4_675 0.84(2) 1.90(3) 2.706(5) 160(8) O5W H11 O1 4_575 0.84(2) 1.87(2) 2.710(5) 171(8)