#------------------------------------------------------------------------------ #$Date: 2012-10-08 19:35:46 +0300 (Mon, 08 Oct 2012) $ #$Revision: 67905 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/11/45/4114575.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4114575 loop_ _publ_author_name 'Andrew S. Lipton' 'Mark D. Smith' 'Richard D. Adams' 'Paul D. Ellis' _publ_section_title ; 67Zn Solid-State and Single-Crystal NMR Spectroscopy and X-ray Crystal Structure of Zinc Formate Dihydrate ; _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 410 _journal_page_last 414 _journal_volume 124 _journal_year 2002 _chemical_formula_moiety 'C4 H12 O12 Zn2 ' _chemical_formula_sum 'C4 H12 O12 Zn2' _chemical_formula_weight 382.89 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _cell_angle_alpha 90 _cell_angle_beta 97.63(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.703(2) _cell_length_b 7.154(2) _cell_length_c 9.315(2) _cell_measurement_reflns_used 15 _cell_measurement_temperature 293.2 _cell_measurement_theta_max 7.8 _cell_measurement_theta_min 3.6 _cell_volume 574.8(2) _diffrn_ambient_temperature 293.2 _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_orient_matrix_UB_11 -0.08846 _diffrn_orient_matrix_UB_12 0.08932 _diffrn_orient_matrix_UB_13 -0.00080 _diffrn_orient_matrix_UB_21 0.04216 _diffrn_orient_matrix_UB_22 0.04214 _diffrn_orient_matrix_UB_23 0.09984 _diffrn_orient_matrix_UB_31 0.06166 _diffrn_orient_matrix_UB_32 0.09903 _diffrn_orient_matrix_UB_33 -0.04206 _diffrn_radiation_detector 'scintillation counter' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.10460 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 1517 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_min 2.20 _diffrn_standards_decay_% 12.48 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 4.233 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.744 _exptl_absorpt_correction_type ; \DF (DIFABS; Walker & Stuart, 1983) ; _exptl_crystal_density_diffrn 2.212 _exptl_crystal_F_000 384.00 _exptl_crystal_size_max 0.00 _exptl_crystal_size_mid 0.00 _exptl_crystal_size_min 0.00 _refine_diff_density_max 0.38 _refine_diff_density_min -0.37 _refine_ls_extinction_coef 0.0000120(9) _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_goodness_of_fit_all 1.264 _refine_ls_goodness_of_fit_ref 1.264 _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 94 _refine_ls_number_reflns 1081 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0270 _refine_ls_shift/esd_max 0.0012 _refine_ls_shift/esd_mean 0.0004 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00164|Fo|^2^]' _refine_ls_wR_factor_all 0.0572 _refine_ls_wR_factor_ref 0.0572 _reflns_number_gt 1081 _reflns_number_total 1429 _reflns_threshold_expression I>3.00\s(I) _[local]_cod_data_source_file ja011701e.cif _[local]_cod_data_source_block C4H12O12Zn2 _[local]_cod_cif_authors_sg_H-M 'P 21/c ' _[local]_cod_chemical_formula_sum_orig 'C4 H12 O12 Zn2 ' _cod_original_cell_volume 574.9(2) _cod_database_code 4114575 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -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_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag Zn(1) 1.0000 0.0000 1.0000 0.0192(2) 0.500 S Uani d Zn(2) 1.5000 0.5000 1.0000 0.0241(2) 0.500 S Uani d O(1) 1.2091(2) 0.1598(2) 0.9993(2) 0.0275(4) 1.000 . Uani d O(2) 1.4355(2) 0.2219(2) 0.9221(2) 0.0349(5) 1.000 . Uani d O(3) 1.0969(2) -0.1047(2) 1.2026(2) 0.0263(4) 1.000 . Uani d O(4) 1.0893(2) -0.2729(2) 1.4008(2) 0.0264(4) 1.000 . Uani d O(5) 1.7184(2) 0.4753(2) 0.9288(2) 0.0289(5) 1.000 . Uani d O(6) 1.4132(2) 0.6081(3) 0.8017(2) 0.0448(6) 1.000 . Uani d C(1) 1.3237(3) 0.1171(3) 0.9375(3) 0.0293(6) 1.000 . Uani d C(2) 1.0362(3) -0.2243(3) 1.2742(2) 0.0268(5) 1.000 . Uani d H(1) 1.324(4) 0.013(4) 0.900(4) 0.038(9) 1.000 . Uiso d H(2) 0.942(5) -0.301(6) 1.204(4) 0.08(1) 1.000 . Uiso d H(3) 1.7629 0.4018 0.9525 0.063 1.000 . Uiso c H(4) 1.7430 0.5773 0.9396 0.063 1.000 . Uiso c H(5) 1.4891 0.6397 0.7442 0.063 1.000 . Uiso c H(6) 1.3205 0.6041 0.7585 0.063 1.000 . Uiso 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 Zn(1) 0.0219(4) 0.0179(4) 0.0176(3) 0.0004(1) 0.0023(2) -0.0001(1) Zn(2) 0.0216(4) 0.0262(4) 0.0243(4) -0.0008(1) 0.0031(3) 0.0014(1) O(1) 0.0234(8) 0.0287(8) 0.0310(8) -0.0044(7) 0.0060(6) -0.0011(6) O(2) 0.0304(9) 0.0319(9) 0.045(1) -0.0057(7) 0.0144(8) -0.0072(8) O(3) 0.0276(9) 0.0273(8) 0.0237(8) -0.0003(7) 0.0016(7) 0.0056(6) O(4) 0.0293(8) 0.0256(8) 0.0231(8) -0.0035(6) -0.0008(6) 0.0059(6) O(5) 0.0272(9) 0.0258(8) 0.034(1) 0.0028(7) 0.0047(7) 0.0005(6) O(6) 0.026(1) 0.074(2) 0.034(1) 0.0013(9) 0.0022(8) 0.020(1) C(1) 0.028(1) 0.026(1) 0.034(1) -0.0043(9) 0.0040(9) -0.0033(9) C(2) 0.027(1) 0.026(1) 0.026(1) -0.0028(9) -0.0024(8) 0.0045(9) loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn 0 4 0.222 1.431 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 24 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 8 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 24 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 0 0 1 1 1 -3 1 1 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Zn(1) O(1) 180.00 . 3_757 yes O(1) Zn(1) O(3) 87.31(6) . . yes O(1) Zn(1) O(3) 92.69(6) . 3_757 yes O(1) Zn(1) O(4) 92.73(6) . 4_544 yes O(1) Zn(1) O(4) 87.27(6) . 2_757 yes O(1) Zn(1) O(3) 92.69(6) 3_757 . yes O(1) Zn(1) O(3) 87.31(6) 3_757 3_757 yes O(1) Zn(1) O(4) 87.27(6) 3_757 4_544 yes O(1) Zn(1) O(4) 92.73(6) 3_757 2_757 yes O(3) Zn(1) O(3) 180.00 . 3_757 yes O(3) Zn(1) O(4) 89.50(6) . 4_544 yes O(3) Zn(1) O(4) 90.50(6) . 2_757 yes O(3) Zn(1) O(4) 90.50(6) 3_757 4_544 yes O(3) Zn(1) O(4) 89.50(6) 3_757 2_757 yes O(4) Zn(1) O(4) 180.0000(1) 4_544 2_757 yes O(2) Zn(2) O(2) 180.00 . 3_867 yes O(2) Zn(2) O(5) 91.27(6) . . yes O(2) Zn(2) O(5) 88.73(6) . 3_867 yes O(2) Zn(2) O(6) 89.78(9) . . yes O(2) Zn(2) O(6) 90.22(9) . 3_867 yes O(2) Zn(2) O(5) 88.73(6) 3_867 . yes O(2) Zn(2) O(5) 91.27(6) 3_867 3_867 yes O(2) Zn(2) O(6) 90.22(9) 3_867 . yes O(2) Zn(2) O(6) 89.78(9) 3_867 3_867 yes O(5) Zn(2) O(5) 180.00 . 3_867 yes O(5) Zn(2) O(6) 89.28(7) . . yes O(5) Zn(2) O(6) 90.72(7) . 3_867 yes O(5) Zn(2) O(6) 90.72(7) 3_867 . yes O(5) Zn(2) O(6) 89.28(7) 3_867 3_867 yes O(6) Zn(2) O(6) 180.00 . 3_867 yes Zn(1) O(1) C(1) 126.7(2) . . yes Zn(2) O(2) C(1) 133.1(2) . . yes Zn(1) O(3) C(2) 125.3(2) . . yes Zn(1) O(4) C(2) 121.5(1) 2_747 . yes Zn(2) O(5) H(3) 117.8 . . no Zn(2) O(5) H(4) 97.3 . . no H(3) O(5) H(4) 124.3 . . no Zn(2) O(6) H(5) 113.9 . . no Zn(2) O(6) H(6) 128.6 . . no H(5) O(6) H(6) 115.9 . . no O(1) C(1) O(2) 125.8(2) . . yes O(1) C(1) H(1) 118(3) . . no O(2) C(1) H(1) 117(3) . . no O(3) C(2) O(4) 124.3(2) . . yes O(3) C(2) H(2) 111(2) . . no O(4) C(2) H(2) 124(2) . . no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn(1) O(1) 2.150(2) . yes Zn(1) O(1) 2.150(2) 3_757 yes Zn(1) O(3) 2.100(2) . yes Zn(1) O(3) 2.100(2) 3_757 yes Zn(1) O(4) 2.071(2) 4_544 yes Zn(1) O(4) 2.071(2) 2_757 yes Zn(2) O(2) 2.166(2) . yes Zn(2) O(2) 2.166(2) 3_867 yes Zn(2) O(5) 2.102(2) . yes Zn(2) O(5) 2.102(2) 3_867 yes Zn(2) O(6) 2.052(2) . yes Zn(2) O(6) 2.052(2) 3_867 yes O(1) C(1) 1.253(3) . yes O(2) C(1) 1.252(3) . yes O(3) C(2) 1.245(3) . yes O(4) C(2) 1.257(3) . yes O(5) H(3) 0.67 . no O(5) H(4) 0.76 . no O(6) H(5) 0.93 . no O(6) H(6) 0.85 . no C(1) H(1) 0.82(3) . no C(2) H(2) 1.12(4) . no