#------------------------------------------------------------------------------ #$Date: 2008-01-26 15:05:32 +0200 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4000226.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_4000226 _journal_name_full 'Chemistry of Materials' _journal_year 2003 _publ_section-title ; Structural Characterization of the Industrially Important Zinc Borate, Zn[B~3~O~4~(OH)~3~] ; loop_ _publ_author_name 'Schubert, David M.' 'Alam, Fazlul' 'Visi, Mandana Z.' 'Knobler, Carolyn B.' _chemical_name_common ; zinc borate ; _chemical_formula_moiety 'Zn B3 O4 (OH)3' _chemical_formula_sum 'H12 B12 O28 Zn4' _chemical_formula_weight 851.30 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.8452(16) _cell_length_b 9.798(2) _cell_length_c 7.6970(18) _cell_angle_alpha 90.00 _cell_angle_beta 106.966(4) _cell_angle_gamma 90.00 _cell_volume 493.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 559 _cell_measurement_2theta_min 8.16 _cell_measurement_2theta_max 53.60 _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 2.863 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 416 _exptl_absorpt_coefficient_mu 4.949 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Bruker software' _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART ccd' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_decay_% none _diffrn_reflns_number 3045 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 28.26 _reflns_number_total 1173 _reflns_number_gt 941 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 1173 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0226 _refine_ls_wR_factor_ref 0.0528 _refine_ls_wR_factor_gt 0.0504 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.06883(5) 0.71619(3) 0.84382(4) 0.01227(10) Uani 1 1 d . . . O1 O -0.0437(3) 0.79026(18) 1.0319(2) 0.0110(4) Uani 1 1 d . . . O2 O -0.3100(3) 0.92158(19) 1.0883(2) 0.0137(4) Uani 1 1 d . . . O3 O 0.0403(3) 0.96357(18) 1.2682(2) 0.0120(4) Uani 1 1 d . . . O4 O 0.1103(3) 0.72302(19) 1.3364(2) 0.0131(4) Uani 1 1 d . . . O5 O 0.2590(3) 0.5673(2) 0.9024(2) 0.0151(4) Uani 1 1 d . . . H5 H 0.304(5) 0.548(3) 0.980(5) 0.020 Uiso 1 1 d . . . O6 O 0.2094(3) 0.86342(19) 0.7595(3) 0.0138(4) Uani 1 1 d . . . H6 H 0.319(5) 0.846(3) 0.781(4) 0.018 Uiso 1 1 d . . . O7 O -0.1930(3) 0.6535(2) 0.6798(3) 0.0145(4) Uani 1 1 d . . . H7 H -0.179(5) 0.604(3) 0.621(4) 0.019 Uiso 1 1 d . . . B3 B 0.1048(4) 0.8367(3) 1.2114(4) 0.0113(6) Uani 1 1 d . . . B1 B -0.2477(5) 0.8273(3) 0.9859(4) 0.0117(6) Uani 1 1 d . . . B2 B -0.1722(5) 0.9874(3) 1.2503(4) 0.0115(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01157(16) 0.01106(16) 0.01410(16) -0.00069(13) 0.00364(11) 0.00030(13) O1 0.0100(9) 0.0122(9) 0.0096(9) -0.0007(7) 0.0014(7) 0.0015(7) O2 0.0110(9) 0.0145(10) 0.0135(10) -0.0051(7) 0.0003(7) 0.0010(7) O3 0.0102(9) 0.0103(9) 0.0137(9) -0.0023(7) 0.0007(7) 0.0007(7) O4 0.0108(9) 0.0134(9) 0.0135(9) 0.0041(8) 0.0008(7) -0.0016(7) O5 0.0196(11) 0.0153(10) 0.0098(10) 0.0016(8) 0.0032(9) 0.0064(8) O6 0.0110(9) 0.0109(10) 0.0198(10) 0.0000(8) 0.0049(8) 0.0003(8) O7 0.0118(9) 0.0160(10) 0.0155(10) -0.0064(8) 0.0039(8) -0.0012(8) B3 0.0105(14) 0.0136(14) 0.0080(14) 0.0000(11) 0.0001(11) -0.0011(11) B1 0.0125(15) 0.0110(14) 0.0106(14) 0.0006(11) 0.0017(12) -0.0001(11) B2 0.0113(14) 0.0104(14) 0.0117(15) -0.0003(11) 0.0019(11) -0.0012(11)