#------------------------------------------------------------------------------ #$Date: 2015-01-27 19:58:39 +0000 (Tue, 27 Jan 2015) $ #$Revision: 130149 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/01/4000171.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_4000171 loop_ _publ_author_name 'Sykora, Richard E.' 'Ok, Kang Min' 'Halasyamani, P. Shiv' 'Wells, Daniel M.' 'Albrecht-Schmitt, T. E.' _journal_name_full 'Chemistry of Materials' _journal_year 2002 _chemical_formula_structural NH4[(VO)2(IO3)3O2] _chemical_formula_sum 'H0 I3 N O13 V2' _chemical_formula_weight 704.59 _space_group_IT_number 46 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'I 2 -2a' _symmetry_space_group_name_H-M 'I m a 2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 14.099(2) _cell_length_b 10.2138(13) _cell_length_c 8.0510(10) _cell_measurement_reflns_used all _cell_measurement_temperature 193(2) _cell_measurement_theta_max 28.33 _cell_measurement_theta_min 2.46 _cell_volume 1159.4(3) _diffrn_ambient_temperature 193(2) _diffrn_measurement_device 'Bruker APEX' _diffrn_measurement_method '0.3 wide w/ exposures' _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 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 3328 _diffrn_reflns_theta_max 28.33 _diffrn_reflns_theta_min 2.46 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count na _diffrn_standards_interval_time na _diffrn_standards_number na _exptl_absorpt_coefficient_mu 9.672 _exptl_absorpt_correction_T_max '0.663349 ratio of min/max' _exptl_absorpt_correction_T_min '0.663349 ratio of min/max' _exptl_absorpt_correction_type 'multiscan (SADABS)' _exptl_crystal_colour brown _exptl_crystal_density_diffrn 4.037 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 1264 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.072 _exptl_crystal_size_min 0.034 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.46(9) _refine_ls_extinction_coef 0.00252(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_all 1.167 _refine_ls_goodness_of_fit_obs 1.170 _refine_ls_hydrogen_treatment 'not located' _refine_ls_matrix_type full _refine_ls_number_parameters 95 _refine_ls_number_reflns 1152 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.167 _refine_ls_restrained_S_obs 1.169 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_obs 0.0353 _refine_ls_shift/esd_max -0.904 _refine_ls_shift/esd_mean 0.018 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+45.4962P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.0823 _refine_ls_wR_factor_obs 0.0822 _reflns_number_observed 1143 _reflns_number_total 1152 _reflns_observed_criterion >2sigma(I) _[local]_cod_cif_authors_sg_H-M Ima2 _cod_database_code 4000171 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y, z' '-x+1/2, y, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1, -y+1/2, z+1/2' '-x+1, y+1/2, z+1/2' 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 V1 0.0333(13) 0.0077(9) 0.0188(11) 0.0013(8) 0.0180(8) -0.0002(9) I1 0.0097(3) 0.0114(3) 0.0116(3) -0.0035(3) 0.0006(3) 0.0001(3) I2 0.0095(4) 0.0081(4) 0.0087(4) 0.0016(4) 0.000 0.000 N1 0.027(8) 0.014(7) 0.055(12) 0.007(10) 0.000 0.000 O1 0.030(5) 0.014(4) 0.014(4) 0.006(4) 0.004(4) 0.000(4) O7 0.019(6) 0.025(6) 0.000(6) 0.000 0.000 -0.008(5) O4 0.016(6) 0.013(5) 0.005(5) -0.004(5) 0.000 0.000 O5 0.014(4) 0.013(4) 0.015(4) 0.004(3) 0.000(4) -0.010(4) O6 0.015(4) 0.017(4) 0.020(4) -0.003(3) 0.002(4) 0.004(4) O8 0.014(6) 0.012(5) 0.011(5) 0.005(5) 0.000 0.000 O3 0.016(4) 0.009(3) 0.019(4) -0.005(3) -0.002(4) -0.004(3) O2 0.013(4) 0.012(4) 0.023(5) -0.003(3) 0.010(4) 0.003(3) 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group V1 V 0.3714(2) 0.0157(2) -0.2215(4) 0.0199(6) Uani 1 d . . I1 I 0.50771(4) -0.24561(7) -0.4466(2) 0.0109(2) Uani 1 d . . I2 I 0.2500 -0.22452(8) 0.02342(8) 0.0088(2) Uani 1 d S . N1 N 0.2500 0.3934(15) -0.1886(32) 0.032(4) Uani 1 d S . O1 O 0.5304(8) -0.3389(8) -0.2621(12) 0.019(2) Uani 1 d . . O7 O 0.5000 0.0000 -0.1643(14) 0.015(3) Uani 1 d S . O4 O 0.2500 -0.1592(11) 0.2305(15) 0.011(2) Uani 1 d S . O5 O 0.3485(7) -0.1256(8) -0.0563(11) 0.014(2) Uani 1 d . . O6 O 0.3466(7) 0.1365(8) -0.0986(11) 0.017(2) Uani 1 d . . O8 O 0.2500 -0.0128(11) -0.3088(17) 0.013(2) Uani 1 d S . O3 O 0.5976(6) -0.1156(7) -0.4207(11) 0.015(2) Uani 1 d . . O2 O 0.4029(7) -0.1527(8) -0.3884(11) 0.016(2) Uani 1 d . .