#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1101053.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_1101053 _journal_name_full 'Journal of Solid State Chemistry' loop_ _publ_author_name 'Kazuo Eda' 'Kin Chin' 'Noriyuki Sotani' 'M. Stanley Whittingham' _chemical_name_common potassium tetramolybdate _chemical_formula_sum 'K2 Mo4 O13' _chemical_formula_weight 669.96 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'Pbca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 7.5479(15) _cell_length_b 15.391(3) _cell_length_c 18.527(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2152.3(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2673 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 23.26 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 4.1 _exptl_crystal_density_diffrn 4.135 _exptl_crystal_density_method 'pycnometry' _exptl_crystal_F_000 2375 _exptl_absorpt_coefficient_mu 5.296 _exptl_absorpt_correction_type 'SADABS ver. 2.03(Sheldrick)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7520 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 23.33 _reflns_number_total 1553 _reflns_number_gt 1359 _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^)+(0.0564P)^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_extinction_coef ? _refine_ls_number_reflns 1553 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0797 _refine_ls_wR_factor_gt 0.0764 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.001 _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 Mo1 Mo 0.70443(7) 0.36156(3) 0.09816(3) 0.0129(2) Uani 1 1 d . . . Mo2 Mo 0.60621(7) 0.56784(3) 0.10711(3) 0.0116(2) Uani 1 1 d . . . Mo3 Mo 0.92180(7) 0.22263(3) 0.25053(3) 0.0104(2) Uani 1 1 d . . . Mo4 Mo 0.32758(7) 0.43128(3) 0.24364(3) 0.0099(2) Uani 1 1 d . . . K5 K 0.3919(2) 0.47107(10) 0.58442(8) 0.0231(4) Uani 1 1 d . . . K6 K 0.7297(2) 0.28462(10) 0.43230(8) 0.0291(4) Uani 1 1 d . . . O1 O 0.8080(5) 0.3214(2) 0.1848(2) 0.0112(9) Uani 1 1 d . . . O2 O 0.8861(6) 0.3774(3) 0.0431(2) 0.0203(11) Uani 1 1 d . . . O3 O 0.4214(5) 0.5156(3) 0.1959(2) 0.0136(10) Uani 1 1 d . . . O4 O 0.6718(6) 0.6467(2) 0.1808(2) 0.0164(11) Uani 1 1 d . . . O5 O 0.4225(6) 0.6207(3) 0.0758(2) 0.0188(10) Uani 1 1 d . . . O6 O 0.7655(6) 0.5867(3) 0.0434(2) 0.0189(10) Uani 1 1 d . . . O7 O 0.6013(6) 0.2724(3) 0.0635(2) 0.0199(11) Uani 1 1 d . . . O8 O 0.4303(6) 0.3348(3) 0.1934(2) 0.0123(10) Uani 1 1 d . . . O9 O 0.5429(6) 0.4492(3) 0.0746(2) 0.0134(9) Uani 1 1 d . . . O10 O 0.1183(6) 0.4271(3) 0.2064(2) 0.0142(10) Uani 1 1 d . . . O11 O 1.1350(6) 0.2303(3) 0.2151(2) 0.0132(9) Uani 1 1 d . . . O12 O 0.2778(6) 0.4792(2) 0.3334(2) 0.0138(9) Uani 1 1 d . . . O13 O 0.9452(6) 0.1579(3) 0.3236(2) 0.0194(10) 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 Mo1 0.0179(3) 0.0135(3) 0.0072(3) -0.0006(2) -0.0018(2) 0.0022(2) Mo2 0.0147(4) 0.0126(3) 0.0076(3) 0.0005(2) 0.0005(2) 0.0006(2) Mo3 0.0116(4) 0.0117(3) 0.0080(3) 0.0002(2) -0.0003(2) 0.0005(2) Mo4 0.0115(4) 0.0117(3) 0.0065(3) 0.00054(19) 0.0012(2) 0.0005(2) K5 0.0280(9) 0.0243(9) 0.0171(8) -0.0022(7) 0.0012(6) -0.0039(6) K6 0.0339(10) 0.0315(9) 0.0218(9) -0.0025(7) 0.0065(7) -0.0074(7) O1 0.013(2) 0.011(2) 0.010(2) -0.0043(17) -0.0028(17) 0.0006(17) O2 0.026(3) 0.025(3) 0.010(2) 0.000(2) -0.0011(19) 0.004(2) O3 0.014(3) 0.017(2) 0.010(2) 0.0020(18) -0.0009(17) -0.0013(18) O4 0.017(3) 0.015(2) 0.017(3) -0.0023(19) 0.0023(18) 0.0018(18) O5 0.022(3) 0.024(2) 0.011(2) 0.0001(19) -0.0013(19) -0.002(2) O6 0.022(3) 0.020(2) 0.015(2) -0.001(2) 0.002(2) -0.0001(19) O7 0.032(3) 0.018(2) 0.010(2) -0.0016(18) -0.003(2) 0.004(2) O8 0.019(3) 0.011(2) 0.007(2) 0.0017(17) 0.0032(17) 0.0039(18) O9 0.019(2) 0.015(2) 0.006(2) -0.0010(17) -0.0026(18) -0.0037(19) O10 0.014(2) 0.018(2) 0.010(2) 0.0009(18) -0.0016(19) -0.0006(18) O11 0.018(2) 0.011(2) 0.011(2) -0.0016(18) -0.0004(19) -0.0019(18) O12 0.015(2) 0.015(2) 0.012(2) 0.0012(18) 0.0025(19) 0.0009(17) O13 0.026(3) 0.020(2) 0.013(2) 0.0055(19) 0.0000(19) 0.000(2)