#------------------------------------------------------------------------------ #$Date: 2015-01-27 19:58:39 +0000 (Tue, 27 Jan 2015) $ #$Revision: 130149 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100986.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_1100986 _chemical_formula_sum 'K2 Mo4 O13' _chemical_formula_weight 669.96 _chemical_name_common 'potassium tetramolybdate' _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 107.104(4) _cell_angle_beta 102.884(5) _cell_angle_gamma 109.765(5) _cell_formula_units_Z 2 _cell_length_a 7.977(2) _cell_length_b 8.346(2) _cell_length_c 10.018(3) _cell_measurement_reflns_used 892 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.892 _cell_measurement_theta_min 2.832 _cell_volume 560.0(3) _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _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 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 3202 _diffrn_reflns_theta_max 27.22 _diffrn_reflns_theta_min 2.28 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 5.089 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type 'SADABS ver. 2.03(Sheldrick)' _exptl_absorpt_process_details ? _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 3.973 _exptl_crystal_density_meas 3.98(5) _exptl_crystal_density_method pycnometry _exptl_crystal_description needle _exptl_crystal_F_000 594 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 172 _refine_ls_number_reflns 2172 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0355 _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^)+(0.0481P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0875 _refine_ls_wR_factor_ref 0.0935 _reflns_number_gt 1711 _reflns_number_total 2172 _reflns_threshold_expression >2sigma(I) _[local]_cod_cif_authors_sg_H-M P-1 _cod_database_code 1100986 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 0.22480(9) 0.89721(8) 0.27148(6) 0.01149(17) Uani 1 1 d . . . Mo2 Mo 0.18990(8) 0.99621(8) -0.04826(6) 0.01047(17) Uani 1 1 d . . . Mo3 Mo 0.17060(8) 0.59255(8) -0.06205(6) 0.01160(17) Uani 1 1 d . . . Mo4 Mo -0.22353(8) 0.70302(8) -0.29193(6) 0.01128(17) Uani 1 1 d . . . K1 K 0.2545(3) 0.7153(2) 0.56403(19) 0.0235(4) Uani 1 1 d . . . K2 K 0.6893(3) 0.7390(3) 0.3091(2) 0.0300(4) Uani 1 1 d . . . O1 O 0.4120(7) 0.8589(7) 0.3457(6) 0.0205(12) Uani 1 1 d . . . O2 O 0.1009(7) 0.8848(7) 0.3898(5) 0.0197(11) Uani 1 1 d . . . O3 O 0.3639(7) 1.1581(6) 0.3383(5) 0.0158(11) Uani 1 1 d . . . O4 O 0.0420(7) 0.9887(6) 0.1369(5) 0.0113(10) Uani 1 1 d . . . O5 O 0.2958(7) 0.8698(6) 0.0584(5) 0.0128(10) Uani 1 1 d . . . O6 O 0.0513(7) 0.6366(6) 0.1179(5) 0.0131(10) Uani 1 1 d . . . O7 O 0.3224(7) 1.2221(6) 0.0875(5) 0.0156(11) Uani 1 1 d . . . O8 O 0.2818(7) 0.9871(7) -0.1859(5) 0.0178(11) Uani 1 1 d . . . O9 O -0.0217(7) 0.7141(6) -0.1430(5) 0.0134(10) Uani 1 1 d . . . O10 O 0.3464(8) 0.5610(7) 0.0397(6) 0.0219(12) Uani 1 1 d . . . O11 O 0.2035(8) 0.5574(7) -0.2287(6) 0.0234(13) Uani 1 1 d . . . O12 O -0.3998(7) 0.4848(7) -0.3532(5) 0.0182(11) Uani 1 1 d . . . O13 O -0.1270(8) 0.6900(7) -0.4291(5) 0.0211(12) 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 0.0154(3) 0.0092(3) 0.0088(3) 0.0025(2) 0.0028(3) 0.0060(3) Mo2 0.0110(3) 0.0092(3) 0.0113(3) 0.0037(2) 0.0041(2) 0.0047(2) Mo3 0.0137(3) 0.0092(3) 0.0131(3) 0.0037(2) 0.0064(3) 0.0059(3) Mo4 0.0133(3) 0.0081(3) 0.0098(3) 0.0016(2) 0.0019(3) 0.0047(3) K1 0.0264(9) 0.0237(9) 0.0214(9) 0.0080(7) 0.0106(8) 0.0115(8) K2 0.0282(10) 0.0332(11) 0.0458(12) 0.0252(9) 0.0210(9) 0.0200(9) O10 0.023(3) 0.019(3) 0.026(3) 0.009(2) 0.009(3) 0.012(3) O6 0.017(3) 0.012(2) 0.011(2) 0.004(2) 0.006(2) 0.006(2) O5 0.014(3) 0.008(2) 0.014(3) 0.002(2) 0.003(2) 0.006(2) O1 0.023(3) 0.018(3) 0.020(3) 0.004(2) 0.006(2) 0.012(2) O2 0.021(3) 0.019(3) 0.019(3) 0.005(2) 0.007(2) 0.010(2) O7 0.013(3) 0.014(3) 0.017(3) 0.003(2) 0.006(2) 0.006(2) O13 0.025(3) 0.022(3) 0.017(3) 0.006(2) 0.009(2) 0.012(3) O12 0.020(3) 0.018(3) 0.012(3) 0.005(2) 0.003(2) 0.006(2) O8 0.021(3) 0.017(3) 0.017(3) 0.006(2) 0.008(2) 0.010(2) O11 0.035(3) 0.021(3) 0.023(3) 0.009(2) 0.019(3) 0.015(3) O9 0.013(2) 0.012(2) 0.016(3) 0.009(2) 0.003(2) 0.005(2) O3 0.015(3) 0.014(3) 0.017(3) 0.006(2) 0.001(2) 0.007(2) O4 0.014(2) 0.004(2) 0.012(2) -0.0009(19) 0.003(2) 0.004(2)