Orientational disorder in crystals of (NH~4~)~3~MoO~3~F~3~ and (NH~4~)~3~WO~3~F~3~
Udovenko, A. A.; Laptash, N. M.; Acta Crystallographica Section B 64 (2008) 305–311; doi:10.1107/S0108768108010288

data_2104130
_publ_section_title
;
 Orientational disorder in crystals of (NH~4~)~3~MoO~3~F~3~ and
 (NH~4~)~3~WO~3~F~3~
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              305
_journal_page_last               311
_journal_paper_doi               10.1107/S0108768108010288
_journal_volume                  64
_journal_year                    2008
_chemical_formula_moiety         '(F3 O3 Mo), 3(NH4)'
_chemical_formula_sum            'F3 H12 Mo N3 O3'
_chemical_formula_weight         255.07
_chemical_name_common            'ammonium trifluorotrioxomolybdate(VI)'
_chemical_name_systematic        'ammonium trifluorotrioxomolybdate(VI)'
_space_group_IT_number           225
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1295(3)
_cell_length_b                   9.1295(3)
_cell_length_c                   9.1295(3)
_cell_measurement_reflns_used    787
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      30.70
_cell_measurement_theta_min      3.87
_cell_volume                     760.92(4)
_computing_cell_refinement       'Bruker SAINT v6.02a (Bruker, 2000)'
_computing_data_collection       'Bruker Smart v5.054 (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT v6.02a (Bruker, 2000)'
_computing_molecular_graphics    'Bruker SHELXTL v5.1 (Bruker, 1998)'
_computing_publication_material  'Bruker SHELXTL v5.1 (Bruker, 1998)'
_computing_structure_refinement  'Bruker SHELXTL v5.1 (Bruker, 1998)'
_computing_structure_solution    'Bruker SHELXTL v5.1 (Bruker, 1998)'
_diffrn_ambient_temperature      297(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       '\w 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  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0118
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2016
_diffrn_reflns_theta_full        30.70
_diffrn_reflns_theta_max         30.70
_diffrn_reflns_theta_min         3.87
_exptl_absorpt_coefficient_mu    1.744
_exptl_absorpt_correction_T_max  0.7558
_exptl_absorpt_correction_T_min  0.5968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2.03; Bruker 1999'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.165
_refine_diff_density_min         -0.204
_refine_ls_extinction_coef       0.0417(6)
_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_ref   1.243
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     18
_refine_ls_number_reflns         89
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.243
_refine_ls_R_factor_all          0.0180
_refine_ls_R_factor_gt           0.0174
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+0.4600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0526
_reflns_number_gt                85
_reflns_number_total             89
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bp5011.cif
_cod_data_source_block           I
_cod_original_formula_sum        ' F3 H12 Mo N3 O3'
_cod_database_code               2104130
_cod_database_fobs_code          2104130