Crystal structure and phase transition in (NH~4~)~3~WO~2~F~5~: from dynamic to static orientational disorder
Udovenko, Anatoly; Laptash, Natalia; Acta Crystallographica Section B 71 (2015) 478–483; doi:10.1107/S2052520615010835

data_2106623
_publ_section_title
;
 Crystal structure and phase transition in (NH~4~)~3~WO~2~F~5~: from
 dynamic to static orientational disorder
;
_journal_coeditor_code           BP5078
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              478
_journal_page_last               483
_journal_paper_doi               10.1107/S2052520615010835
_journal_volume                  71
_journal_year                    2015
_chemical_formula_moiety         'F4 W O2, F, 3(H4 N)'
_chemical_formula_sum            'F5 H12 N3 O2 W'
_chemical_formula_weight         370.98
_space_group_IT_number           205
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_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            8
_cell_length_a                   11.9635(7)
_cell_length_b                   11.9635(7)
_cell_length_c                   11.9635(7)
_cell_measurement_reflns_used    868
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      32.99
_cell_measurement_theta_min      1.70
_cell_volume                     1712.28(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0101
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27085
_diffrn_reflns_theta_full        32.99
_diffrn_reflns_theta_max         32.99
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    13.562
_exptl_absorpt_correction_T_max  0.1939
_exptl_absorpt_correction_T_min  0.1939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.878
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sphere
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.904
_refine_diff_density_min         -1.317
_refine_ls_extinction_coef       0.00054(7)
_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   0.979
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         1079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0310P)^2^+14.1528P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.1009
_reflns_number_gt                696
_reflns_number_total             1134
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bp5078sup1.cif
_cod_data_source_block           193K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/IUCr/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/IUCr/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_original_sg_symbol_Hall     '-P 2ac 2ab'
_cod_original_sg_symbol_H-M      Pa-3
_cod_original_formula_sum        'F5 H12 N3 O2 W '
_cod_database_code               2106623