Dynamic orientational disorder in crystals of fluoroelpasolites, structural refinement of (NH~4~)~3~AlF~6~, (NH~4~)~3~TiOF~5~ and Rb~2~KTiOF~5~
Udovenko, Anatoly A.; Laptash, Natalia M.; Acta Crystallographica Section B 67 (2011) 447–454; doi:10.1107/S0108768111044867

data_2104990
_publ_section_title
;
 Dynamic orientational disorder in crystals of fluoroelpasolites,
 structural refinement of (NH~4~)~3~AlF~6~, (NH~4~)~3~TiOF~5~ and
 Rb~2~KTiOF~5~
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              447
_journal_page_last               454
_journal_paper_doi               10.1107/S0108768111044867
_journal_volume                  67
_journal_year                    2011
_chemical_formula_moiety         '(NH4)3 Ti O F5'
_chemical_formula_sum            'F5 H12 N3 O Ti'
_chemical_formula_weight         213.03
_chemical_name_common            'ammonium oxopentafluorotitanate'
_chemical_name_systematic        'ammonium oxopentafluorotitanate'
_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   difmap
_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                   9.1144(6)
_cell_length_b                   9.1144(6)
_cell_length_c                   9.1144(6)
_cell_measurement_reflns_used    846
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      34.97
_cell_measurement_theta_min      3.87
_cell_volume                     757.15(9)
_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 P4'
_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  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0080
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4778
_diffrn_reflns_theta_full        38.95
_diffrn_reflns_theta_max         38.95
_diffrn_reflns_theta_min         3.87
_exptl_absorpt_coefficient_mu    1.171
_exptl_absorpt_correction_T_max  0.7996
_exptl_absorpt_correction_T_min  0.7057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2.03; Bruker 1999'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.168
_refine_diff_density_min         -0.247
_refine_ls_extinction_coef       0.0176(15)
_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   1.161
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     18
_refine_ls_number_reflns         149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0210
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+0.3720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0625
_reflns_number_gt                149
_reflns_number_total             149
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bp5038.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      Fm-3m
_cod_original_formula_sum        ' H12F5N3OTi '
_cod_database_code               2104990
_cod_database_fobs_code          2104990