Ammonium tantalum oxide fluorides: new features of dynamic disorder
Udovenko, Anatoly A.; Laptash, Natalia M.; Acta Crystallographica Section B 75 (2019) –; doi:10.1107/S2052520619013994

data_2108544
_publ_section_title
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 Ammonium tantalum oxide fluorides: new features of dynamic disorder
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520619013994
_journal_volume                  75
_journal_year                    2019
_chemical_formula_moiety         '(N H4)2.75, [Ta F6.75 O0.125], F0.75'
_chemical_formula_sum            'F7.5 H11 N2.75 O0.125 Ta'
_chemical_formula_weight         375.44
_chemical_name_common            'ammonium  tantalum oxide fluoride'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.50180(10)
_cell_length_b                   8.57360(10)
_cell_length_c                   33.4597(4)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.94
_cell_measurement_theta_min      2.43
_cell_volume                     3299.52(6)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
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_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         1.872
_exptl_absorpt_coefficient_mu    13.410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.023
_exptl_crystal_description       plate
_exptl_crystal_F_000             2750
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   0.746
_exptl_transmission_factor_min   0.382
_refine_diff_density_max         1.792
_refine_diff_density_min         -1.315
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       0.00053(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         5102
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+8.7205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4364
_reflns_number_total             5102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wf5152sup1.cif
_cod_data_source_block           III
_cod_original_formula_sum        'F7.5 O0.125 H11 N2.75 Ta'
_cod_database_code               2108544
_shelx_estimated_absorpt_t_min   0.134
_shelx_estimated_absorpt_t_max   0.554
_shelx_res_checksum              83894
_shelx_hkl_checksum              63327
_cod_database_fobs_code 2108544