Orientational disorder and phase transitions in crystals of (NH~4~)~2~NbOF~5~
Udovenko, Anatoly A.; Laptash, Natalia M.; Acta Crystallographica Section B 64 (2008) 527–533; doi:10.1107/S0108768108021289

data_2104205
_publ_section_title
;
 Orientational disorder and phase transitions in crystals of
 (NH~4~)~2~NbOF~5~
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              527
_journal_page_last               533
_journal_paper_doi               10.1107/S0108768108021289
_journal_volume                  64
_journal_year                    2008
_chemical_formula_moiety         'F5 Nb O, 2(H4 N)'
_chemical_formula_sum            'F5 H8 N2 Nb O'
_chemical_formula_weight         239.99
_chemical_name_common            'ammonium pentafluorooxoniobate(V)'
_chemical_name_systematic        'ammonium pentafluorooxoniobate(V)'
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'I -2ya'
_symmetry_space_group_name_H-M   'I 1 a 1'
_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                 90.110(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.3384(14)
_cell_length_b                   5.9804(6)
_cell_length_c                   14.4524(14)
_cell_measurement_reflns_used    944
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      39.01
_cell_measurement_theta_min      2.00
_cell_volume                     1239.3(2)
_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      198(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker Smart 1000 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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16431
_diffrn_reflns_theta_full        39.01
_diffrn_reflns_theta_max         38.01
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    1.978
_exptl_absorpt_correction_T_max  0.5702
_exptl_absorpt_correction_T_min  0.5702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2.03; Bruker 1999'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sphere
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.32
_exptl_crystal_size_rad          0.16
_refine_diff_density_max         0.891
_refine_diff_density_min         -1.276
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.11(10)
_refine_ls_extinction_coef       0.02053(17)
_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   1.054
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         6354
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0226
_refine_ls_shift/su_max          0.108
_refine_ls_shift/su_mean         0.028
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0199P)^2^+1.2051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0591
_reflns_number_gt                5715
_reflns_number_total             6354
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bp5012.cif
_cod_data_source_block           198K
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      Ia
_cod_original_formula_sum        ' F5 H8 N2 Nb O'
_cod_database_code               2104205
_cod_database_fobs_code          2104205