Reconstructive phase transition in (NH~4~)~3~TiF~7~ accompained by the ordering TiF~6~ of octahera
Molokeev, Maxim; Misjul, Sergey V.; Flerov, Igor N.; Laptash, Natalia M.; Acta Crystallographica, Section B: Structural Science, Crystal Engineering and Materials 70 (2014) 924–931; doi:10.1107/s2052520614021192

data_2106652
_publ_section_title
;
 Reconstructive phase transition in (NH~4~)~3~TiF~7~ accompained by
 the ordering TiF~6~ of octahera
;
_journal_coden_ASTM              ACSBDA
_journal_coeditor_code           BP5070
_journal_issue                   6
_journal_name_full
;
 Acta Crystallographica, Section B: Structural Science,
 Crystal Engineering and Materials
;
_journal_page_first              924
_journal_page_last               931
_journal_paper_doi               10.1107/s2052520614021192
_journal_volume                  70
_journal_year                    2014
_chemical_formula_moiety         'F6 Ti, F, 3(H4 N)'
_chemical_formula_sum            'F7 H12 N3 Ti'
_chemical_formula_weight         235.03
_chemical_name_common
;
 Ammonium heptafluorotitanate
;
_chemical_name_systematic
; 
 Ammonium heptafluorotitanate 
;
_space_group_IT_number           128
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4 2n'
_symmetry_space_group_name_H-M   'P 4/m n c'
_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            8
_cell_length_a                   11.9597(19)
_cell_length_b                   11.9597(19)
_cell_length_c                   11.6747(19)
_cell_measurement_reflns_used    1741
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.97
_cell_measurement_theta_min      3.41
_cell_volume                     1669.9(5)
_computing_cell_refinement       'APEX2 (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II 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  0.0748
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13112
_diffrn_reflns_theta_full        26.94
_diffrn_reflns_theta_max         26.94
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    1.096
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1. Bruker AXS Inc., Madison, Wisconsin, USA, 2004
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.870
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bulk
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.0028(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   1.068
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         959
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+3.8962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1524
_reflns_number_gt                483
_reflns_number_total             959
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            NH43TiF7_296K.cif
_cod_data_source_block           z
_cod_depositor_comments
;
 Updated bibliographic information.

 Antanas Vaitkus,
 2019-10-01
;
_cod_original_sg_symbol_Hall
;
-P 4 2n 
;
_cod_original_sg_symbol_H-M      P4/mnc
_cod_database_code               2106652
_cod_database_fobs_code          2106652