#------------------------------------------------------------------------------
#$Date: 2019-11-22 08:26:23 +0200 (Fri, 22 Nov 2019) $
#$Revision: 231197 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/85/2108546.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2108546
loop_
_publ_author_name
'Udovenko, Anatoly A.'
'Slobodyuk, Arseny B.'
'Emelina, Tatiana B.'
'Laptash, Natalia M.'
_publ_section_title
;
 Fluxional seven-coordinated fluorido- and oxofluoridotantalates
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520619013465
_journal_volume                  75
_journal_year                    2019
_chemical_formula_moiety         'F7 Ta, H8 N2'
_chemical_formula_sum            'F7 H8 N2 Ta'
_chemical_formula_weight         350.03
_chemical_name_common            'ammonium heptafluorotantalate'
_chemical_name_systematic        'ammonium heptafluorotantalate'
_space_group_crystal_system      tetragonal
_space_group_IT_number           129
_space_group_name_Hall           '-P 4a 2a'
_space_group_name_H-M_alt        'P 4/n m m :2'
_atom_sites_solution_hydrogens   difmap
_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            2
_cell_length_a                   5.8613(2)
_cell_length_b                   5.8613(2)
_cell_length_c                   10.5817(3)
_cell_measurement_reflns_used    7755
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      40.08
_cell_measurement_theta_min      3.48
_cell_volume                     363.53(2)
_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      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8074
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         40.077
_diffrn_reflns_theta_min         3.851
_exptl_absorpt_coefficient_mu    15.187
_exptl_absorpt_correction_T_max  0.1156
_exptl_absorpt_correction_T_min  0.1156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.198
_exptl_crystal_description       sphere
_exptl_crystal_F_000             316
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_refine_diff_density_max         1.398
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       0.0070(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     30
_refine_ls_number_reflns         712
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0122
_refine_ls_R_factor_gt           0.0122
_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/[σ²(Fo²)+(0.0086P)²+0.8194P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0307
_refine_ls_wR_factor_ref         0.0307
_reflns_Friedel_coverage         0.000
_reflns_number_gt                710
_reflns_number_total             712
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wf5151sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        363.53(3)
_cod_original_sg_symbol_H-M      'P 4/n m m'
_cod_database_code               2108546
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.116
_shelx_estimated_absorpt_t_max   0.116
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, y+1/2, -z'
'x+1/2, -y, -z'
'y+1/2, x+1/2, -z'
'-y, -x, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'
'x, -y-1/2, z'
'-x-1/2, y, z'
'-y-1/2, -x-1/2, z'
'y, x, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ta1 Ta 0.2500 0.2500 0.26030(2) 0.00887(2) Uani 1 8 d S T P
N1 N 0.2500 0.7500 0.5000 0.0142(3) Uani 1 8 d S T P
N2 N 0.2500 0.2500 0.8658(3) 0.0350(8) Uani 1 8 d S T P
F1 F 0.2500 0.2500 0.44913(14) 0.0146(3) Uani 1 8 d S T P
F2 F 0.02111(13) 0.47889(13) 0.30015(14) 0.0341(3) Uani 1 2 d S T P
F3 F 0.1764(6) 0.4341(5) 0.1132(2) 0.0357(8) Uani 0.25 1 d . . P
H1 H 0.2500 0.8478 0.5385 0.074(14) Uiso 1 2 d R . P
H2 H 0.2500 0.2500 0.9357 0.12(4) Uiso 1 8 d R . P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
F3 Ta1 F3 67.50(18) . 13_565
F3 Ta1 F3 73.49(17) . 2
F3 Ta1 F3 73.49(17) 13_565 14_655
F3 Ta1 F3 66.70(17) 3 14_655
F3 Ta1 F3 73.49(17) 3 4
F3 Ta1 F3 67.50(18) 15_665 4
F3 Ta1 F2 86.76(11) . 4
F3 Ta1 F2 86.76(11) 16 4
F3 Ta1 F2 68.73(9) 14_655 4
F3 Ta1 F2 68.73(9) 4 4
F3 Ta1 F2 68.73(9) 13_565 3
F3 Ta1 F2 68.73(9) 3 3
F3 Ta1 F2 86.76(11) 15_665 3
F3 Ta1 F2 86.76(11) 2 3
F2 N1 F2 91.36(4) 12_666 4
F2 N1 F2 64.79(4) 10_666 11_566
F2 N1 F2 89.04(4) 12_666 11_566
F2 N1 F2 89.04(4) 4 3_565
F2 N1 F2 91.36(4) 11_566 3_565
F2 N1 F2 89.04(4) . 2_565
F2 N1 F2 91.36(4) 10_666 2_565
F2 N1 F2 120.56(2) 12_666 2_565
F2 N1 F2 64.79(4) 4 2_565
F2 N1 F2 91.36(4) . 9_566
F2 N1 F2 89.04(4) 10_666 9_566
F2 N1 F2 64.79(4) 12_666 9_566
F2 N1 F1 71.57(3) 4 9_666
F2 N1 F1 71.57(3) 2_565 9_666
F1 N1 F1 91.870(10) 9_666 1_565
F2 N1 H1 87.5 12_666 .
F2 N1 H1 88.7 3_565 .
F2 N1 H1 88.7 2_565 .
F2 N1 H1 87.5 9_566 .
F1 N1 H1 84.0 9_666 .
F1 N1 H1 45.8 1_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ta1 F3 1.943(2) .
Ta1 F3 1.943(2) 13_565
Ta1 F3 1.943(2) 3
Ta1 F3 1.943(2) 15_665
Ta1 F3 1.943(2) 2
Ta1 F3 1.943(2) 16
Ta1 F3 1.943(2) 14_655
Ta1 F3 1.943(2) 4
Ta1 F2 1.9436(11) 4
Ta1 F2 1.9436(11) 3
N1 F2 2.9660(11) .
N1 F2 2.9660(11) 10_666
N1 F2 2.9660(11) 12_666
N1 F2 2.9660(11) 4
N1 F2 2.9660(11) 11_566
N1 F2 2.9660(11) 3_565
N1 F2 2.9660(11) 2_565
N1 F2 2.9660(11) 9_566
N1 F1 2.9797(3) 9_666
N1 F1 2.9797(3) 1_565
N1 H1 0.7033 .
N2 F2 2.852(2) 11_556
N2 F2 2.852(2) 12_666
N2 F2 2.852(2) 10_656
N2 F2 2.852(2) 9_566
N2 F3 2.864(3) 14_656
N2 F3 2.864(3) 4_556
N2 F3 2.864(3) 16_556
N2 F3 2.864(3) 1_556
N2 F3 2.864(3) 15_666
N2 F3 2.864(3) 2_556
N2 H2 0.7397 .
F1 F2 2.4668(16) 3
F1 F2 2.4668(16) 2
F1 F2 2.4668(16) 4
F1 F2 2.4668(16) .
F1 N1 2.9797(3) 9_666
F1 N1 2.9797(3) 9_566
F1 N1 2.9797(3) 1_545
F2 F3 2.194(3) 15_665
F2 F3 2.194(3) .
F2 F3 2.669(3) 3
F2 F3 2.669(3) 14_655
F2 F2 2.6832(15) 4
F2 F2 2.6832(15) 3
F2 N2 2.852(2) 9_566
F3 F3 2.324(6) 2
F3 F2 2.669(3) 4

_cod_database_fobs_code 2108546
