#------------------------------------------------------------------------------
#$Date: 2019-11-22 08:25:09 +0200 (Fri, 22 Nov 2019) $
#$Revision: 231196 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/85/2108543.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_2108543
loop_
_publ_author_name
'Udovenko, Anatoly A.'
'Laptash, Natalia M.'
_publ_section_title
;
 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)3, [Ta F6.83 O0.17], F0.83'
_chemical_formula_sum            'F7.66 H12 N3 O0.17 Ta'
_chemical_formula_weight         383.91
_chemical_name_common            'ammonium  tantalum oxide fluoride'
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m :H'
_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                120
_cell_formula_units_Z            6
_cell_length_a                   8.54140(10)
_cell_length_b                   8.54140(10)
_cell_length_c                   41.4381(4)
_cell_measurement_reflns_used    9478
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      34.02
_cell_measurement_theta_min      4.41
_cell_volume                     2618.11(5)
_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 0.934
_diffrn_measured_fraction_theta_max 0.962
_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  0.0283
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 0.934
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            16286
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.078
_diffrn_reflns_theta_min         4.773
_exptl_absorpt_coefficient_mu    12.682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.922
_exptl_crystal_description       prism
_exptl_crystal_F_000             2118
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.160
_exptl_transmission_factor_max   0.7467
_exptl_transmission_factor_min   0.6067
_refine_diff_density_max         1.405
_refine_diff_density_min         -1.366
_refine_diff_density_rms         0.191
_refine_ls_extinction_coef       0.00028(8)
_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   1.188
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1353
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.228
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0520P)²+12.6611P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1014
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1257
_reflns_number_total             1353
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wf5152sup1.cif
_cod_data_source_block           II
_cod_original_cell_volume        2618.11(7)
_cod_database_code               2108543
_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   0.115
_shelx_estimated_absorpt_t_max   0.236
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
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 0.6667 0.3333 0.03301(14) 0.0351(14) Uani 0.65(4) 6 d S T P
Ta11 Ta 0.6317(12) 0.331(3) 0.0390(4) 0.0359(19) Uani 0.058(6) 1 d . . P
Ta2 Ta 0.0000 0.0000 0.13224(19) 0.0284(6) Uani 0.52(5) 6 d S T P
Ta22 Ta 0.0000 0.0000 0.1281(4) 0.0374(12) Uani 0.48(5) 6 d S T P
F1 F 0.6667 0.3333 -0.0113(3) 0.097(4) Uani 1 6 d DS T P
F2 F 0.6667 0.3333 0.0861(4) 0.120(7) Uani 0.7353 6 d DS T P
F3 F 0.4032(9) 0.2016(5) 0.02183(19) 0.116(3) Uani 1 2 d DS T P
F4 F 0.5381(6) 0.0762(12) 0.0532(3) 0.109(3) Uani 0.7575 2 d DS T P
F5 F -0.1004(4) 0.1004(4) 0.09892(12) 0.0727(14) Uani 1 2 d S T P
F6 F 0.1280(4) 0.2560(8) 0.14164(15) 0.0847(18) Uani 1 2 d S T P
F7 F 0.0000 0.0000 0.1781(2) 0.090(4) Uani 1 6 d S T P
F8 F 0.3333 0.6667 0.2454(4) 0.093(4) Uani 1 6 d S T P
F9 F 0.3333 0.6667 0.1667 0.058(5) Uani 0.4507 12 d S T P
F10 F 0.0000 0.0000 0.0000 0.082(5) Uani 0.8856 12 d S T P
N1 N 0.1682(5) 0.8318(5) 0.21132(18) 0.0613(16) Uani 1 2 d S T P
N2 N 0.6775(14) 0.8387(7) 0.04667(19) 0.091(4) Uani 1 2 d S T P
H1 H 0.2231 0.7769 0.2230 0.068 Uiso 1 2 d S . 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
Ta11 Ta1 Ta11 39(6) 23_655 2_655
Ta11 Ta1 Ta11 50(5) 23_655 3_665
Ta11 Ta1 Ta11 82(3) 2_655 3_665
Ta11 Ta1 Ta11 82(3) 23_655 24
Ta11 Ta1 Ta11 50(5) 2_655 24
Ta11 Ta1 Ta11 98(4) 3_665 24
Ta11 Ta1 Ta11 82(3) 23_655 22_665
Ta11 Ta1 Ta11 98(4) 2_655 22_665
Ta11 Ta1 Ta11 39(6) 3_665 22_665
Ta11 Ta1 Ta11 82(3) 24 22_665
Ta11 Ta1 F1 130.8(18) 23_655 .
Ta11 Ta1 F1 130.8(18) 2_655 .
Ta11 Ta1 F1 130.8(18) 3_665 .
Ta11 Ta1 F1 130.8(18) 24 .
Ta11 Ta1 F1 130.8(18) 22_665 .
Ta11 Ta1 F3 59(2) 23_655 2_655
Ta11 Ta1 F3 59(2) 2_655 2_655
Ta11 Ta1 F3 101(3) 3_665 2_655
Ta11 Ta1 F3 101(3) 24 2_655
Ta11 Ta1 F3 140(3) 22_665 2_655
F1 Ta1 F3 76.6(3) . 2_655
Ta11 Ta1 F3 140(3) 23_655 .
Ta11 Ta1 F3 101(3) 2_655 .
Ta11 Ta1 F3 140(3) 3_665 .
Ta11 Ta1 F3 59(2) 24 .
Ta11 Ta1 F3 101(3) 22_665 .
F1 Ta1 F3 76.6(3) . .
F3 Ta1 F3 114.8(2) 2_655 .
Ta11 Ta1 F3 101(3) 23_655 3_665
Ta11 Ta1 F3 140(3) 2_655 3_665
Ta11 Ta1 F3 59(2) 3_665 3_665
Ta11 Ta1 F3 140(3) 24 3_665
Ta11 Ta1 F3 59(2) 22_665 3_665
F1 Ta1 F3 76.6(3) . 3_665
F3 Ta1 F3 114.8(2) 2_655 3_665
F3 Ta1 F3 114.8(2) . 3_665
Ta11 Ta1 F2 49.2(18) 23_655 .
Ta11 Ta1 F2 49.2(18) 2_655 .
Ta11 Ta1 F2 49.2(18) 3_665 .
Ta11 Ta1 F2 49.2(18) 24 .
Ta11 Ta1 F2 49.2(18) 22_665 .
F1 Ta1 F2 180.0 . .
F3 Ta1 F2 103.4(3) 2_655 .
F3 Ta1 F2 103.4(3) . .
F3 Ta1 F2 103.4(3) 3_665 .
Ta11 Ta1 F4 33(3) 23_655 2_655
Ta11 Ta1 F4 72(3) 2_655 2_655
Ta11 Ta1 F4 33(3) 3_665 2_655
Ta11 Ta1 F4 110.9(19) 24 2_655
Ta11 Ta1 F4 72(3) 22_665 2_655
F1 Ta1 F4 113.8(3) . 2_655
F3 Ta1 F4 69.40(15) 2_655 2_655
F3 Ta1 F4 169.6(5) . 2_655
F3 Ta1 F4 69.40(15) 3_665 2_655
F2 Ta1 F4 66.2(3) . 2_655
Ta11 Ta1 F4 72(3) 23_655 .
Ta11 Ta1 F4 33(3) 2_655 .
Ta11 Ta1 F4 110.9(19) 3_665 .
Ta11 Ta1 F4 33(3) 24 .
Ta11 Ta1 F4 110.9(19) 22_665 .
F1 Ta1 F4 113.8(3) . .
F3 Ta1 F4 69.40(15) 2_655 .
F3 Ta1 F4 69.40(15) . .
F3 Ta1 F4 169.6(5) 3_665 .
F2 Ta1 F4 66.2(3) . .
F4 Ta1 F4 104.8(4) 2_655 .
Ta11 Ta11 Ta11 120.00(14) 24 22_665
Ta11 Ta11 Ta11 94(4) 24 3_665
Ta11 Ta11 Ta11 26(4) 22_665 3_665
Ta11 Ta11 Ta11 34(4) 24 2_655
Ta11 Ta11 Ta11 86(4) 22_665 2_655
Ta11 Ta11 Ta11 60.000(3) 3_665 2_655
Ta11 Ta11 Ta11 60.00(6) 24 23_655
Ta11 Ta11 Ta11 60.00(2) 22_665 23_655
Ta11 Ta11 Ta11 34(4) 3_665 23_655
Ta11 Ta11 Ta11 26(4) 2_655 23_655
Ta11 Ta11 F4 149.1(6) 24 3_665
Ta11 Ta11 F4 84.8(5) 22_665 3_665
Ta11 Ta11 F4 110(4) 3_665 3_665
Ta11 Ta11 F4 158.6(18) 2_655 3_665
Ta11 Ta11 F4 140.2(4) 23_655 3_665
Ta11 Ta11 F2 86.3(6) 24 .
Ta11 Ta11 F2 85.4(5) 22_665 .
Ta11 Ta11 F2 82.7(3) 3_665 .
Ta11 Ta11 F2 82.7(3) 2_655 .
Ta11 Ta11 F2 81.6(3) 23_655 .
F4 Ta11 F2 77.2(8) 3_665 .
Ta11 Ta11 F3 86.0(6) 24 .
Ta11 Ta11 F3 146.2(6) 22_665 .
Ta11 Ta11 F3 157.2(6) 3_665 .
Ta11 Ta11 F3 117(4) 2_655 .
Ta11 Ta11 F3 139.6(6) 23_655 .
F4 Ta11 F3 80.1(4) 3_665 .
F2 Ta11 F3 119.9(8) . .
Ta11 Ta11 F4 27.1(5) 24 .
Ta11 Ta11 F4 138.2(3) 22_665 .
Ta11 Ta11 F4 114(4) 3_665 .
Ta11 Ta11 F4 57(4) 2_655 .
Ta11 Ta11 F4 81.7(3) 23_655 .
F4 Ta11 F4 122.0(8) 3_665 .
F2 Ta11 F4 72.3(7) . .
F3 Ta11 F4 74.5(6) . .
Ta11 Ta11 F3 137.6(4) 24 3_665
Ta11 Ta11 F3 29.0(3) 22_665 3_665
Ta11 Ta11 F3 51(3) 3_665 3_665
Ta11 Ta11 F3 107(4) 2_655 3_665
Ta11 Ta11 F3 82.2(3) 23_655 3_665
F4 Ta11 F3 72.9(8) 3_665 3_665
F2 Ta11 F3 107.8(8) . 3_665
F3 Ta11 F3 117.2(9) . 3_665
F4 Ta11 F3 163.7(6) . 3_665
Ta11 Ta11 F1 86.5(5) 24 .
Ta11 Ta11 F1 85.6(4) 22_665 .
Ta11 Ta11 F1 83.2(2) 3_665 .
Ta11 Ta11 F1 83.2(2) 2_655 .
Ta11 Ta11 F1 82.1(3) 23_655 .
F4 Ta11 F1 115.4(9) 3_665 .
F2 Ta11 F1 163.7(5) . .
F3 Ta11 F1 74.0(6) . .
F4 Ta11 F1 106.3(9) . .
F3 Ta11 F1 68.8(6) 3_665 .
Ta11 Ta11 F4 86.7(5) 24 2_655
Ta11 Ta11 F4 36.3(5) 22_665 2_655
Ta11 Ta11 F4 16.8(15) 3_665 2_655
Ta11 Ta11 F4 54(3) 2_655 2_655
Ta11 Ta11 F4 30.4(5) 23_655 2_655
F4 Ta11 F4 109.8(9) 3_665 2_655
F2 Ta11 F4 67.1(5) . 2_655
F3 Ta11 F4 169.5(11) . 2_655
F4 Ta11 F4 101.9(7) . 2_655
F3 Ta11 F4 64.4(4) 3_665 2_655
F1 Ta11 F4 98.0(6) . 2_655
F7 Ta2 F6 78.4(3) . .
F7 Ta2 F6 78.4(3) . 2
F6 Ta2 F6 116.0(2) . 2
F7 Ta2 F6 78.4(3) . 3
F6 Ta2 F6 116.0(2) . 3
F6 Ta2 F6 116.0(2) 2 3
F7 Ta2 F5 132.9(2) . .
F6 Ta2 F5 77.20(19) . .
F6 Ta2 F5 77.21(19) 2 .
F6 Ta2 F5 148.7(5) 3 .
F7 Ta2 F5 132.9(2) . 2
F6 Ta2 F5 148.7(5) . 2
F6 Ta2 F5 77.21(19) 2 2
F6 Ta2 F5 77.21(19) 3 2
F5 Ta2 F5 78.7(4) . 2
F7 Ta2 F5 132.9(2) . 3
F6 Ta2 F5 77.20(19) . 3
F6 Ta2 F5 148.7(5) 2 3
F6 Ta2 F5 77.21(19) 3 3
F5 Ta2 F5 78.7(4) . 3
F5 Ta2 F5 78.7(4) 2 3
F5 Ta22 F5 84.3(6) . 2
F5 Ta22 F5 84.3(6) . 3
F5 Ta22 F5 84.3(6) 2 3
F5 Ta22 F6 78.9(2) . .
F5 Ta22 F6 157.3(8) 2 .
F5 Ta22 F6 78.9(2) 3 .
F5 Ta22 F6 78.9(2) . 2
F5 Ta22 F6 78.9(2) 2 2
F5 Ta22 F6 157.3(8) 3 2
F6 Ta22 F6 112.3(4) . 2
F5 Ta22 F6 157.3(8) . 3
F5 Ta22 F6 78.9(2) 2 3
F5 Ta22 F6 78.9(2) 3 3
F6 Ta22 F6 112.3(4) . 3
F6 Ta22 F6 112.3(4) 2 3
F5 Ta22 F7 129.2(4) . .
F5 Ta22 F7 129.2(4) 2 .
F5 Ta22 F7 129.2(4) 3 .
F6 Ta22 F7 73.5(5) . .
F6 Ta22 F7 73.5(5) 2 .
F6 Ta22 F7 73.5(5) 3 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ta1 Ta11 0.381(11) 23_655
Ta1 Ta11 0.381(11) 2_655
Ta1 Ta11 0.381(11) 3_665
Ta1 Ta11 0.381(11) 24
Ta1 Ta11 0.381(11) 22_665
Ta1 F1 1.835(12) .
Ta1 F3 2.003(7) 2_655
Ta1 F3 2.003(7) .
Ta1 F3 2.003(7) 3_665
Ta1 F2 2.201(19) .
Ta1 F4 2.079(9) 2_655
Ta1 F4 2.079(9) .
Ta11 Ta11 0.26(4) 24
Ta11 Ta11 0.32(3) 22_665
Ta11 Ta11 0.499(16) 3_665
Ta11 Ta11 0.499(16) 2_655
Ta11 Ta11 0.575(19) 23_655
Ta11 F4 1.77(2) 3_665
Ta11 F2 1.97(2) .
Ta11 F3 1.839(13) .
Ta11 F4 1.99(2) .
Ta11 F3 2.11(2) 3_665
Ta11 F1 2.10(2) .
Ta11 F4 2.243(12) 2_655
Ta2 F7 1.901(12) .
Ta2 F6 1.933(6) .
Ta2 F6 1.933(6) 2
Ta2 F6 1.933(6) 3
Ta2 F5 2.028(7) .
Ta2 F5 2.028(7) 2
Ta2 F5 2.028(7) 3
Ta22 F5 1.917(11) .
Ta22 F5 1.917(11) 2
Ta22 F5 1.917(11) 3
Ta22 F6 1.975(7) .
Ta22 F6 1.975(7) 2
Ta22 F6 1.975(7) 3
Ta22 F7 2.070(18) .
F1 Ta11 2.10(2) 23_655
F1 Ta11 2.10(2) 3_665
F1 Ta11 2.10(2) 2_655
F1 Ta11 2.10(2) 24
F1 Ta11 2.10(2) 22_665
F2 Ta11 1.97(2) 2_655
F2 Ta11 1.97(2) 23_655
F2 Ta11 1.97(2) 24
F2 Ta11 1.97(2) 3_665
F2 Ta11 1.97(2) 22_665
F3 Ta11 1.839(13) 24
F3 Ta11 2.11(2) 22_665
F3 Ta11 2.11(2) 2_655
F3 Ta11 2.307(18) 3_665
F3 Ta11 2.307(18) 23_655
F4 Ta11 1.77(2) 24
F4 Ta11 1.77(2) 2_655
F4 Ta11 1.99(2) 23_655
F4 Ta11 2.243(12) 22_665
F4 Ta11 2.243(12) 3_665
N1 H1 0.9462 .

_cod_database_fobs_code 2108543
