#------------------------------------------------------------------------------
#$Date: 2019-11-22 08:26:23 +0200 (Fri, 22 Nov 2019) $
#$Revision: 231197 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/85/2108548.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_2108548
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),Rb2'
_chemical_formula_sum            'F7 Rb2 Ta'
_chemical_formula_weight         484.89
_chemical_name_common            'rubidium heptafluorotantalate'
_chemical_name_systematic        'rubidium 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_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                   5.9118(3)
_cell_length_b                   5.9118(3)
_cell_length_c                   10.6173(10)
_cell_measurement_reflns_used    512
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      37.99
_cell_measurement_theta_min      3.84
_cell_volume                     371.07(4)
_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      297(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9610
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.988
_diffrn_reflns_theta_min         3.838
_exptl_absorpt_coefficient_mu    27.898
_exptl_absorpt_correction_T_max  0.1116
_exptl_absorpt_correction_T_min  0.0518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.340
_exptl_crystal_description       Prism
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.512
_refine_diff_density_min         -1.889
_refine_diff_density_rms         0.238
_refine_ls_extinction_coef       0.0205(13)
_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   1.177
_refine_ls_matrix_type           full
_refine_ls_number_parameters     28
_refine_ls_number_reflns         638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0244P)²+0.6642P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                562
_reflns_number_total             638
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wf5151sup1.cif
_cod_data_source_block           II-RT
_cod_original_cell_volume        371.07(5)
_cod_original_sg_symbol_H-M      'P 4/n m m'
_cod_database_code               2108548
_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   0.052
_shelx_estimated_absorpt_t_max   0.112
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 0.25483(2) 0.02409(10) Uani 1 8 d S T P
Rb1 Rb 0.2500 0.7500 0.5000 0.02940(15) Uani 1 8 d S T P
Rb2 Rb 0.2500 0.2500 0.86308(8) 0.0425(2) Uani 1 8 d S T P
F1 F 0.2500 0.2500 0.4444(4) 0.0378(11) Uani 1 8 d S T P
F2 F 0.0243(4) 0.4757(4) 0.2991(3) 0.0518(8) Uani 1 2 d S T P
F3 F 0.204(5) 0.4466(14) 0.1096(5) 0.067(9) Uani 0.25 1 d . . P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Rb Rb -0.9393 2.9676 '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
F2 Ta1 F2 152.0(2) 4 3
F2 Ta1 F2 86.65(5) 4 2
F2 Ta1 F2 86.65(5) 3 2
F2 Ta1 F2 86.65(5) 4 .
F2 Ta1 F2 86.65(5) 3 .
F2 Ta1 F3 71.8(7) 3 13_565
F2 Ta1 F3 83.0(7) 2 13_565
F2 Ta1 F3 71.8(7) 3 3
F2 Ta1 F3 83.0(7) . 3
F2 Ta1 F3 83.0(7) 3 15_665
F2 Ta1 F3 71.8(7) . 15_665
F2 Ta1 F3 83.0(7) 3 2
F2 Ta1 F3 71.8(6) 2 2
F3 Ta1 F3 62.6(14) 15_665 2
F2 Ta1 F3 83.0(7) 4 16
F2 Ta1 F3 83.0(7) . 14_655
F3 Ta1 F3 75.5(6) 13_565 14_655
F3 Ta1 F3 62.6(14) 3 14_655
F3 Ta1 F3 51.3(4) 15_665 14_655
F3 Ta1 F3 73.2(5) 2 14_655
F3 Ta1 F3 51.3(4) 16 14_655
F2 Ta1 F3 71.8(7) 4 4
F2 Ta1 F3 83.0(7) 2 4
F2 Ta1 F3 120.3(8) . 4
F3 Ta1 F3 62.6(14) 13_565 4
F3 Ta1 F3 75.5(6) 3 4
F3 Ta1 F3 73.2(5) 15_665 4
F2 Ta1 F3 83.0(7) 4 .
F2 Ta1 F3 71.8(6) . .
F3 Ta1 F3 73.2(5) 13_565 .
F3 Ta1 F3 51.3(4) 3 .
F3 Ta1 F3 37.7(15) 15_665 .
F3 Ta1 F3 75.5(6) 2 .
F3 Ta1 F3 62.6(14) 16 .
F3 Ta1 F3 16.0(18) 14_655 .
F3 Ta1 F3 51.3(4) 4 .
F2 Ta1 F1 76.01(11) 4 .
F2 Ta1 F1 76.01(11) 3 .
F2 Ta1 F1 76.01(11) 2 .
F2 Ta1 F1 76.01(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ta1 F2 1.945(3) 4
Ta1 F2 1.945(3) 3
Ta1 F2 1.945(3) 2
Ta1 F2 1.945(3) .
Ta1 F3 1.949(8) 13_565
Ta1 F3 1.949(8) 3
Ta1 F3 1.949(8) 15_665
Ta1 F3 1.949(8) 2
Ta1 F3 1.949(8) 16
Ta1 F3 1.949(8) 14_655
Ta1 F3 1.949(8) 4
Ta1 F3 1.949(8) .
Ta1 F1 2.013(5) .
Ta1 Rb1 3.9387(3) 9_666
Ta1 Rb1 3.9387(3) .
Ta1 Rb1 3.9387(3) 9_566
Ta1 Rb1 3.9387(3) 1_545
Rb1 F2 2.993(3) .
Rb1 F2 2.993(3) 10_666
Rb1 F2 2.993(3) 12_666
Rb1 F2 2.993(3) 4
Rb1 F2 2.993(3) 11_566
Rb1 F2 2.993(3) 3_565
Rb1 F2 2.993(3) 9_566
Rb1 F2 2.993(3) 2_565
Rb1 F1 3.0143(9) 9_666
Rb1 F1 3.0143(9) 9_566
Rb1 F1 3.0143(9) 1_565
Rb1 F1 3.0143(9) .
Rb1 Ta1 3.9387(3) 9_666
Rb1 Ta1 3.9387(3) 1_565
Rb1 Ta1 3.9387(3) 9_566
Rb2 F2 2.868(3) 11_556
Rb2 F2 2.868(3) 12_666
Rb2 F2 2.868(3) 10_656
Rb2 F2 2.868(3) 9_566
Rb2 F3 2.877(7) 14_656
Rb2 F3 2.877(7) 4_556
Rb2 F3 2.877(7) 16_556
Rb2 F3 2.877(7) 1_556
Rb2 F3 2.877(7) 15_666
Rb2 F3 2.877(7) 2_556
Rb2 F3 2.877(7) 13_566
Rb2 F3 2.877(7) 3_556
Rb2 F3 3.24(3) 6_566
Rb2 F3 3.24(3) 12_666
Rb2 F3 3.24(3) 11_556
Rb2 F3 3.24(3) 5_546
Rb2 F3 3.24(3) 7_456
Rb2 F3 3.24(3) 10_656
Rb2 F3 3.24(3) 8_656
Rb2 F3 3.24(3) 9_566
F1 F2 2.437(4) 3
F1 F2 2.437(4) 2
F1 F2 2.437(4) 4
F1 F2 2.437(4) .
F1 Rb1 3.0143(9) 9_666
F1 Rb1 3.0143(9) 9_566
F1 Rb1 3.0143(9) 1_545
F2 F3 2.282(16) .
F2 F3 2.282(16) 15_665
F2 F3 2.58(2) 3
F2 F3 2.58(2) 14_655
F2 F2 2.669(4) 4
F2 F2 2.669(4) 3
F3 F3 2.324(17) 13_565
F3 F3 2.39(2) 2
F3 F2 2.58(2) 4
F3 Rb2 2.877(7) 1_554

_cod_database_fobs_code 2108548
