#------------------------------------------------------------------------------
#$Date: 2019-11-22 08:26:23 +0200 (Fri, 22 Nov 2019) $
#$Revision: 231197 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/85/2108547.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_2108547
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),2(Rb)'
_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      orthorhombic
_space_group_IT_number           67
_space_group_name_Hall           '-C 2a 2'
_space_group_name_H-M_alt        'C m m a'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2419(5)
_cell_length_b                   8.2749(5)
_cell_length_c                   10.5694(7)
_cell_measurement_reflns_used    512
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      32.09
_cell_measurement_theta_min      3.86
_cell_volume                     720.84(8)
_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      123(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.971
_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  0.0384
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4382
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.087
_diffrn_reflns_theta_min         3.856
_exptl_absorpt_coefficient_mu    28.722
_exptl_absorpt_correction_T_max  0.1077
_exptl_absorpt_correction_T_min  0.0500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2.03; Bruker 1999'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.468
_exptl_crystal_description       Prism
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.140
_refine_diff_density_max         2.228
_refine_diff_density_min         -3.298
_refine_diff_density_rms         0.267
_refine_ls_extinction_coef       0.0013(2)
_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   1.147
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         693
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0222
_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)+(0.0298P)²+5.6867P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0597
_reflns_Friedel_coverage         0.000
_reflns_number_gt                661
_reflns_number_total             693
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wf5151sup1.cif
_cod_data_source_block           II-LT
_cod_original_sg_symbol_Hall     '-C 2b 2'
_cod_database_code               2108547
_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   0.050
_shelx_estimated_absorpt_t_max   0.108
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z'
'-x, y+1/2, -z'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z'
'-x+1/2, y+1, -z'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z'
'x, -y-1/2, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z'
'x+1/2, -y, z'
'-x+1/2, y+1/2, 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 0.0000 0.7500 0.24367(2) 0.01309(13) Uani 1 4 d S T P
Rb1 Rb 0.2500 0.5000 0.0000 0.01505(16) Uani 1 4 d S T P
Rb2 Rb 0.0000 0.7500 0.63582(7) 0.02155(18) Uani 1 4 d S T P
F1 F 0.0000 0.7500 0.0548(4) 0.0181(9) Uani 1 4 d S T P
F2 F 0.0000 0.5222(5) 0.2033(4) 0.0283(8) Uani 1 2 d S T P
F3 F 0.1029(8) 0.6509(9) 0.3895(4) 0.0378(15) Uani 0.5 1 d . U P
F4 F 0.2286(5) 0.7500 0.2014(4) 0.0277(8) Uani 1 2 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 '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 F4 87.08(4) . 2_565
F2 Ta1 F4 87.08(4) 2_565 2_565
F2 Ta1 F4 87.08(4) . .
F2 Ta1 F4 87.08(4) 2_565 .
F4 Ta1 F4 153.3(2) 2_565 .
F2 Ta1 F3 76.3(2) . .
F4 Ta1 F3 76.0(2) . .
F2 Ta1 F3 76.3(2) 2_565 11_575
F4 Ta1 F3 76.0(2) . 11_575
F2 Ta1 F3 76.3(2) 2_565 2_565
F4 Ta1 F3 76.0(2) 2_565 2_565
F4 Ta1 F3 76.0(2) 2_565 12
F3 Ta1 F3 74.8(4) 11_575 12
F2 Ta1 F1 77.25(12) . .
F2 Ta1 F1 77.25(12) 2_565 .
F4 Ta1 F1 76.67(11) 2_565 .
F4 Ta1 F1 76.67(11) . .
F3 Ta1 Rb1 93.99(18) 12 9_565
F1 Ta1 Rb1 48.586(4) . 9_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ta1 F2 1.933(4) .
Ta1 F2 1.933(4) 2_565
Ta1 F4 1.936(4) 2_565
Ta1 F4 1.936(4) .
Ta1 F3 1.941(5) .
Ta1 F3 1.941(5) 11_575
Ta1 F3 1.941(5) 2_565
Ta1 F3 1.941(5) 12
Ta1 F1 1.997(4) .
Ta1 Rb1 3.8933(2) 9_565
Rb1 F4 2.974(3) .
Rb1 F4 2.974(3) 10
Rb1 F4 2.974(3) 6
Rb1 F4 2.974(3) 13_565
Rb1 F1 2.9766(9) 9_565
Rb1 F1 2.9766(9) .
Rb1 F1 2.9766(9) 13_565
Rb1 F1 2.9766(9) 5_545
Rb1 F2 2.983(3) .
Rb1 F2 2.983(3) 9_565
Rb2 F4 2.822(4) 13_566
Rb2 F4 2.822(4) 14_456
Rb2 F2 2.822(4) 10_566
Rb2 F2 2.822(4) 9_566
Rb2 F3 2.858(5) 12
Rb2 F3 2.858(5) 2_565
Rb2 F3 2.858(5) 11_575
Rb2 F3 2.858(5) .
Rb2 F3 3.385(7) 14_456
Rb2 F3 3.385(7) 13_566
F1 F4 2.440(5) .
F1 F4 2.440(5) 2_565
F1 F2 2.453(5) .
F1 F2 2.453(5) 2_565
F1 Rb1 2.9766(9) 9_565
F1 Rb1 2.9766(9) 13_565
F1 Rb1 2.9766(9) 5_455
F1 F4 3.512(5) 14_455
F2 F3 2.393(7) .
F2 F3 2.393(7) 12
F2 F4 2.665(4) .
F2 F4 2.665(4) 2_565
F2 Rb2 2.822(4) 9_566
F2 Rb1 2.983(3) 9_565
F2 F4 3.174(4) 5_445
F3 F3 1.640(15) 11_575
F3 F3 1.696(14) 12
F3 F3 2.359(12) 2_565
F3 F4 2.387(7) .
F3 F3 3.367(11) 7_546
F3 Rb2 3.385(7) 13_566
F3 F3 3.420(12) 4_566
F4 F3 2.387(7) 11_575
F4 F2 2.665(4) 2_565
F4 Rb2 2.822(4) 13_566
F4 Rb1 2.974(3) 13_565
F4 F2 3.174(4) 5

_cod_database_fobs_code 2108547
