# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_0510_2_0m
_database_code_depnum_ccdc_archive 'CCDC 1847859'
_audit_update_record             
;
2018-06-07 deposited with the CCDC.
2018-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'F3 H8 N2 O4 S Sb'
_chemical_formula_weight         310.89

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   10.8684(4)
_cell_length_b                   10.9090(5)
_cell_length_c                   13.3631(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1584.37(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    512
_cell_measurement_theta_min      6.100
_cell_measurement_theta_max      56.621

_exptl_crystal_description       rodlike
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.607
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    3.777
_shelx_estimated_absorpt_T_min   0.519
_shelx_estimated_absorpt_T_max   0.601
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21423
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.049
_diffrn_reflns_theta_max         28.348
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1979
_reflns_number_gt                1678
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0375P)²+0.8225P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1979
_refine_ls_number_parameters     100
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0222
_refine_ls_wR_factor_ref         0.0595
_refine_ls_wR_factor_gt          0.0551
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.43893(2) 0.37970(2) 0.37964(2) 0.01079(8) Uani 1 1 d . . . . .
S1 S 0.73344(6) 0.38431(5) 0.50098(5) 0.01119(13) Uani 1 1 d . . . . .
F1 F 0.48323(14) 0.24537(14) 0.29092(12) 0.0186(3) Uani 1 1 d . . . . .
F3 F 0.28492(15) 0.38115(12) 0.30596(12) 0.0186(3) Uani 1 1 d . . . . .
F2 F 0.50792(15) 0.48475(14) 0.27535(12) 0.0193(3) Uani 1 1 d . . . . .
O3 O 0.64926(18) 0.38861(15) 0.58824(15) 0.0155(4) Uani 1 1 d . . . . .
O2 O 0.76936(18) 0.51018(17) 0.47385(13) 0.0204(4) Uani 1 1 d . . . . .
O4 O 0.84395(18) 0.31329(19) 0.52618(17) 0.0278(5) Uani 1 1 d . . . . .
O1 O 0.66884(18) 0.32678(18) 0.41649(15) 0.0224(4) Uani 1 1 d . . . . .
N2 N 0.7587(2) 0.13500(17) 0.28870(18) 0.0165(5) Uani 1 1 d . . . . .
H2A H 0.8294 0.1402 0.2729 0.025 Uiso 1 1 d R U . . .
H2B H 0.7161 0.1195 0.2385 0.025 Uiso 1 1 d R U . . .
H2C H 0.7591 0.0717 0.3319 0.025 Uiso 1 1 d R U . . .
H2D H 0.7280 0.2042 0.3154 0.025 Uiso 1 1 d R U . . .
N1 N 0.05677(19) 0.36298(19) 0.40776(19) 0.0140(4) Uani 1 1 d . . . . .
H1A H -0.0134 0.3562 0.4373 0.021 Uiso 1 1 d R U . . .
H1B H 0.0805 0.2985 0.4000 0.021 Uiso 1 1 d R U . . .
H1C H 0.1114 0.4055 0.4450 0.021 Uiso 1 1 d R U . . .
H1D H 0.0329 0.4073 0.3572 0.021 Uiso 1 1 d R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 F3 1.9420(16) . ?
Sb1 F1 1.9456(15) . ?
Sb1 F2 1.9539(15) . ?
S1 O4 1.4684(19) . ?
S1 O1 1.470(2) . ?
S1 O2 1.4729(18) . ?
S1 O3 1.483(2) . ?
N2 H2A 0.7986 . ?
N2 H2B 0.8322 . ?
N2 H2C 0.8997 . ?
N2 H2D 0.8985 . ?
N1 H1A 0.8626 . ?
N1 H1B 0.7564 . ?
N1 H1C 0.9029 . ?
N1 H1D 0.8704 . ?

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
_geom_angle_publ_flag
F3 Sb1 F1 84.86(6) . . ?
F3 Sb1 F2 87.95(7) . . ?
F1 Sb1 F2 84.96(7) . . ?
O4 S1 O1 109.97(13) . . ?
O4 S1 O2 109.36(12) . . ?
O1 S1 O2 109.60(12) . . ?
O4 S1 O3 109.94(12) . . ?
O1 S1 O3 108.83(11) . . ?
O2 S1 O3 109.12(11) . . ?
H2A N2 H2B 109.6 . . ?
H2A N2 H2C 102.6 . . ?
H2B N2 H2C 111.3 . . ?
H2A N2 H2D 113.7 . . ?
H2B N2 H2D 106.5 . . ?
H2C N2 H2D 113.1 . . ?
H1A N1 H1B 106.5 . . ?
H1A N1 H1C 111.9 . . ?
H1B N1 H1C 109.2 . . ?
H1A N1 H1D 98.0 . . ?
H1B N1 H1D 120.8 . . ?
H1C N1 H1D 109.8 . . ?

_refine_diff_density_max         0.450
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.160

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_0508_5_0m
_database_code_depnum_ccdc_archive 'CCDC 1847860'
_audit_update_record             
;
2018-06-07 deposited with the CCDC.
2018-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'F6 O8 Rb4 S2 Sb2'
_chemical_formula_weight         891.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
S S 0.1246 0.1234 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   9.2727(7)
_cell_length_b                   5.7702(4)
_cell_length_c                   14.4934(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     775.47(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4216
_cell_measurement_theta_min      7.132
_cell_measurement_theta_max      52.642

_exptl_crystal_description       rodlike
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.818
_exptl_crystal_F_000             800
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    16.319
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9775
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.608
_diffrn_reflns_theta_max         26.380
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1594
_reflns_number_gt                1482
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.667
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0323P)²+6.5139P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 559 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.483(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1594
_refine_ls_number_parameters     100
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0326
_refine_ls_wR_factor_ref         0.0801
_refine_ls_wR_factor_gt          0.0780
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.69107(8) 0.27077(14) 0.77282(5) 0.0216(2) Uani 1 1 d . . . . .
Rb1 Rb 1.06604(11) 0.2660(2) 0.63375(7) 0.0247(3) Uani 1 1 d . . . . .
Rb2 Rb 0.73737(11) 0.7550(2) 0.56097(7) 0.0257(2) Uani 1 1 d . . . . .
S1 S 0.4548(3) 0.2177(5) 0.59579(18) 0.0224(6) Uani 1 1 d . . . . .
F1 F 0.8196(9) 0.0337(11) 0.7170(6) 0.0265(18) Uani 1 1 d . . . . .
F2 F 0.8409(7) 0.2852(13) 0.8720(4) 0.0263(15) Uani 1 1 d . . . . .
F3 F 0.8225(9) 0.4824(12) 0.7116(5) 0.0240(18) Uani 1 1 d . . . . .
O1 O 0.3764(10) 0.1654(16) 0.6833(6) 0.030(2) Uani 1 1 d . . . . .
O4 O 0.6025(9) 0.3037(16) 0.6209(5) 0.030(2) Uani 1 1 d . . . . .
O2 O 0.4671(10) 0.0081(15) 0.5404(7) 0.030(2) Uani 1 1 d . . . . .
O3 O 0.3794(13) 0.4007(17) 0.5460(8) 0.043(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 F3 1.940(8) . ?
Sb1 F1 1.986(8) . ?
Sb1 F2 2.001(6) . ?
Sb1 O4 2.358(8) . ?
Sb1 O1 2.446(9) 3_656 ?
Sb1 Rb1 3.8823(14) 3_756 ?
Sb1 Rb1 3.9230(14) 3_746 ?
Sb1 Rb1 4.0191(12) . ?
Sb1 Rb2 4.1737(13) . ?
Sb1 Rb2 4.2313(12) 2_665 ?
Sb1 Rb2 4.2974(14) 1_545 ?
Rb1 F3 2.816(9) . ?
Rb1 F1 2.862(8) 3_756 ?
Rb1 F2 2.907(8) 3_746 ?
Rb1 F1 2.911(8) . ?
Rb1 F3 2.962(7) 3_746 ?
Rb1 O2 2.985(10) 4_556 ?
Rb1 O1 3.022(9) 1_655 ?
Rb1 F2 3.119(8) 3_756 ?
Rb1 O3 3.265(13) 1_655 ?
Rb1 O3 3.272(12) 4_556 ?
Rb1 S1 3.484(3) 4_556 ?
Rb1 S1 3.657(3) 1_655 ?
Rb2 F3 2.804(7) . ?
Rb2 F2 2.842(6) 2_664 ?
Rb2 O3 2.843(10) 4_566 ?
Rb2 F1 2.878(8) 1_565 ?
Rb2 O2 2.916(10) 1_565 ?
Rb2 O2 3.000(9) 4_556 ?
Rb2 O4 3.017(9) . ?
Rb2 O4 3.513(10) 1_565 ?
Rb2 S1 3.775(3) 1_565 ?
Rb2 Sb1 4.2313(12) 2_664 ?
Rb2 Rb1 4.2574(16) 4_466 ?
S1 O2 1.456(9) . ?
S1 O3 1.458(10) . ?
S1 O1 1.492(9) . ?
S1 O4 1.502(9) . ?
S1 Rb1 3.484(3) 4_456 ?
S1 Rb1 3.657(3) 1_455 ?
S1 Rb2 3.775(3) 1_545 ?
F1 Rb1 2.862(8) 3_746 ?
F1 Rb2 2.878(8) 1_545 ?
F2 Rb2 2.842(6) 2_665 ?
F2 Rb1 2.907(8) 3_756 ?
F2 Rb1 3.119(8) 3_746 ?
F3 Rb1 2.962(7) 3_756 ?
O1 Sb1 2.446(9) 3_646 ?
O1 Rb1 3.022(9) 1_455 ?
O4 Rb2 3.513(10) 1_545 ?
O2 Rb2 2.916(10) 1_545 ?
O2 Rb1 2.985(10) 4_456 ?
O2 Rb2 3.000(9) 4_456 ?
O3 Rb2 2.843(10) 4_466 ?
O3 Rb1 3.265(12) 1_455 ?
O3 Rb1 3.272(12) 4_456 ?

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
_geom_angle_publ_flag
F3 Sb1 F1 82.6(2) . . ?
F3 Sb1 F2 82.3(3) . . ?
F1 Sb1 F2 84.5(3) . . ?
F3 Sb1 O4 75.0(3) . . ?
F1 Sb1 O4 83.4(3) . . ?
F2 Sb1 O4 155.4(3) . . ?
F3 Sb1 O1 72.2(3) . 3_656 ?
F1 Sb1 O1 154.2(3) . 3_656 ?
F2 Sb1 O1 87.2(3) . 3_656 ?
O4 Sb1 O1 94.5(3) . 3_656 ?
F3 Sb1 Rb1 48.1(2) . 3_756 ?
F1 Sb1 Rb1 107.5(2) . 3_756 ?
F2 Sb1 Rb1 46.8(2) . 3_756 ?
O4 Sb1 Rb1 117.9(2) . 3_756 ?
O1 Sb1 Rb1 51.1(2) 3_656 3_756 ?
F3 Sb1 Rb1 105.3(2) . 3_746 ?
F1 Sb1 Rb1 44.3(2) . 3_746 ?
F2 Sb1 Rb1 52.0(2) . 3_746 ?
O4 Sb1 Rb1 125.6(2) . 3_746 ?
O1 Sb1 Rb1 138.4(2) 3_656 3_746 ?
Rb1 Sb1 Rb1 95.34(3) 3_756 3_746 ?
F3 Sb1 Rb1 39.8(2) . . ?
F1 Sb1 Rb1 43.3(2) . . ?
F2 Sb1 Rb1 76.12(18) . . ?
O4 Sb1 Rb1 80.4(2) . . ?
O1 Sb1 Rb1 111.0(2) 3_656 . ?
Rb1 Sb1 Rb1 71.22(2) 3_756 . ?
Rb1 Sb1 Rb1 70.81(2) 3_746 . ?
F3 Sb1 Rb2 34.7(2) . . ?
F1 Sb1 Rb2 95.7(2) . . ?
F2 Sb1 Rb2 115.4(2) . . ?
O4 Sb1 Rb2 45.2(2) . . ?
O1 Sb1 Rb2 66.1(2) 3_656 . ?
Rb1 Sb1 Rb2 72.79(3) 3_756 . ?
Rb1 Sb1 Rb2 133.79(3) 3_746 . ?
Rb1 Sb1 Rb2 63.04(2) . . ?
F3 Sb1 Rb2 112.0(2) . 2_665 ?
F1 Sb1 Rb2 106.5(2) . 2_665 ?
F2 Sb1 Rb2 35.25(18) . 2_665 ?
O4 Sb1 Rb2 168.3(2) . 2_665 ?
O1 Sb1 Rb2 79.4(2) 3_656 2_665 ?
Rb1 Sb1 Rb2 65.83(3) 3_756 2_665 ?
Rb1 Sb1 Rb2 62.81(2) 3_746 2_665 ?
Rb1 Sb1 Rb2 111.04(3) . 2_665 ?
Rb2 Sb1 Rb2 137.18(2) . 2_665 ?
F3 Sb1 Rb2 92.7(2) . 1_545 ?
F1 Sb1 Rb2 34.1(2) . 1_545 ?
F2 Sb1 Rb2 118.2(2) . 1_545 ?
O4 Sb1 Rb2 54.8(2) . 1_545 ?
O1 Sb1 Rb2 148.9(2) 3_656 1_545 ?
Rb1 Sb1 Rb2 134.51(3) 3_756 1_545 ?
Rb1 Sb1 Rb2 71.04(3) 3_746 1_545 ?
Rb1 Sb1 Rb2 63.29(2) . 1_545 ?
Rb2 Sb1 Rb2 85.86(2) . 1_545 ?
Rb2 Sb1 Rb2 131.70(2) 2_665 1_545 ?
F3 Rb1 F1 75.8(2) . 3_756 ?
F3 Rb1 F2 132.3(2) . 3_746 ?
F1 Rb1 F2 115.27(19) 3_756 3_746 ?
F3 Rb1 F1 53.74(17) . . ?
F1 Rb1 F1 103.07(17) 3_756 . ?
F2 Rb1 F1 78.79(19) 3_746 . ?
F3 Rb1 F3 102.81(17) . 3_746 ?
F1 Rb1 F3 66.22(17) 3_756 3_746 ?
F2 Rb1 F3 52.47(18) 3_746 3_746 ?
F1 Rb1 F3 72.9(2) . 3_746 ?
F3 Rb1 O2 84.2(2) . 4_556 ?
F1 Rb1 O2 121.1(2) 3_756 4_556 ?
F2 Rb1 O2 118.9(2) 3_746 4_556 ?
F1 Rb1 O2 108.1(2) . 4_556 ?
F3 Rb1 O2 171.3(2) 3_746 4_556 ?
F3 Rb1 O1 138.9(2) . 1_655 ?
F1 Rb1 O1 64.6(2) 3_756 1_655 ?
F2 Rb1 O1 62.7(2) 3_746 1_655 ?
F1 Rb1 O1 124.1(2) . 1_655 ?
F3 Rb1 O1 51.8(2) 3_746 1_655 ?
O2 Rb1 O1 125.3(3) 4_556 1_655 ?
F3 Rb1 F2 78.86(19) . 3_756 ?
F1 Rb1 F2 53.07(18) 3_756 3_756 ?
F2 Rb1 F2 146.5(2) 3_746 3_756 ?
F1 Rb1 F2 132.11(19) . 3_756 ?
F3 Rb1 F2 117.03(19) 3_746 3_756 ?
O2 Rb1 F2 69.1(2) 4_556 3_756 ?
O1 Rb1 F2 85.8(2) 1_655 3_756 ?
F3 Rb1 O3 139.8(2) . 1_655 ?
F1 Rb1 O3 80.6(3) 3_756 1_655 ?
F2 Rb1 O3 87.2(2) 3_746 1_655 ?
F1 Rb1 O3 165.8(2) . 1_655 ?
F3 Rb1 O3 96.7(2) 3_746 1_655 ?
O2 Rb1 O3 80.8(3) 4_556 1_655 ?
O1 Rb1 O3 44.8(2) 1_655 1_655 ?
F2 Rb1 O3 61.0(2) 3_756 1_655 ?
F3 Rb1 O3 91.4(3) . 4_556 ?
F1 Rb1 O3 163.0(2) 3_756 4_556 ?
F2 Rb1 O3 81.6(2) 3_746 4_556 ?
F1 Rb1 O3 77.3(2) . 4_556 ?
F3 Rb1 O3 128.7(2) 3_746 4_556 ?
O2 Rb1 O3 45.0(2) 4_556 4_556 ?
O1 Rb1 O3 129.5(3) 1_655 4_556 ?
F2 Rb1 O3 114.0(2) 3_756 4_556 ?
O3 Rb1 O3 103.33(14) 1_655 4_556 ?
F3 Rb1 S1 97.64(16) . 4_556 ?
F1 Rb1 S1 144.76(16) 3_756 4_556 ?
F2 Rb1 S1 94.95(13) 3_746 4_556 ?
F1 Rb1 S1 100.12(18) . 4_556 ?
F3 Rb1 S1 147.24(16) 3_746 4_556 ?
O2 Rb1 S1 24.49(18) 4_556 4_556 ?
O1 Rb1 S1 120.92(17) 1_655 4_556 ?
F2 Rb1 S1 91.74(12) 3_756 4_556 ?
O3 Rb1 S1 83.41(19) 1_655 4_556 ?
O3 Rb1 S1 24.66(17) 4_556 4_556 ?
F3 Rb1 S1 152.18(17) . 1_655 ?
F1 Rb1 S1 77.85(18) 3_756 1_655 ?
F2 Rb1 S1 68.30(14) 3_746 1_655 ?
F1 Rb1 S1 143.23(17) . 1_655 ?
F3 Rb1 S1 74.20(18) 3_746 1_655 ?
O2 Rb1 S1 102.07(19) 4_556 1_655 ?
O1 Rb1 S1 23.43(17) 1_655 1_655 ?
F2 Rb1 S1 78.25(13) 3_756 1_655 ?
O3 Rb1 S1 23.45(17) 1_655 1_655 ?
O3 Rb1 S1 112.3(2) 4_556 1_655 ?
S1 Rb1 S1 98.65(5) 4_556 1_655 ?
F3 Rb2 F2 140.9(2) . 2_664 ?
F3 Rb2 O3 133.3(3) . 4_566 ?
F2 Rb2 O3 69.5(3) 2_664 4_566 ?
F3 Rb2 F1 68.11(17) . 1_565 ?
F2 Rb2 F1 150.5(2) 2_664 1_565 ?
O3 Rb2 F1 85.2(3) 4_566 1_565 ?
F3 Rb2 O2 127.1(3) . 1_565 ?
F2 Rb2 O2 73.9(2) 2_664 1_565 ?
O3 Rb2 O2 89.6(3) 4_566 1_565 ?
F1 Rb2 O2 91.6(2) 1_565 1_565 ?
F3 Rb2 O2 84.1(3) . 4_556 ?
F2 Rb2 O2 70.6(2) 2_664 4_556 ?
O3 Rb2 O2 76.0(3) 4_566 4_556 ?
F1 Rb2 O2 118.6(2) 1_565 4_556 ?
O2 Rb2 O2 144.45(11) 1_565 4_556 ?
F3 Rb2 O4 53.7(2) . . ?
F2 Rb2 O4 95.8(2) 2_664 . ?
O3 Rb2 O4 162.2(3) 4_566 . ?
F1 Rb2 O4 111.5(2) 1_565 . ?
O2 Rb2 O4 96.1(3) 1_565 . ?
O2 Rb2 O4 89.9(3) 4_556 . ?
F3 Rb2 O4 114.4(2) . 1_565 ?
F2 Rb2 O4 102.8(2) 2_664 1_565 ?
O3 Rb2 O4 70.7(3) 4_566 1_565 ?
F1 Rb2 O4 52.9(2) 1_565 1_565 ?
O2 Rb2 O4 42.9(2) 1_565 1_565 ?
O2 Rb2 O4 146.1(2) 4_556 1_565 ?
O4 Rb2 O4 124.0(3) . 1_565 ?
F3 Rb2 S1 119.22(18) . 1_565 ?
F2 Rb2 S1 90.54(15) 2_664 1_565 ?
O3 Rb2 S1 84.3(2) 4_566 1_565 ?
F1 Rb2 S1 71.56(17) 1_565 1_565 ?
O2 Rb2 S1 20.42(18) 1_565 1_565 ?
O2 Rb2 S1 156.40(19) 4_556 1_565 ?
O4 Rb2 S1 106.51(19) . 1_565 ?
O4 Rb2 S1 23.43(14) 1_565 1_565 ?
F3 Rb2 Sb1 23.17(17) . . ?
F2 Rb2 Sb1 128.89(16) 2_664 . ?
O3 Rb2 Sb1 156.4(3) 4_566 . ?
F1 Rb2 Sb1 79.82(15) 1_565 . ?
O2 Rb2 Sb1 108.80(19) 1_565 . ?
O2 Rb2 Sb1 95.41(18) 4_556 . ?
O4 Rb2 Sb1 33.66(15) . . ?
O4 Rb2 Sb1 112.64(13) 1_565 . ?
S1 Rb2 Sb1 107.68(5) 1_565 . ?
F3 Rb2 Sb1 134.79(17) . 2_664 ?
F2 Rb2 Sb1 23.97(13) 2_664 2_664 ?
O3 Rb2 Sb1 54.1(2) 4_566 2_664 ?
F1 Rb2 Sb1 138.92(16) 1_565 2_664 ?
O2 Rb2 Sb1 92.94(19) 1_565 2_664 ?
O2 Rb2 Sb1 52.24(18) 4_556 2_664 ?
O4 Rb2 Sb1 108.58(16) . 2_664 ?
O4 Rb2 Sb1 109.36(13) 1_565 2_664 ?
S1 Rb2 Sb1 105.41(5) 1_565 2_664 ?
Sb1 Rb2 Sb1 135.94(3) . 2_664 ?
F3 Rb2 Rb1 170.14(17) . 4_466 ?
F2 Rb2 Rb1 47.09(15) 2_664 4_466 ?
O3 Rb2 Rb1 50.0(3) 4_566 4_466 ?
F1 Rb2 Rb1 104.89(16) 1_565 4_466 ?
O2 Rb2 Rb1 44.46(19) 1_565 4_466 ?
O2 Rb2 Rb1 105.61(18) 4_556 4_466 ?
O4 Rb2 Rb1 126.61(17) . 4_466 ?
O4 Rb2 Rb1 56.35(13) 1_565 4_466 ?
S1 Rb2 Rb1 50.98(5) 1_565 4_466 ?
Sb1 Rb2 Rb1 152.11(3) . 4_466 ?
Sb1 Rb2 Rb1 55.05(2) 2_664 4_466 ?
O2 S1 O3 111.5(6) . . ?
O2 S1 O1 109.8(5) . . ?
O3 S1 O1 109.5(6) . . ?
O2 S1 O4 109.7(6) . . ?
O3 S1 O4 108.5(6) . . ?
O1 S1 O4 107.8(5) . . ?
O2 S1 Rb1 58.2(4) . 4_456 ?
O3 S1 Rb1 69.5(5) . 4_456 ?
O1 S1 Rb1 163.9(4) . 4_456 ?
O4 S1 Rb1 87.3(3) . 4_456 ?
O2 S1 Rb1 102.9(4) . 1_455 ?
O3 S1 Rb1 63.0(5) . 1_455 ?
O1 S1 Rb1 53.7(4) . 1_455 ?
O4 S1 Rb1 146.9(4) . 1_455 ?
Rb1 S1 Rb1 115.69(8) 4_456 1_455 ?
O2 S1 Rb2 44.3(4) . 1_545 ?
O3 S1 Rb2 141.2(5) . 1_545 ?
O1 S1 Rb2 108.0(4) . 1_545 ?
O4 S1 Rb2 68.5(4) . 1_545 ?
Rb1 S1 Rb2 71.69(6) 4_456 1_545 ?
Rb1 S1 Rb2 139.32(9) 1_455 1_545 ?
Sb1 F1 Rb1 106.6(3) . 3_746 ?
Sb1 F1 Rb2 123.1(4) . 1_545 ?
Rb1 F1 Rb2 113.0(2) 3_746 1_545 ?
Sb1 F1 Rb1 108.8(3) . . ?
Rb1 F1 Rb1 105.7(3) 3_746 . ?
Rb2 F1 Rb1 98.0(2) 1_545 . ?
Sb1 F2 Rb2 120.8(3) . 2_665 ?
Sb1 F2 Rb1 103.0(3) . 3_756 ?
Rb2 F2 Rb1 100.5(2) 2_665 3_756 ?
Sb1 F2 Rb1 97.6(3) . 3_746 ?
Rb2 F2 Rb1 91.03(19) 2_665 3_746 ?
Rb1 F2 Rb1 146.5(2) 3_756 3_746 ?
Sb1 F3 Rb2 122.2(4) . . ?
Sb1 F3 Rb1 114.1(3) . . ?
Rb2 F3 Rb1 99.4(2) . . ?
Sb1 F3 Rb1 102.8(3) . 3_756 ?
Rb2 F3 Rb1 112.2(2) . 3_756 ?
Rb1 F3 Rb1 105.6(3) . 3_756 ?
S1 O1 Sb1 122.3(5) . 3_646 ?
S1 O1 Rb1 102.9(4) . 1_455 ?
Sb1 O1 Rb1 89.8(3) 3_646 1_455 ?
S1 O4 Sb1 121.1(4) . . ?
S1 O4 Rb2 126.4(5) . . ?
Sb1 O4 Rb2 101.2(3) . . ?
S1 O4 Rb2 88.1(4) . 1_545 ?
Sb1 O4 Rb2 92.0(3) . 1_545 ?
Rb2 O4 Rb2 124.0(3) . 1_545 ?
S1 O2 Rb2 115.3(5) . 1_545 ?
S1 O2 Rb1 97.4(4) . 4_456 ?
Rb2 O2 Rb1 92.4(3) 1_545 4_456 ?
S1 O2 Rb2 129.4(5) . 4_456 ?
Rb2 O2 Rb2 114.0(3) 1_545 4_456 ?
Rb1 O2 Rb2 91.5(3) 4_456 4_456 ?
S1 O3 Rb2 176.6(7) . 4_466 ?
S1 O3 Rb1 93.5(5) . 1_455 ?
Rb2 O3 Rb1 88.1(3) 4_466 1_455 ?
S1 O3 Rb1 85.8(5) . 4_456 ?
Rb2 O3 Rb1 90.9(3) 4_466 4_456 ?
Rb1 O3 Rb1 135.3(4) 1_455 4_456 ?

_refine_diff_density_max         0.671
_refine_diff_density_min         -1.038
_refine_diff_density_rms         0.323

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_523
_database_code_depnum_ccdc_archive 'CCDC 1859398'
_audit_update_record             
;
2018-07-31 deposited with the CCDC.
2018-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'F12 Na8 O16 S4 Sb4'
_chemical_formula_weight         1283.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_H-M_alt        'C m c a'
_space_group_name_Hall           '-C 2bc 2'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   15.1698(6)
_cell_length_b                   7.1773(3)
_cell_length_c                   11.0738(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1205.70(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7484
_cell_measurement_theta_min      3.2300
_cell_measurement_theta_max      30.4680

_exptl_crystal_description       block-like
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.534
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    5.088
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9506
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.640
_diffrn_reflns_theta_max         30.477
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             950
_reflns_number_gt                936
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0357P)²+3.6395P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         950
_refine_ls_number_parameters     55
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0195
_refine_ls_wR_factor_ref         0.0532
_refine_ls_wR_factor_gt          0.0530
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.5000 0.88927(3) 0.66366(2) 0.01225(9) Uani 1 2 d S T P . .
S1 S 0.31660(5) 1.0000 0.5000 0.01027(14) Uani 1 2 d S T P . .
Na1 Na 0.2500 0.72040(19) 0.2500 0.0206(3) Uani 1 2 d S T P . .
Na2 Na 0.38226(10) 0.5000 0.5000 0.0294(4) Uani 1 2 d S T P . .
F1 F 0.5000 0.6262(3) 0.6157(2) 0.0191(4) Uani 1 2 d S T P . .
F2 F 0.59015(10) 0.8119(2) 0.78056(13) 0.0250(3) Uani 1 1 d . . . . .
O1 O 0.37424(11) 0.8368(2) 0.52382(16) 0.0183(3) Uani 1 1 d . . . . .
O2 O 0.26091(11) 0.9652(2) 0.39369(14) 0.0171(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 F1 1.9613(19) . ?
Sb1 F2 1.9632(14) . ?
Sb1 F2 1.9632(14) 12_655 ?
Sb1 O1 2.4859(17) 12_655 ?
Sb1 O1 2.4860(17) . ?
S1 O2 1.4704(16) . ?
S1 O2 1.4704(16) 4_576 ?
S1 O1 1.4855(17) . ?
S1 O1 1.4855(17) 4_576 ?
S1 Na2 3.0167(16) 13_566 ?
S1 Na1 3.3448(7) 10_566 ?
S1 Na1 3.3448(7) 13_566 ?
Na1 O2 2.3763(19) . ?
Na1 O2 2.3763(19) 7_545 ?
Na1 O2 2.4317(19) 10_556 ?
Na1 O2 2.4317(19) 16_545 ?
Na1 F2 2.4594(15) 8_466 ?
Na1 F2 2.4594(15) 2_664 ?
Na1 S1 3.3448(7) 10_556 ?
Na1 S1 3.3448(7) 13_566 ?
Na1 Na1 3.58864(14) 10_556 ?
Na1 Na1 3.58866(15) 10_566 ?
Na1 Na2 3.7673(10) . ?
Na1 Na2 3.7673(10) 6_554 ?
Na2 F1 2.3776(19) . ?
Na2 F1 2.3776(18) 9_666 ?
Na2 O1 2.4344(17) 4_566 ?
Na2 O1 2.4344(17) . ?
Na2 O2 2.483(2) 16_545 ?
Na2 O2 2.483(2) 13_566 ?
Na2 F2 2.8113(16) 3_646 ?
Na2 F2 2.8113(16) 2_664 ?
Na2 S1 3.0167(16) 13_566 ?
Na2 Na2 3.572(3) 9_666 ?
Na2 Na1 3.7673(10) 6 ?
F1 Na2 2.3776(18) 9_666 ?
F2 Na1 2.4594(15) 2_665 ?
F2 Na2 2.8112(16) 2_665 ?
O2 Na1 2.4318(19) 10_566 ?
O2 Na2 2.483(2) 13_566 ?

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
_geom_angle_publ_flag
F1 Sb1 F2 84.61(7) . . ?
F1 Sb1 F2 84.61(7) . 12_655 ?
F2 Sb1 F2 88.31(9) . 12_655 ?
F1 Sb1 O1 71.66(6) . 12_655 ?
F2 Sb1 O1 80.40(6) . 12_655 ?
F2 Sb1 O1 154.48(7) 12_655 12_655 ?
F1 Sb1 O1 71.67(6) . . ?
F2 Sb1 O1 154.48(7) . . ?
F2 Sb1 O1 80.40(6) 12_655 . ?
O1 Sb1 O1 100.25(8) 12_655 . ?
O2 S1 O2 109.86(14) . 4_576 ?
O2 S1 O1 110.27(10) . . ?
O2 S1 O1 109.26(9) 4_576 . ?
O2 S1 O1 109.26(10) . 4_576 ?
O2 S1 O1 110.27(10) 4_576 4_576 ?
O1 S1 O1 107.89(14) . 4_576 ?
O2 S1 Na2 54.93(7) . 13_566 ?
O2 S1 Na2 54.93(7) 4_576 13_566 ?
O1 S1 Na2 126.05(7) . 13_566 ?
O1 S1 Na2 126.06(7) 4_576 13_566 ?
O2 S1 Na1 40.89(7) . 10_566 ?
O2 S1 Na1 114.14(7) 4_576 10_566 ?
O1 S1 Na1 134.25(7) . 10_566 ?
O1 S1 Na1 69.99(7) 4_576 10_566 ?
Na2 S1 Na1 72.419(12) 13_566 10_566 ?
O2 S1 Na1 114.14(7) . 13_566 ?
O2 S1 Na1 40.89(7) 4_576 13_566 ?
O1 S1 Na1 69.99(7) . 13_566 ?
O1 S1 Na1 134.25(7) 4_576 13_566 ?
Na2 S1 Na1 72.419(12) 13_566 13_566 ?
Na1 S1 Na1 144.84(2) 10_566 13_566 ?
O2 Na1 O2 84.63(9) . 7_545 ?
O2 Na1 O2 172.02(8) . 10_556 ?
O2 Na1 O2 97.10(6) 7_545 10_556 ?
O2 Na1 O2 97.10(6) . 16_545 ?
O2 Na1 O2 172.02(8) 7_545 16_545 ?
O2 Na1 O2 82.27(9) 10_556 16_545 ?
O2 Na1 F2 103.33(6) . 8_466 ?
O2 Na1 F2 84.77(6) 7_545 8_466 ?
O2 Na1 F2 84.61(6) 10_556 8_466 ?
O2 Na1 F2 87.24(6) 16_545 8_466 ?
O2 Na1 F2 84.77(6) . 2_664 ?
O2 Na1 F2 103.33(6) 7_545 2_664 ?
O2 Na1 F2 87.24(6) 10_556 2_664 ?
O2 Na1 F2 84.61(6) 16_545 2_664 ?
F2 Na1 F2 169.18(10) 8_466 2_664 ?
O2 Na1 S1 151.99(5) . 10_556 ?
O2 Na1 S1 79.43(4) 7_545 10_556 ?
O2 Na1 S1 23.32(4) 10_556 10_556 ?
O2 Na1 S1 101.88(6) 16_545 10_556 ?
F2 Na1 S1 98.01(4) 8_466 10_556 ?
F2 Na1 S1 76.79(4) 2_664 10_556 ?
O2 Na1 S1 79.43(4) . 13_566 ?
O2 Na1 S1 151.99(5) 7_545 13_566 ?
O2 Na1 S1 101.88(6) 10_556 13_566 ?
O2 Na1 S1 23.32(4) 16_545 13_566 ?
F2 Na1 S1 76.79(4) 8_466 13_566 ?
F2 Na1 S1 98.01(4) 2_664 13_566 ?
S1 Na1 S1 123.55(4) 10_556 13_566 ?
O2 Na1 Na1 137.69(4) . 10_556 ?
O2 Na1 Na1 137.69(4) 7_545 10_556 ?
O2 Na1 Na1 41.14(4) 10_556 10_556 ?
O2 Na1 Na1 41.14(4) 16_545 10_556 ?
F2 Na1 Na1 84.59(5) 8_466 10_556 ?
F2 Na1 Na1 84.59(5) 2_664 10_556 ?
S1 Na1 Na1 61.77(2) 10_556 10_556 ?
S1 Na1 Na1 61.77(2) 13_566 10_556 ?
O2 Na1 Na1 42.31(4) . 10_566 ?
O2 Na1 Na1 42.31(4) 7_545 10_566 ?
O2 Na1 Na1 138.86(4) 10_556 10_566 ?
O2 Na1 Na1 138.86(4) 16_545 10_566 ?
F2 Na1 Na1 95.41(5) 8_466 10_566 ?
F2 Na1 Na1 95.41(5) 2_664 10_566 ?
S1 Na1 Na1 118.23(2) 10_556 10_566 ?
S1 Na1 Na1 118.23(2) 13_566 10_566 ?
Na1 Na1 Na1 180.0 10_556 10_566 ?
O2 Na1 Na2 77.37(4) . . ?
O2 Na1 Na2 147.10(5) 7_545 . ?
O2 Na1 Na2 97.37(5) 10_556 . ?
O2 Na1 Na2 40.46(5) 16_545 . ?
F2 Na1 Na2 125.92(5) 8_466 . ?
F2 Na1 Na2 48.26(4) 2_664 . ?
S1 Na1 Na2 104.40(3) 10_556 . ?
S1 Na1 Na2 49.76(2) 13_566 . ?
Na1 Na1 Na2 65.17(2) 10_556 . ?
Na1 Na1 Na2 114.83(2) 10_566 . ?
O2 Na1 Na2 147.10(5) . 6_554 ?
O2 Na1 Na2 77.37(4) 7_545 6_554 ?
O2 Na1 Na2 40.46(5) 10_556 6_554 ?
O2 Na1 Na2 97.37(5) 16_545 6_554 ?
F2 Na1 Na2 48.25(4) 8_466 6_554 ?
F2 Na1 Na2 125.92(5) 2_664 6_554 ?
S1 Na1 Na2 49.76(2) 10_556 6_554 ?
S1 Na1 Na2 104.40(3) 13_566 6_554 ?
Na1 Na1 Na2 65.17(2) 10_556 6_554 ?
Na1 Na1 Na2 114.83(2) 10_566 6_554 ?
Na2 Na1 Na2 130.34(4) . 6_554 ?
F1 Na2 F1 82.61(9) . 9_666 ?
F1 Na2 O1 118.31(7) . 4_566 ?
F1 Na2 O1 66.48(6) 9_666 4_566 ?
F1 Na2 O1 66.48(6) . . ?
F1 Na2 O1 118.31(7) 9_666 . ?
O1 Na2 O1 174.27(11) 4_566 . ?
F1 Na2 O2 161.98(6) . 16_545 ?
F1 Na2 O2 111.30(6) 9_666 16_545 ?
O1 Na2 O2 78.76(6) 4_566 16_545 ?
O1 Na2 O2 96.17(7) . 16_545 ?
F1 Na2 O2 111.30(5) . 13_566 ?
F1 Na2 O2 161.98(6) 9_666 13_566 ?
O1 Na2 O2 96.17(7) 4_566 13_566 ?
O1 Na2 O2 78.76(6) . 13_566 ?
O2 Na2 O2 57.98(8) 16_545 13_566 ?
F1 Na2 F2 66.75(6) . 3_646 ?
F1 Na2 F2 99.85(7) 9_666 3_646 ?
O1 Na2 F2 67.93(5) 4_566 3_646 ?
O1 Na2 F2 112.99(5) . 3_646 ?
O2 Na2 F2 119.46(6) 16_545 3_646 ?
O2 Na2 F2 76.62(5) 13_566 3_646 ?
F1 Na2 F2 99.85(7) . 2_664 ?
F1 Na2 F2 66.75(6) 9_666 2_664 ?
O1 Na2 F2 112.99(5) 4_566 2_664 ?
O1 Na2 F2 67.93(5) . 2_664 ?
O2 Na2 F2 76.62(5) 16_545 2_664 ?
O2 Na2 F2 119.46(6) 13_566 2_664 ?
F2 Na2 F2 162.88(9) 3_646 2_664 ?
F1 Na2 S1 138.70(5) . 13_566 ?
F1 Na2 S1 138.69(5) 9_666 13_566 ?
O1 Na2 S1 87.13(5) 4_566 13_566 ?
O1 Na2 S1 87.13(5) . 13_566 ?
O2 Na2 S1 28.99(4) 16_545 13_566 ?
O2 Na2 S1 28.99(4) 13_566 13_566 ?
F2 Na2 S1 98.56(4) 3_646 13_566 ?
F2 Na2 S1 98.56(4) 2_664 13_566 ?
F1 Na2 Na2 41.30(5) . 9_666 ?
F1 Na2 Na2 41.31(5) 9_666 9_666 ?
O1 Na2 Na2 92.87(5) 4_566 9_666 ?
O1 Na2 Na2 92.87(5) . 9_666 ?
O2 Na2 Na2 151.01(4) 16_545 9_666 ?
O2 Na2 Na2 151.01(4) 13_566 9_666 ?
F2 Na2 Na2 81.44(4) 3_646 9_666 ?
F2 Na2 Na2 81.44(4) 2_664 9_666 ?
S1 Na2 Na2 180.0 13_566 9_666 ?
F1 Na2 Na1 129.51(5) . . ?
F1 Na2 Na1 99.44(5) 9_666 . ?
O1 Na2 Na1 108.10(5) 4_566 . ?
O1 Na2 Na1 68.66(5) . . ?
O2 Na2 Na1 39.46(4) 16_545 . ?
O2 Na2 Na1 80.82(5) 13_566 . ?
F2 Na2 Na1 156.37(6) 3_646 . ?
F2 Na2 Na1 40.75(3) 2_664 . ?
S1 Na2 Na1 57.82(2) 13_566 . ?
Na2 Na2 Na1 122.18(2) 9_666 . ?
F1 Na2 Na1 99.44(5) . 6 ?
F1 Na2 Na1 129.51(5) 9_666 6 ?
O1 Na2 Na1 68.66(5) 4_566 6 ?
O1 Na2 Na1 108.10(5) . 6 ?
O2 Na2 Na1 80.82(5) 16_545 6 ?
O2 Na2 Na1 39.46(4) 13_566 6 ?
F2 Na2 Na1 40.75(3) 3_646 6 ?
F2 Na2 Na1 156.37(6) 2_664 6 ?
S1 Na2 Na1 57.82(2) 13_566 6 ?
Na2 Na2 Na1 122.18(2) 9_666 6 ?
Na1 Na2 Na1 115.64(4) . 6 ?
Sb1 F1 Na2 120.84(6) . 9_666 ?
Sb1 F1 Na2 120.84(6) . . ?
Na2 F1 Na2 97.39(9) 9_666 . ?
Sb1 F2 Na1 128.52(7) . 2_665 ?
Sb1 F2 Na2 122.53(8) . 2_665 ?
Na1 F2 Na2 91.00(6) 2_665 2_665 ?
S1 O1 Na2 142.49(11) . . ?
S1 O1 Sb1 116.28(9) . . ?
Na2 O1 Sb1 100.35(7) . . ?
S1 O2 Na1 134.56(10) . . ?
S1 O2 Na1 115.80(9) . 10_566 ?
Na1 O2 Na1 96.55(5) . 10_566 ?
S1 O2 Na2 96.08(8) . 13_566 ?
Na1 O2 Na2 109.32(7) . 13_566 ?
Na1 O2 Na2 100.08(6) 10_566 13_566 ?

_refine_diff_density_max         0.432
_refine_diff_density_min         -1.473
_refine_diff_density_rms         0.171

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1859397'
_audit_update_record             
;
2018-07-31 deposited with the CCDC.
2018-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'F6 K4 O8 S2 Sb2'
_chemical_formula_weight         706.02

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   5.60751(13)
_cell_length_b                   9.0874(2)
_cell_length_c                   14.1966(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     723.43(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1637
_cell_measurement_theta_min      5.7700
_cell_measurement_theta_max      72.2630

_exptl_crystal_description       rod-like
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.241
_exptl_crystal_F_000             656
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    43.670
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2388
_diffrn_reflns_av_unetI/netI     0.0647
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         5.781
_diffrn_reflns_theta_max         66.995
_diffrn_reflns_theta_full        66.995
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 0.964
_reflns_number_total             1248
_reflns_number_gt                1213
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.594
_reflns_Friedel_fraction_max     0.910
_reflns_Friedel_fraction_full    0.910

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0957P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0080(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 431 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.053(19)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1248
_refine_ls_number_parameters     101
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0533
_refine_ls_wR_factor_ref         0.1324
_refine_ls_wR_factor_gt          0.1310
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.47303(18) 0.55762(8) 0.47751(5) 0.0249(5) Uani 1 1 d . . . . .
K1 K -0.0034(6) 0.5089(4) 0.6910(2) 0.0344(8) Uani 1 1 d . . . . .
K2 K 0.4809(6) 0.1863(3) 0.6114(2) 0.0318(8) Uani 1 1 d . . . . .
S1 S 0.5227(7) 0.7935(3) 0.6614(2) 0.0257(8) Uani 1 1 d . . . . .
F1 F 0.4623(18) 0.4070(10) 0.3760(5) 0.036(2) Uani 1 1 d . . . . .
F2 F 0.2532(14) 0.4224(9) 0.5389(5) 0.0263(17) Uani 1 1 d . . . . .
F3 F 0.7162(16) 0.4261(10) 0.5357(7) 0.035(2) Uani 1 1 d . . . . .
O1 O 0.742(2) 0.7733(13) 0.7135(9) 0.042(3) Uani 1 1 d . . . . .
O2 O 0.573(3) 0.8777(13) 0.5742(9) 0.043(3) Uani 1 1 d . . . . .
O3 O 0.427(3) 0.6504(13) 0.6313(8) 0.048(3) Uani 1 1 d . . . . .
O4 O 0.347(3) 0.868(3) 0.7174(14) 0.082(6) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 F2 1.946(8) . ?
Sb1 F1 1.989(8) . ?
Sb1 F3 1.992(9) . ?
Sb1 O3 2.355(12) . ?
Sb1 O2 2.434(14) 4_466 ?
Sb1 K2 3.758(3) 4_456 ?
Sb1 K2 3.823(3) 4_556 ?
Sb1 K2 3.873(3) . ?
Sb1 K1 4.064(3) . ?
Sb1 K1 4.116(3) 2_564 ?
K1 O4 2.653(16) 3_546 ?
K1 F2 2.712(8) . ?
K1 F1 2.745(8) 2_565 ?
K1 F3 2.810(10) 1_455 ?
K1 O1 2.812(13) 1_455 ?
K1 O3 2.863(14) . ?
K1 O1 2.927(13) 3_646 ?
K1 S1 3.732(5) 1_455 ?
K1 Sb1 4.116(3) 2_565 ?
K1 K2 4.153(4) . ?
K1 K2 4.200(5) 3_556 ?
K2 F2 2.701(9) . ?
K2 F3 2.758(10) 4_456 ?
K2 F3 2.765(10) . ?
K2 F2 2.803(9) 4_556 ?
K2 F1 2.835(11) 4_556 ?
K2 O1 2.894(13) 3_646 ?
K2 O2 2.899(12) 1_545 ?
K2 F1 3.035(11) 4_456 ?
K2 O4 3.09(2) 3_646 ?
K2 O4 3.35(3) 1_545 ?
K2 S1 3.370(4) 3_646 ?
K2 S1 3.646(4) 1_545 ?
S1 O4 1.436(16) . ?
S1 O1 1.448(12) . ?
S1 O3 1.470(12) . ?
S1 O2 1.482(12) . ?
S1 K2 3.370(4) 3_656 ?
S1 K2 3.646(4) 1_565 ?
S1 K1 3.732(5) 1_655 ?
F1 K1 2.745(8) 2_564 ?
F1 K2 2.835(11) 4_456 ?
F1 K2 3.035(11) 4_556 ?
F2 K2 2.803(9) 4_456 ?
F3 K2 2.758(10) 4_556 ?
F3 K1 2.810(10) 1_655 ?
O1 K1 2.812(13) 1_655 ?
O1 K2 2.894(13) 3_656 ?
O1 K1 2.927(13) 3_656 ?
O2 Sb1 2.434(14) 4_566 ?
O2 K2 2.899(12) 1_565 ?
O4 K1 2.653(16) 3_556 ?
O4 K2 3.09(2) 3_656 ?
O4 K2 3.35(3) 1_565 ?

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
_geom_angle_publ_flag
F2 Sb1 F1 82.6(4) . . ?
F2 Sb1 F3 82.5(4) . . ?
F1 Sb1 F3 84.8(4) . . ?
F2 Sb1 O3 75.0(4) . . ?
F1 Sb1 O3 156.2(4) . . ?
F3 Sb1 O3 84.6(5) . . ?
F2 Sb1 O2 72.8(4) . 4_466 ?
F1 Sb1 O2 85.4(4) . 4_466 ?
F3 Sb1 O2 154.3(4) . 4_466 ?
O3 Sb1 O2 95.3(5) . 4_466 ?
F2 Sb1 K2 46.6(2) . 4_456 ?
F1 Sb1 K2 47.8(3) . 4_456 ?
F3 Sb1 K2 106.7(3) . 4_456 ?
O3 Sb1 K2 116.2(3) . 4_456 ?
O2 Sb1 K2 50.5(3) 4_466 4_456 ?
F2 Sb1 K2 104.7(2) . 4_556 ?
F1 Sb1 K2 52.0(3) . 4_556 ?
F3 Sb1 K2 43.9(3) . 4_556 ?
O3 Sb1 K2 126.5(4) . 4_556 ?
O2 Sb1 K2 136.7(3) 4_466 4_556 ?
K2 Sb1 K2 95.42(7) 4_456 4_556 ?
F2 Sb1 K2 40.3(3) . . ?
F1 Sb1 K2 75.9(3) . . ?
F3 Sb1 K2 42.8(3) . . ?
O3 Sb1 K2 81.9(3) . . ?
O2 Sb1 K2 111.7(3) 4_466 . ?
K2 Sb1 K2 70.08(6) 4_456 . ?
K2 Sb1 K2 69.41(6) 4_556 . ?
F2 Sb1 K1 35.0(2) . . ?
F1 Sb1 K1 116.5(3) . . ?
F3 Sb1 K1 94.3(3) . . ?
O3 Sb1 K1 43.6(3) . . ?
O2 Sb1 K1 69.2(3) 4_466 . ?
K2 Sb1 K1 72.75(7) 4_456 . ?
K2 Sb1 K1 132.27(7) 4_556 . ?
K2 Sb1 K1 63.05(7) . . ?
F2 Sb1 K1 112.1(2) . 2_564 ?
F1 Sb1 K1 35.3(3) . 2_564 ?
F3 Sb1 K1 107.1(3) . 2_564 ?
O3 Sb1 K1 166.8(3) . 2_564 ?
O2 Sb1 K1 77.0(3) 4_466 2_564 ?
K2 Sb1 K1 67.16(7) 4_456 2_564 ?
K2 Sb1 K1 63.76(7) 4_556 2_564 ?
K2 Sb1 K1 110.88(6) . 2_564 ?
K1 Sb1 K1 138.43(4) . 2_564 ?
O4 K1 F2 129.4(6) 3_546 . ?
O4 K1 F1 74.1(5) 3_546 2_565 ?
F2 K1 F1 142.9(3) . 2_565 ?
O4 K1 F3 81.3(5) 3_546 1_455 ?
F2 K1 F3 66.1(3) . 1_455 ?
F1 K1 F3 150.7(3) 2_565 1_455 ?
O4 K1 O1 89.4(6) 3_546 1_455 ?
F2 K1 O1 127.4(3) . 1_455 ?
F1 K1 O1 72.3(3) 2_565 1_455 ?
F3 K1 O1 91.9(3) 1_455 1_455 ?
O4 K1 O3 166.8(5) 3_546 . ?
F2 K1 O3 56.4(3) . . ?
F1 K1 O3 95.0(3) 2_565 . ?
F3 K1 O3 111.1(3) 1_455 . ?
O1 K1 O3 94.4(4) 1_455 . ?
O4 K1 O1 77.4(5) 3_546 3_646 ?
F2 K1 O1 83.8(3) . 3_646 ?
F1 K1 O1 73.6(3) 2_565 3_646 ?
F3 K1 O1 116.6(3) 1_455 3_646 ?
O1 K1 O1 145.70(17) 1_455 3_646 ?
O3 K1 O1 92.5(4) . 3_646 ?
O4 K1 S1 82.8(5) 3_546 1_455 ?
F2 K1 S1 119.3(2) . 1_455 ?
F1 K1 S1 88.5(2) 2_565 1_455 ?
F3 K1 S1 72.5(2) 1_455 1_455 ?
O1 K1 S1 19.9(3) 1_455 1_455 ?
O3 K1 S1 104.8(3) . 1_455 ?
O1 K1 S1 156.3(3) 3_646 1_455 ?
O4 K1 Sb1 153.5(5) 3_546 . ?
F2 K1 Sb1 24.33(18) . . ?
F1 K1 Sb1 128.9(2) 2_565 . ?
F3 K1 Sb1 79.2(2) 1_455 . ?
O1 K1 Sb1 109.0(3) 1_455 . ?
O3 K1 Sb1 34.5(2) . . ?
O1 K1 Sb1 95.5(3) 3_646 . ?
S1 K1 Sb1 107.97(9) 1_455 . ?
O4 K1 Sb1 58.3(5) 3_546 2_565 ?
F2 K1 Sb1 136.3(2) . 2_565 ?
F1 K1 Sb1 24.75(19) 2_565 2_565 ?
F3 K1 Sb1 139.4(2) 1_455 2_565 ?
O1 K1 Sb1 92.0(3) 1_455 2_565 ?
O3 K1 Sb1 108.9(3) . 2_565 ?
O1 K1 Sb1 54.1(2) 3_646 2_565 ?
S1 K1 Sb1 104.04(9) 1_455 2_565 ?
Sb1 K1 Sb1 136.53(9) . 2_565 ?
O4 K1 K2 105.4(5) 3_546 . ?
F2 K1 K2 39.78(19) . . ?
F1 K1 K2 113.7(2) 2_565 . ?
F3 K1 K2 87.9(2) 1_455 . ?
O1 K1 K2 164.9(3) 1_455 . ?
O3 K1 K2 71.7(3) . . ?
O1 K1 K2 44.2(2) 3_646 . ?
S1 K1 K2 157.54(11) 1_455 . ?
Sb1 K1 K2 56.23(6) . . ?
Sb1 K1 K2 97.95(8) 2_565 . ?
O4 K1 K2 52.8(6) 3_546 3_556 ?
F2 K1 K2 169.0(2) . 3_556 ?
F1 K1 K2 46.2(2) 2_565 3_556 ?
F3 K1 K2 105.7(2) 1_455 3_556 ?
O1 K1 K2 43.4(3) 1_455 3_556 ?
O3 K1 K2 124.2(3) . 3_556 ?
O1 K1 K2 106.9(3) 3_646 3_556 ?
S1 K1 K2 49.86(7) 1_455 3_556 ?
Sb1 K1 K2 151.10(10) . 3_556 ?
Sb1 K1 K2 54.73(6) 2_565 3_556 ?
K2 K1 K2 150.42(10) . 3_556 ?
F2 K2 F3 75.6(3) . 4_456 ?
F2 K2 F3 56.7(2) . . ?
F3 K2 F3 104.8(2) 4_456 . ?
F2 K2 F2 104.33(19) . 4_556 ?
F3 K2 F2 65.6(3) 4_456 4_556 ?
F3 K2 F2 73.9(3) . 4_556 ?
F2 K2 F1 135.4(3) . 4_556 ?
F3 K2 F1 116.7(3) 4_456 4_556 ?
F3 K2 F1 78.8(3) . 4_556 ?
F2 K2 F1 54.8(2) 4_556 4_556 ?
F2 K2 O1 84.6(3) . 3_646 ?
F3 K2 O1 121.3(3) 4_456 3_646 ?
F3 K2 O1 108.9(3) . 3_646 ?
F2 K2 O1 170.3(3) 4_556 3_646 ?
F1 K2 O1 116.0(3) 4_556 3_646 ?
F2 K2 O2 141.5(3) . 1_545 ?
F3 K2 O2 66.4(3) 4_456 1_545 ?
F3 K2 O2 127.4(4) . 1_545 ?
F2 K2 O2 54.8(3) 4_556 1_545 ?
F1 K2 O2 63.5(3) 4_556 1_545 ?
O1 K2 O2 119.8(4) 3_646 1_545 ?
F2 K2 F1 78.0(3) . 4_456 ?
F3 K2 F1 54.9(2) 4_456 4_456 ?
F3 K2 F1 134.5(3) . 4_456 ?
F2 K2 F1 118.0(2) 4_556 4_456 ?
F1 K2 F1 145.6(4) 4_556 4_456 ?
O1 K2 F1 67.1(3) 3_646 4_456 ?
O2 K2 F1 84.9(3) 1_545 4_456 ?
F2 K2 O4 91.4(5) . 3_646 ?
F3 K2 O4 163.9(5) 4_456 3_646 ?
F3 K2 O4 74.7(4) . 3_646 ?
F2 K2 O4 128.0(4) 4_556 3_646 ?
F1 K2 O4 79.1(4) 4_556 3_646 ?
O1 K2 O4 46.7(4) 3_646 3_646 ?
O2 K2 O4 127.1(5) 1_545 3_646 ?
F1 K2 O4 113.7(4) 4_456 3_646 ?
F2 K2 O4 138.7(4) . 1_545 ?
F3 K2 O4 84.2(4) 4_456 1_545 ?
F3 K2 O4 164.5(4) . 1_545 ?
F2 K2 O4 99.2(3) 4_556 1_545 ?
F1 K2 O4 85.8(4) 4_556 1_545 ?
O1 K2 O4 75.7(4) 3_646 1_545 ?
O2 K2 O4 44.4(4) 1_545 1_545 ?
F1 K2 O4 61.1(4) 4_456 1_545 ?
O4 K2 O4 100.2(3) 3_646 1_545 ?
F2 K2 S1 97.6(2) . 3_646 ?
F3 K2 S1 146.0(2) 4_456 3_646 ?
F3 K2 S1 98.4(2) . 3_646 ?
F2 K2 S1 146.5(2) 4_556 3_646 ?
F1 K2 S1 91.81(18) 4_556 3_646 ?
O1 K2 S1 25.3(2) 3_646 3_646 ?
O2 K2 S1 117.1(3) 1_545 3_646 ?
F1 K2 S1 91.05(17) 4_456 3_646 ?
O4 K2 S1 25.2(3) 3_646 3_646 ?
O4 K2 S1 79.5(3) 1_545 3_646 ?
F2 K2 S1 151.9(2) . 1_545 ?
F3 K2 S1 79.6(2) 4_456 1_545 ?
F3 K2 S1 144.7(2) . 1_545 ?
F2 K2 S1 76.61(19) 4_556 1_545 ?
F1 K2 S1 68.5(2) 4_556 1_545 ?
O1 K2 S1 97.3(3) 3_646 1_545 ?
O2 K2 S1 22.7(3) 1_545 1_545 ?
F1 K2 S1 77.10(19) 4_456 1_545 ?
O4 K2 S1 110.4(4) 3_646 1_545 ?
O4 K2 S1 23.2(3) 1_545 1_545 ?
S1 K2 S1 95.57(9) 3_646 1_545 ?
O4 S1 O1 111.2(10) . . ?
O4 S1 O3 108.9(12) . . ?
O1 S1 O3 110.2(8) . . ?
O4 S1 O2 110.5(11) . . ?
O1 S1 O2 109.4(7) . . ?
O3 S1 O2 106.5(7) . . ?
O4 S1 K2 66.5(9) . 3_656 ?
O1 S1 K2 58.6(5) . 3_656 ?
O3 S1 K2 91.1(5) . 3_656 ?
O2 S1 K2 161.8(5) . 3_656 ?
O4 S1 K2 66.7(10) . 1_565 ?
O1 S1 K2 106.2(5) . 1_565 ?
O3 S1 K2 141.8(6) . 1_565 ?
O2 S1 K2 49.0(5) . 1_565 ?
K2 S1 K2 117.98(11) 3_656 1_565 ?
O4 S1 K1 138.8(9) . 1_655 ?
O1 S1 K1 41.3(5) . 1_655 ?
O3 S1 K1 71.3(6) . 1_655 ?
O2 S1 K1 108.5(6) . 1_655 ?
K2 S1 K1 72.30(10) 3_656 1_655 ?
K2 S1 K1 138.25(14) 1_565 1_655 ?
Sb1 F1 K1 120.0(4) . 2_564 ?
Sb1 F1 K2 100.9(4) . 4_456 ?
K1 F1 K2 102.9(3) 2_564 4_456 ?
Sb1 F1 K2 96.9(4) . 4_556 ?
K1 F1 K2 93.1(3) 2_564 4_556 ?
K2 F1 K2 145.6(3) 4_456 4_556 ?
Sb1 F2 K2 111.9(3) . . ?
Sb1 F2 K1 120.6(4) . . ?
K2 F2 K1 100.2(3) . . ?
Sb1 F2 K2 103.1(3) . 4_456 ?
K2 F2 K2 105.5(3) . 4_456 ?
K1 F2 K2 114.8(3) . 4_456 ?
Sb1 F3 K2 106.0(4) . 4_556 ?
Sb1 F3 K2 107.9(4) . . ?
K2 F3 K2 105.0(3) 4_556 . ?
Sb1 F3 K1 123.2(4) . 1_655 ?
K2 F3 K1 113.1(3) 4_556 1_655 ?
K2 F3 K1 100.0(3) . 1_655 ?
S1 O1 K1 118.8(7) . 1_655 ?
S1 O1 K2 96.1(6) . 3_656 ?
K1 O1 K2 94.8(3) 1_655 3_656 ?
S1 O1 K1 124.7(7) . 3_656 ?
K1 O1 K1 115.1(4) 1_655 3_656 ?
K2 O1 K1 91.0(4) 3_656 3_656 ?
S1 O2 Sb1 123.4(7) . 4_566 ?
S1 O2 K2 108.3(7) . 1_565 ?
Sb1 O2 K2 89.1(4) 4_566 1_565 ?
S1 O3 Sb1 123.1(7) . . ?
S1 O3 K1 128.3(8) . . ?
Sb1 O3 K1 101.9(4) . . ?
S1 O4 K1 175.7(13) . 3_556 ?
S1 O4 K2 88.3(10) . 3_656 ?
K1 O4 K2 95.7(6) 3_556 3_656 ?
S1 O4 K2 90.1(10) . 1_565 ?
K1 O4 K2 88.0(6) 3_556 1_565 ?
K2 O4 K2 138.1(7) 3_656 1_565 ?

_refine_diff_density_max         1.466
_refine_diff_density_min         -1.440
_refine_diff_density_rms         0.288

