# Supplementary Information (SI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_xi097
_database_code_depnum_ccdc_archive 'CCDC 2368718'
loop_
_audit_author_name
_audit_author_address
'Valentin Bockmair'
;Ludwig Maximilian University
Germany
;
_audit_update_record             
;
2024-07-08 deposited with the CCDC.	2024-08-21 downloaded from the CCDC.
;
_audit_block_code                ?
_audit_creation_method           SHELXL-2018/3
_audit_creation_date             2022-01-17
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        '[FS(OH)(OMe)][SbF6]'
_chemical_name_common            'methylated fluorosulfurous acid'
_chemical_melting_point          ?
_chemical_formula_moiety         'F6 Sb, C H4 F O2 S'
_chemical_formula_sum            'C H4 F7 O2 S Sb'
_chemical_formula_weight         334.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Sb Sb -0.5866 1.5461 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'

_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, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'

_cell_length_a                   13.5681(5)
_cell_length_b                   10.8817(5)
_cell_length_c                   22.3347(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3297.6(2)
_cell_formula_units_Z            16
_cell_measurement_temperature    102(2)
_cell_measurement_reflns_used    5816
_cell_measurement_theta_min      1.8600
_cell_measurement_theta_max      31.9830

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.698
_exptl_crystal_F_000             2496
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.438
_exptl_crystal_size_mid          0.365
_exptl_crystal_size_min          0.163
_exptl_absorpt_coefficient_mu    3.683
_shelx_estimated_absorpt_T_min   0.295
_shelx_estimated_absorpt_T_max   0.585
_exptl_absorpt_correction_T_min  0.67253
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      102(2) # in K
_diffrn_source_type              'Spellman generator'
_diffrn_source_power             ? # in kW
_diffrn_source_voltage           50 # kV
_diffrn_source_current           40 # mA
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_collimation    0.5
_diffrn_measurement_device       'CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809

_diffrn_reflns_number            13848
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.824
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_point_group_measured_fraction_full 0.913
_reflns_number_total             6546
_reflns_number_gt                5979
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.756
_reflns_Friedel_fraction_max     0.797
_reflns_Friedel_fraction_full    0.821

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_structure_solution    
'SHELXT (Sheldrick, G. M. (2015). Acta Cryst. A71, 3-8.)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'ORTEP-3, Version ORTEP-III (1.0.3), L. J. Farrugia, J. Appl. Cryst. (2012),45, 849-854'
_computing_publication_material  
'PLATON (A.L.Spek, Acta Cryst. 2009, D65, 148-155.) '
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0186P)²+5.7870P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.46(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6546
_refine_ls_number_parameters     450
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0279
_refine_ls_wR_factor_ref         0.0665
_refine_ls_wR_factor_gt          0.0635
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.101
_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 0.26910(4) 0.30620(5) 0.36916(2) 0.01688(13) Uani 1 1 d . . . . .
Sb2 Sb 0.75351(7) 0.18929(5) 0.64501(2) 0.01731(13) Uani 1 1 d . . . . .
Sb3 Sb 0.25292(7) 0.31255(4) 0.61733(2) 0.01655(13) Uani 1 1 d . . . . .
Sb4 Sb 0.28069(4) 0.81274(5) 0.39513(2) 0.01755(13) Uani 1 1 d . . . . .
S4 S 0.59980(16) 0.4870(2) 0.48385(10) 0.0191(4) Uani 1 1 d . . . . .
S1 S 0.42995(15) 0.5076(2) 0.23399(9) 0.0199(4) Uani 1 1 d . . . . .
S3 S 0.59762(17) 0.9880(2) 0.52418(10) 0.0211(4) Uani 1 1 d . . . . .
S2 S 0.59341(19) 0.9728(2) 0.27711(10) 0.0237(5) Uani 1 1 d . . . . .
F5 F 0.3955(4) 0.2433(5) 0.3573(2) 0.0298(12) Uani 1 1 d . . . . .
F21 F 0.3846(4) 0.2919(5) 0.5956(3) 0.0328(12) Uani 1 1 d . . . . .
F8 F 0.1407(4) 0.3633(4) 0.3824(2) 0.0267(12) Uani 1 1 d . . . . .
F9 F 0.2248(4) 0.2195(5) 0.3022(2) 0.0319(13) Uani 1 1 d . . . . .
F3 F 0.5253(4) 0.9134(5) 0.5642(2) 0.0348(13) Uani 1 1 d . . . . .
F6 F 0.2972(4) 0.4434(4) 0.3217(2) 0.0322(13) Uani 1 1 d . . . . .
F19 F 0.2627(4) 0.1702(5) 0.6672(2) 0.0307(13) Uani 1 1 d . . . . .
F22 F 0.2414(4) 0.4514(5) 0.5684(2) 0.0315(13) Uani 1 1 d . . . . .
F10 F 0.3108(4) 0.3858(5) 0.4384(2) 0.0333(12) Uani 1 1 d . . . . .
F14 F 0.6913(4) 0.3154(5) 0.6869(2) 0.0366(13) Uani 1 1 d . . . . .
F1 F 0.4954(4) 0.5586(5) 0.1829(2) 0.0332(12) Uani 1 1 d . . . . .
F18 F 0.1204(4) 0.3273(5) 0.6401(2) 0.0288(12) Uani 1 1 d . . . . .
F7 F 0.2359(4) 0.1662(5) 0.4170(2) 0.0319(12) Uani 1 1 d . . . . .
F26 F 0.3299(5) 0.9497(5) 0.3549(2) 0.0368(13) Uani 1 1 d . . . . .
F11 F 0.6310(4) 0.1149(5) 0.6333(2) 0.0307(12) Uani 1 1 d . . . . .
F24 F 0.1535(4) 0.8471(5) 0.3672(3) 0.0340(12) Uani 1 1 d . . . . .
F20 F 0.2894(4) 0.4100(5) 0.6822(2) 0.0326(12) Uani 1 1 d . . . . .
F4 F 0.5299(4) 0.4323(5) 0.4353(2) 0.0304(13) Uani 1 1 d . . . . .
F13 F 0.8147(4) 0.0659(5) 0.6011(2) 0.0339(12) Uani 1 1 d . . . . .
F15 F 0.7319(4) 0.2795(5) 0.5729(2) 0.0299(12) Uani 1 1 d . . . . .
F12 F 0.7699(4) 0.1011(5) 0.7158(2) 0.0311(12) Uani 1 1 d . . . . .
F23 F 0.3045(4) 0.7170(5) 0.3253(2) 0.0328(13) Uani 1 1 d . . . . .
F17 F 0.2146(4) 0.2107(5) 0.5538(2) 0.0283(12) Uani 1 1 d . . . . .
F2 F 0.5270(5) 0.8892(6) 0.3171(3) 0.0488(17) Uani 1 1 d . . . . .
O1 O 0.4527(5) 0.6074(6) 0.2804(3) 0.0260(15) Uani 1 1 d D . . . .
O4 O 0.5275(5) 1.0854(6) 0.2695(3) 0.0278(16) Uani 1 1 d . . . . .
F16 F 0.8746(4) 0.2683(5) 0.6549(3) 0.0392(14) Uani 1 1 d . . . . .
O3 O 0.5805(5) 0.9019(6) 0.2186(3) 0.0299(16) Uani 1 1 d D . . . .
O6 O 0.5390(5) 1.1047(6) 0.5143(3) 0.0268(14) Uani 1 1 d . . . . .
O8 O 0.5397(5) 0.5966(5) 0.5045(3) 0.0239(14) Uani 1 1 d . . . . .
O2 O 0.4899(5) 0.3983(5) 0.2536(3) 0.0234(13) Uani 1 1 d . . . . .
O5 O 0.5836(5) 0.9147(6) 0.4668(3) 0.0291(16) Uani 1 1 d D . . . .
F25 F 0.2309(4) 0.6726(5) 0.4331(3) 0.0379(14) Uani 1 1 d . . . . .
F28 F 0.2561(4) 0.9067(5) 0.4638(2) 0.0319(13) Uani 1 1 d . . . . .
F27 F 0.4066(4) 0.7736(5) 0.4212(3) 0.0405(14) Uani 1 1 d . . . . .
O7 O 0.5812(5) 0.3887(6) 0.5310(3) 0.0279(15) Uani 1 1 d D . . . .
C2 C 0.4322(7) 1.0837(9) 0.2368(4) 0.027(2) Uani 1 1 d . . . . .
H6 H 0.439019 1.034565 0.200297 0.041 Uiso 1 1 calc R U . . .
H8 H 0.413392 1.167871 0.226249 0.041 Uiso 1 1 calc R U . . .
H7 H 0.381159 1.047448 0.262420 0.041 Uiso 1 1 calc R U . . .
C4 C 0.4404(8) 0.5837(10) 0.5329(5) 0.033(2) Uani 1 1 d . . . . .
H15 H 0.406125 0.662913 0.531715 0.049 Uiso 1 1 calc R U . . .
H16 H 0.448239 0.557458 0.574607 0.049 Uiso 1 1 calc R U . . .
H14 H 0.401859 0.522225 0.511002 0.049 Uiso 1 1 calc R U . . .
C3 C 0.4404(8) 1.1061(10) 0.4856(5) 0.036(3) Uani 1 1 d . . . . .
H10 H 0.447261 1.088538 0.442767 0.054 Uiso 1 1 calc R U . . .
H12 H 0.410213 1.187207 0.490897 0.054 Uiso 1 1 calc R U . . .
H11 H 0.398449 1.043437 0.504183 0.054 Uiso 1 1 calc R U . . .
C1 C 0.5903(8) 0.4074(10) 0.2799(4) 0.027(2) Uani 1 1 d . . . . .
H2 H 0.631142 0.461105 0.254907 0.040 Uiso 1 1 calc R U . . .
H3 H 0.620039 0.325461 0.281759 0.040 Uiso 1 1 calc R U . . .
H4 H 0.585774 0.441748 0.320371 0.040 Uiso 1 1 calc R U . . .
H1 H 0.399(4) 0.640(9) 0.290(5) 0.040 Uiso 1 1 d D U . . .
H13 H 0.639(3) 0.366(9) 0.537(5) 0.040 Uiso 1 1 d D U . . .
H5 H 0.634(4) 0.881(9) 0.202(4) 0.040 Uiso 1 1 d D U . . .
H9 H 0.639(4) 0.884(9) 0.458(5) 0.040 Uiso 1 1 d D 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 F10 1.861(5) . ?
Sb1 F5 1.865(5) . ?
Sb1 F9 1.869(5) . ?
Sb1 F6 1.870(5) . ?
Sb1 F8 1.873(5) . ?
Sb1 F7 1.914(5) . ?
Sb2 F13 1.859(5) . ?
Sb2 F14 1.863(5) . ?
Sb2 F12 1.863(5) . ?
Sb2 F11 1.867(5) . ?
Sb2 F16 1.868(5) . ?
Sb2 F15 1.909(5) . ?
Sb3 F20 1.863(5) . ?
Sb3 F21 1.865(5) . ?
Sb3 F22 1.871(5) . ?
Sb3 F17 1.874(5) . ?
Sb3 F18 1.875(5) . ?
Sb3 F19 1.912(5) . ?
Sb4 F27 1.855(5) . ?
Sb4 F26 1.864(5) . ?
Sb4 F25 1.871(5) . ?
Sb4 F24 1.873(5) . ?
Sb4 F28 1.874(5) . ?
Sb4 F23 1.903(5) . ?
S4 O8 1.517(6) . ?
S4 O7 1.522(7) . ?
S4 F4 1.559(6) . ?
S1 O2 1.507(6) . ?
S1 O1 1.532(6) . ?
S1 F1 1.549(5) . ?
S3 O6 1.515(6) . ?
S3 O5 1.521(7) . ?
S3 F3 1.556(6) . ?
S2 O4 1.526(7) . ?
S2 O3 1.528(7) . ?
S2 F2 1.561(6) . ?
O1 H1 0.837(14) . ?
O4 C2 1.486(11) . ?
O3 H5 0.842(14) . ?
O6 C3 1.484(12) . ?
O8 C4 1.496(11) . ?
O2 C1 1.487(11) . ?
O5 H9 0.841(14) . ?
O7 H13 0.839(14) . ?
C2 H6 0.9800 . ?
C2 H8 0.9800 . ?
C2 H7 0.9800 . ?
C4 H15 0.9800 . ?
C4 H16 0.9800 . ?
C4 H14 0.9800 . ?
C3 H10 0.9800 . ?
C3 H12 0.9800 . ?
C3 H11 0.9800 . ?
C1 H2 0.9800 . ?
C1 H3 0.9800 . ?
C1 H4 0.9800 . ?

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
F10 Sb1 F5 90.6(2) . . ?
F10 Sb1 F9 177.0(2) . . ?
F5 Sb1 F9 89.8(2) . . ?
F10 Sb1 F6 92.1(2) . . ?
F5 Sb1 F6 91.4(2) . . ?
F9 Sb1 F6 90.9(2) . . ?
F10 Sb1 F8 89.8(2) . . ?
F5 Sb1 F8 177.7(2) . . ?
F9 Sb1 F8 89.7(2) . . ?
F6 Sb1 F8 90.8(2) . . ?
F10 Sb1 F7 88.8(2) . . ?
F5 Sb1 F7 90.2(2) . . ?
F9 Sb1 F7 88.2(2) . . ?
F6 Sb1 F7 178.1(3) . . ?
F8 Sb1 F7 87.5(2) . . ?
F13 Sb2 F14 178.3(2) . . ?
F13 Sb2 F12 91.3(2) . . ?
F14 Sb2 F12 90.4(2) . . ?
F13 Sb2 F11 90.6(2) . . ?
F14 Sb2 F11 89.2(3) . . ?
F12 Sb2 F11 90.1(2) . . ?
F13 Sb2 F16 90.1(3) . . ?
F14 Sb2 F16 90.0(3) . . ?
F12 Sb2 F16 91.8(2) . . ?
F11 Sb2 F16 178.0(3) . . ?
F13 Sb2 F15 89.7(2) . . ?
F14 Sb2 F15 88.6(2) . . ?
F12 Sb2 F15 178.0(2) . . ?
F11 Sb2 F15 88.2(2) . . ?
F16 Sb2 F15 89.9(3) . . ?
F20 Sb3 F21 90.9(2) . . ?
F20 Sb3 F22 91.0(2) . . ?
F21 Sb3 F22 91.5(2) . . ?
F20 Sb3 F17 178.1(2) . . ?
F21 Sb3 F17 89.9(2) . . ?
F22 Sb3 F17 90.7(2) . . ?
F20 Sb3 F18 89.7(2) . . ?
F21 Sb3 F18 177.9(2) . . ?
F22 Sb3 F18 90.5(2) . . ?
F17 Sb3 F18 89.4(2) . . ?
F20 Sb3 F19 89.4(2) . . ?
F21 Sb3 F19 89.3(3) . . ?
F22 Sb3 F19 179.2(3) . . ?
F17 Sb3 F19 88.9(2) . . ?
F18 Sb3 F19 88.7(2) . . ?
F27 Sb4 F26 90.3(3) . . ?
F27 Sb4 F25 90.2(3) . . ?
F26 Sb4 F25 178.1(2) . . ?
F27 Sb4 F24 178.0(3) . . ?
F26 Sb4 F24 90.6(3) . . ?
F25 Sb4 F24 88.9(3) . . ?
F27 Sb4 F28 91.8(3) . . ?
F26 Sb4 F28 91.3(2) . . ?
F25 Sb4 F28 90.5(2) . . ?
F24 Sb4 F28 90.0(3) . . ?
F27 Sb4 F23 88.5(3) . . ?
F26 Sb4 F23 89.0(2) . . ?
F25 Sb4 F23 89.2(2) . . ?
F24 Sb4 F23 89.6(2) . . ?
F28 Sb4 F23 179.5(3) . . ?
O8 S4 O7 104.7(4) . . ?
O8 S4 F4 100.6(3) . . ?
O7 S4 F4 96.5(4) . . ?
O2 S1 O1 104.7(4) . . ?
O2 S1 F1 100.8(3) . . ?
O1 S1 F1 97.5(4) . . ?
O6 S3 O5 104.6(4) . . ?
O6 S3 F3 101.0(3) . . ?
O5 S3 F3 97.5(4) . . ?
O4 S2 O3 104.1(4) . . ?
O4 S2 F2 101.1(4) . . ?
O3 S2 F2 97.4(4) . . ?
S1 O1 H1 108(8) . . ?
C2 O4 S2 123.7(6) . . ?
S2 O3 H5 114(7) . . ?
C3 O6 S3 123.0(6) . . ?
C4 O8 S4 122.6(6) . . ?
C1 O2 S1 123.8(6) . . ?
S3 O5 H9 107(7) . . ?
S4 O7 H13 100(8) . . ?
O4 C2 H6 109.5 . . ?
O4 C2 H8 109.5 . . ?
H6 C2 H8 109.5 . . ?
O4 C2 H7 109.5 . . ?
H6 C2 H7 109.5 . . ?
H8 C2 H7 109.5 . . ?
O8 C4 H15 109.5 . . ?
O8 C4 H16 109.5 . . ?
H15 C4 H16 109.5 . . ?
O8 C4 H14 109.5 . . ?
H15 C4 H14 109.5 . . ?
H16 C4 H14 109.5 . . ?
O6 C3 H10 109.5 . . ?
O6 C3 H12 109.5 . . ?
H10 C3 H12 109.5 . . ?
O6 C3 H11 109.5 . . ?
H10 C3 H11 109.5 . . ?
H12 C3 H11 109.5 . . ?
O2 C1 H2 109.5 . . ?
O2 C1 H3 109.5 . . ?
H2 C1 H3 109.5 . . ?
O2 C1 H4 109.5 . . ?
H2 C1 H4 109.5 . . ?
H3 C1 H4 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 S2 O4 C2 34.9(8) . . . . ?
F2 S2 O4 C2 -65.7(8) . . . . ?
O5 S3 O6 C3 41.5(8) . . . . ?
F3 S3 O6 C3 -59.4(8) . . . . ?
O7 S4 O8 C4 -37.6(8) . . . . ?
F4 S4 O8 C4 62.1(7) . . . . ?
O1 S1 O2 C1 -37.1(8) . . . . ?
F1 S1 O2 C1 63.7(7) . . . . ?

_refine_diff_density_max         0.988
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.124



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: HF'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
####################################################################### 
# 
# 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_xj014
_database_code_depnum_ccdc_archive 'CCDC 2368721'
loop_
_audit_author_name
_audit_author_address
'Valentin Bockmair'
;Ludwig Maximilian University
Germany
;
_audit_update_record             
;
2024-07-08 deposited with the CCDC.	2024-08-21 downloaded from the CCDC.
;
_audit_block_code                ?
_audit_creation_method           SHELXL-2018/3
_audit_creation_date             2022-04-06
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        '[FS(OMe)2][Sb2F11]'
_chemical_name_common            'methylated fluorosulfurous acid methyl ester'
_chemical_melting_point          ?
_chemical_formula_moiety         'F11 Sb2, C2 H6 F O2 S'
_chemical_formula_sum            'C2 H6 F12 O2 S Sb2'
_chemical_formula_weight         565.63

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.7473(9)
_cell_length_b                   12.6004(9)
_cell_length_c                   10.6035(8)
_cell_angle_alpha                90
_cell_angle_beta                 100.743(8)
_cell_angle_gamma                90
_cell_volume                     1279.49(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    2374
_cell_measurement_theta_min      2.6580
_cell_measurement_theta_max      30.2030

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.936
_exptl_crystal_F_000             1040
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.762
_exptl_crystal_size_mid          0.355
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    4.527
_shelx_estimated_absorpt_T_min   0.130
_shelx_estimated_absorpt_T_max   0.465
_exptl_absorpt_correction_T_min  0.07109
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.517
_oxdiff_exptl_absorpt_empirical_full_max 9.424
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      103(2) # in K
_diffrn_source_type              'Spellman generator'
_diffrn_source_power             ? # in kW
_diffrn_source_voltage           50 # kV
_diffrn_source_current           40 # mA
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_collimation    0.5
_diffrn_measurement_device       'CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809

_diffrn_reflns_number            8759
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.607
_diffrn_reflns_theta_max         24.407
_diffrn_reflns_theta_full        24.407
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2104
_reflns_number_gt                1743
_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       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_structure_solution    
'SHELXT (Sheldrick, G. M. (2015). Acta Cryst. A71, 3-8.)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'ORTEP-3, Version ORTEP-III (1.0.3), L. J. Farrugia, J. Appl. Cryst. (2012),45, 849-854'
_computing_publication_material  
'PLATON (A.L.Spek, Acta Cryst. 2009, D65, 148-155.) '
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0454P)²+0.8942P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2104
_refine_ls_number_parameters     174
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.0894
_refine_ls_wR_factor_gt          0.0830
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_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 0.73971(5) 0.49278(4) 0.44094(4) 0.02308(17) Uani 1 1 d . . . . .
Sb2 Sb 0.90008(5) 0.60436(4) 0.15901(4) 0.02650(17) Uani 1 1 d . . . . .
S1 S 0.3948(2) 0.71022(15) 0.26172(18) 0.0309(5) Uani 1 1 d . . . . .
F7 F 0.8506(4) 0.5088(3) 0.2978(4) 0.0278(10) Uani 1 1 d . . . . .
F3 F 0.6609(4) 0.6246(3) 0.3921(4) 0.0295(10) Uani 1 1 d . . . . .
F1 F 0.5103(5) 0.7940(3) 0.2535(4) 0.0352(11) Uani 1 1 d . . . . .
F11 F 1.0859(5) 0.5692(4) 0.2210(4) 0.0417(12) Uani 1 1 d . . . . .
F9 F 0.7092(5) 0.6270(4) 0.1105(4) 0.0443(12) Uani 1 1 d . . . . .
F8 F 0.8785(5) 0.4836(4) 0.0578(4) 0.0435(12) Uani 1 1 d . . . . .
F6 F 0.8275(5) 0.3625(3) 0.4738(4) 0.0351(11) Uani 1 1 d . . . . .
F5 F 0.8887(4) 0.5617(3) 0.5429(4) 0.0320(10) Uani 1 1 d . . . . .
F2 F 0.6410(5) 0.4771(4) 0.5734(4) 0.0380(11) Uani 1 1 d . . . . .
F12 F 0.9433(5) 0.6930(4) 0.0317(4) 0.0387(11) Uani 1 1 d . . . . .
F10 F 0.9133(6) 0.7111(3) 0.2795(4) 0.0443(12) Uani 1 1 d . . . . .
F4 F 0.6064(5) 0.4317(4) 0.3150(4) 0.0407(12) Uani 1 1 d . . . . .
O1 O 0.4075(6) 0.6353(4) 0.1524(5) 0.0349(13) Uani 1 1 d . . . . .
O2 O 0.2648(5) 0.7754(4) 0.2052(5) 0.0337(13) Uani 1 1 d . . . . .
C2 C 0.2046(9) 0.8451(7) 0.2943(8) 0.038(2) Uani 1 1 d . . . . .
H4 H 0.193677 0.804559 0.370610 0.057 Uiso 1 1 calc R U . . .
H6 H 0.113293 0.871395 0.251007 0.057 Uiso 1 1 calc R U . . .
H5 H 0.267325 0.905317 0.319841 0.057 Uiso 1 1 calc R U . . .
C1 C 0.3916(9) 0.6724(7) 0.0185(7) 0.041(2) Uani 1 1 d . . . . .
H3 H 0.295589 0.696905 -0.011359 0.061 Uiso 1 1 calc R U . . .
H1 H 0.412061 0.613928 -0.036019 0.061 Uiso 1 1 calc R U . . .
H2 H 0.456527 0.731055 0.013948 0.061 Uiso 1 1 calc 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 F4 1.849(4) . ?
Sb1 F6 1.854(4) . ?
Sb1 F2 1.855(4) . ?
Sb1 F5 1.857(4) . ?
Sb1 F3 1.863(4) . ?
Sb1 F7 2.031(4) . ?
Sb2 F10 1.843(4) . ?
Sb2 F8 1.852(4) . ?
Sb2 F9 1.858(4) . ?
Sb2 F12 1.860(4) . ?
Sb2 F11 1.861(4) . ?
Sb2 F7 2.028(4) . ?
S1 O1 1.517(6) . ?
S1 O2 1.535(5) . ?
S1 F1 1.558(5) . ?
O1 C1 1.476(9) . ?
O2 C2 1.488(9) . ?

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
F4 Sb1 F6 90.3(2) . . ?
F4 Sb1 F2 96.2(2) . . ?
F6 Sb1 F2 92.8(2) . . ?
F4 Sb1 F5 169.6(2) . . ?
F6 Sb1 F5 91.20(19) . . ?
F2 Sb1 F5 94.0(2) . . ?
F4 Sb1 F3 88.44(19) . . ?
F6 Sb1 F3 173.66(19) . . ?
F2 Sb1 F3 93.5(2) . . ?
F5 Sb1 F3 88.95(18) . . ?
F4 Sb1 F7 84.37(19) . . ?
F6 Sb1 F7 86.40(18) . . ?
F2 Sb1 F7 179.03(18) . . ?
F5 Sb1 F7 85.47(18) . . ?
F3 Sb1 F7 87.29(17) . . ?
F10 Sb2 F8 170.9(2) . . ?
F10 Sb2 F9 91.0(2) . . ?
F8 Sb2 F9 88.1(2) . . ?
F10 Sb2 F12 94.0(2) . . ?
F8 Sb2 F12 95.1(2) . . ?
F9 Sb2 F12 93.3(2) . . ?
F10 Sb2 F11 89.5(2) . . ?
F8 Sb2 F11 90.4(2) . . ?
F9 Sb2 F11 173.1(2) . . ?
F12 Sb2 F11 93.6(2) . . ?
F10 Sb2 F7 85.75(19) . . ?
F8 Sb2 F7 85.19(19) . . ?
F9 Sb2 F7 86.04(18) . . ?
F12 Sb2 F7 179.25(18) . . ?
F11 Sb2 F7 87.11(18) . . ?
O1 S1 O2 102.3(3) . . ?
O1 S1 F1 102.5(3) . . ?
O2 S1 F1 99.7(3) . . ?
Sb2 F7 Sb1 146.4(2) . . ?
C1 O1 S1 122.0(5) . . ?
C2 O2 S1 117.5(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 S1 O1 C1 44.7(7) . . . . ?
F1 S1 O1 C1 -58.3(6) . . . . ?
O1 S1 O2 C2 169.3(5) . . . . ?
F1 S1 O2 C2 -85.6(6) . . . . ?

_refine_diff_density_max         1.256
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.176



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: SO2'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
