The electrophilic methylating agent [SO<sub>2</sub>Me]<sup>+</sup> parent of two cationic species.
Hollenwäger, Dirk; Bockmair, Valentin; Kornath, Andreas J.; Chemical communications (Cambridge, England) 60 (2024) 10148–10151; doi:10.1039/d4cc03400g

data_7133606
_publ_section_title
;
 The electrophilic methylating agent [SO<sub>2</sub>Me]<sup>+</sup> parent
 of two cationic species.
;
_journal_issue                   74
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10148
_journal_page_last               10151
_journal_paper_doi               10.1039/d4cc03400g
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'F6 Sb, C H4 F O2 S'
_chemical_formula_sum            'C H4 F7 O2 S Sb'
_chemical_formula_weight         334.85
_chemical_name_common            'methylated fluorosulfurous acid'
_chemical_name_systematic        '[FS(OH)(OMe)][SbF6]'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-01-17
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-07-08 deposited with the CCDC.	2024-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   13.5681(5)
_cell_length_b                   10.8817(5)
_cell_length_c                   22.3347(8)
_cell_measurement_reflns_used    5816
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      31.9830
_cell_measurement_theta_min      1.8600
_cell_volume                     3297.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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.) '
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution
'SHELXT (Sheldrick, G. M. (2015). Acta Cryst. A71, 3-8.)'
_diffrn_ambient_temperature      102(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    0.5
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            13848
_diffrn_reflns_point_group_measured_fraction_full 0.913
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         1.824
_diffrn_source_current           40
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.683
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67253
_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.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2496
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: HF'
_exptl_crystal_size_max          0.438
_exptl_crystal_size_mid          0.365
_exptl_crystal_size_min          0.163
_refine_diff_density_max         0.988
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.46(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         6546
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0186P)^2^+5.7870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0665
_reflns_Friedel_coverage         0.756
_reflns_Friedel_fraction_full    0.821
_reflns_Friedel_fraction_max     0.797
_reflns_number_gt                5979
_reflns_number_total             6546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03400g2.cif
_cod_data_source_block           xi097
_cod_depositor_comments
'Adding full bibliography for 7133606--7133607.cif.'
_cod_database_code               7133606
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.295
_shelx_estimated_absorpt_t_max   0.585
_shelx_res_checksum              26883
_shelx_hkl_checksum              30077