Shrinking of C-S bonds of organosulfonic acids in superacidic media-investigation of the protonation of methanesulfonic acid and benzenesulfonic acid and their limits.
Bockmair, Valentin; Xu, Tong; Hollenwäger, Dirk; Kornath, Andreas J.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 12169–12179; doi:10.1039/d5dt00864f

data_7719127
_publ_section_title
;
 Shrinking of C-S bonds of organosulfonic acids in superacidic
 media-investigation of the protonation of methanesulfonic acid and
 benzenesulfonic acid and their limits.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12169
_journal_page_last               12179
_journal_paper_doi               10.1039/d5dt00864f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C H4 O3 S'
_chemical_formula_sum            'C H4 O3 S'
_chemical_formula_weight         96.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-12-20
_audit_creation_method           'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_audit_update_record
;
2025-01-25 deposited with the CCDC.	2025-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.214(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3920(11)
_cell_length_b                   5.8234(7)
_cell_length_c                   8.2047(8)
_cell_measurement_reflns_used    722
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      31.5580
_cell_measurement_theta_min      2.6110
_cell_volume                     385.02(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (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-2019/2 (Sheldrick, 2019)'
_computing_structure_solution
'SHELXT (Sheldrick, G. M. (2015). Acta Cryst. A71, 3-8.)'
_diffrn_ambient_temperature      115(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0217
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2075
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.130
_diffrn_reflns_theta_min         2.528
_diffrn_source_current           40
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56793
_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.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             200
_exptl_crystal_size_max          0.408
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+0.2351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.000
_reflns_number_gt                867
_reflns_number_total             1030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00864f2.cif
_cod_data_source_block           xl030
_cod_depositor_comments
'Adding full bibliography for 7719127--7719131.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7719127
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.772
_shelx_estimated_absorpt_t_max   0.945
_oxdiff_exptl_absorpt_empirical_full_min 0.729
_oxdiff_exptl_absorpt_empirical_full_max 1.429
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              65262
_shelx_hkl_checksum              47563