Synthesis, structure and proton conductivity of 2,4,5-trimethylbenzenesulfonic acid dihydrate
Pisareva, A. V.; Shilov, G. V.; Karelin, A. I.; Pisarev, R. V.; Shilova, I. A.; Dobrovolsky, Yu A.; Aldoshin, S. M.; New Journal of Chemistry 42 (2018) 7428–; doi:10.1039/C7NJ05068B

data_1549208
_publ_section_title
;
 Synthesis, structure and proton conductivity of
 2,4,5-trimethylbenzenesulfonic acid dihydrate
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7428
_journal_paper_doi               10.1039/C7NJ05068B
_journal_volume                  42
_journal_year                    2018
_chemical_formula_sum            'C9 H16 O5 S'
_chemical_formula_weight         236.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-12-15 deposited with the CCDC.
2018-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.123(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.7445(3)
_cell_length_b                   7.5360(3)
_cell_length_c                   9.9477(4)
_cell_measurement_reflns_used    1491
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      31.3116
_cell_measurement_theta_min      3.2689
_cell_volume                     580.17(4)
_computing_cell_refinement
'CrysAlisPro 1.171.36.20 (Agilent Technologies, 2012)'
_computing_data_collection
'CrysAlisPro 1.171.36.20 (Agilent Technologies, 2012)'
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'CrysAlisPro 1.171.36.20 (Agilent Technologies, 2012)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 16.2060
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0122
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2882
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.066
_diffrn_reflns_theta_min         3.276
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96124
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       plate
_exptl_crystal_F_000             252
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.27(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2427
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0427P)^2^+0.0254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0809
_reflns_Friedel_coverage         0.866
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                2356
_reflns_number_total             2427
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj05068b1.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 1549208.cif.'
_cod_database_code               1549208
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              81476