Synthesis and crystal structures of N,2,4,6-tetramethylanilinium trifluoromethanesulfonate and N-isopropylidene-N,2,4,6-tetramethylanilinium trifluoromethanesulfonate
Stewart, John W.; Irons, Elena M.; Osorio Abanto, Giovanna; Zeller, Matthias; Zaleski, Curtis M.; Predecki, Daniel P.; Acta Crystallographica Section E Crystallographic Communications 80 (2024) –; doi:10.1107/S2056989024003438

data_2023111
_publ_section_title
;
 Synthesis and crystal structures of N,2,4,6-tetramethylanilinium
 trifluoromethanesulfonate and
 N-isopropylidene-N,2,4,6-tetramethylanilinium trifluoromethanesulfonate
;
_journal_coeditor_code           EJ2004
_journal_issue                   5
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989024003438
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          'C10 H16 N +, C F3 O3 S -'
_chemical_formula_moiety         'C10 H16 N +, C F3 O3 S -'
_chemical_formula_sum            'C11 H16 F3 N O3 S'
_chemical_formula_weight         299.31
_chemical_name_systematic
;
<i>N</i>,2,4,6-Tetramethylanilinium trifluoromethanesulfonate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 105.106(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5194(7)
_cell_length_b                   18.1257(13)
_cell_length_c                   9.0875(8)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.7105
_cell_measurement_theta_min      2.5794
_cell_volume                     1354.80(19)
_computing_cell_refinement
;
SAINT V8.40B (Bruker, 2022)
;
_computing_data_collection
;
APEX4 v2022.10-0 (Bruker, 2022)
;
_computing_data_reduction
;
SAINT V8.40B (Bruker, 2022)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2019/2</i> (Sheldrick, 2015b),
<i>ShelXle</i> Rev1594 (H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS D8 Quest'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            47829
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.262
_diffrn_reflns_theta_min         2.579
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           30
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.278
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al</i>., 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       plate
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.430
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.559
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         5186
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0667P)^2^+0.3108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1326
_reflns_number_gt                3572
_reflns_number_total             5186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ej2004.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2023111
_shelx_estimated_absorpt_t_min   0.885
_shelx_estimated_absorpt_t_max   0.944
_shelx_hkl_checksum              35328
_shelx_res_checksum              80373