Trioxatriangulenium (TOTA+) as a robust carbon-based Lewis acid in frustrated Lewis pair chemistry
Shaikh, Aslam C.; Veleta, José M.; Moutet, Jules; Gianetti, Thomas L.; Chemical Science 12 (2021) 4841–4849; doi:10.1039/D0SC05893A

data_1560304
_publ_section_title
;
 Trioxatriangulenium (TOTA+) as a robust carbon-based Lewis acid in
 frustrated Lewis pair chemistry
;
_journal_issue                   13
_journal_name_full               'Chemical Science'
_journal_page_first              4841
_journal_page_last               4849
_journal_paper_doi               10.1039/D0SC05893A
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C25 H14 O3 S'
_chemical_formula_sum            'C25 H14 O3 S'
_chemical_formula_weight         394.42
_chemical_name_common            4a
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-08 deposited with the CCDC.	2021-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.325(2)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   7.5851(7)
_cell_length_b                   43.318(3)
_cell_length_c                   8.5930(8)
_cell_measurement_reflns_used    3904
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      22.889
_cell_measurement_theta_min      2.409
_cell_volume                     2777.7(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            19541
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.752
_diffrn_reflns_theta_min         0.940
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.200
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6708
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0738 before and 0.0447 after correction. The Ratio of minimum to maximum transmission is 0.9000. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear yellowish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       plate
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          1
_exptl_crystal_size_mid          0.58
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.152
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         5359
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0390P)^2^+0.6974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1028
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3930
_reflns_number_total             5359
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05893a2.cif
_cod_data_source_block           4a
_cod_depositor_comments
'Adding full bibliography for 1560304--1560308.cif.'
_cod_database_code               1560304
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.825
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C28 \\sim C39 \\sim C27 \\sim C33 \\sim C50 \\sim C46 \\sim C44 \\sim C40 \\sim
C32 \\sim C34 \\sim C38 \\sim C49 \\sim C47 \\sim C43 \\sim C41 \\sim O6 \\sim
C29 \\sim O5 \\sim C31 \\sim C35 \\sim C37 \\sim C48 \\sim C42 \\sim C30 \\sim
C36: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O5(0.5) C44(0.5) C39(0.5) C40(0.5) C41(0.5) H41(0.5) C42(0.5)
 H42(0.5) C43(0.5) H43(0.5) C27(0.5) C28(0.5) C29(0.5) H29(0.5) C30(0.5)
 H30(0.5) C31(0.5) H31(0.5) C32(0.5) C33(0.5) C34(0.5) C35(0.5) H35(0.5)
 C36(0.5) H36(0.5) C37(0.5) H37(0.5) C38(0.5) O6(0.5) C50(0.5) H50(0.5)
 C49(0.5) H49(0.5) C48(0.5) H48(0.5) C47(0.5) H47(0.5) C46(0.5) H46(0.5)
 C26(0.5) S2(0.5) C45(0.5) O4(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C18(H18), C25(H25), C6(H6), C21(H21), C5(H5), C16(H16), C10(H10),
 C24(H24), C12(H12), C11(H11), C17(H17), C23(H23), C22(H22), C41(H41), C42(H42),
  C43(H43), C29(H29), C30(H30), C31(H31), C35(H35), C36(H36), C37(H37),
 C50(H50), C49(H49), C48(H48), C47(H47), C46(H46)
;
_shelx_res_checksum              49708
_shelx_hkl_checksum              41108
_olex2_submission_special_instructions 'No special instructions were received'