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_1560306
_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
'C38 H43 N3 O3 P, C32 H12 B F24, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C70.5 H56 B Cl F24 N3 O3 P'
_chemical_formula_weight         1526.41
_chemical_name_common            9
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.16 svn.r6f6c53a7 for OlexSys, GUI svn.r6139)
;
_audit_update_record
;
2020-10-08 deposited with the CCDC.	2021-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                114.902(3)
_cell_angle_beta                 105.306(3)
_cell_angle_gamma                96.778(3)
_cell_formula_units_Z            2
_cell_length_a                   13.1828(13)
_cell_length_b                   17.1020(16)
_cell_length_c                   17.4082(17)
_cell_measurement_reflns_used    9781
_cell_measurement_temperature    103.85
_cell_measurement_theta_max      27.465
_cell_measurement_theta_min      2.344
_cell_volume                     3313.7(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      103.85
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.983
_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  0.0512
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45023
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         1.360
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0930 before and 0.0576 after correction.
The Ratio of minimum to maximum transmission is 0.9244.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             1554
_exptl_crystal_size_max          0.462
_exptl_crystal_size_mid          0.345
_exptl_crystal_size_min          0.222
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0012(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     956
_refine_ls_number_reflns         12828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0846P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1531
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8899
_reflns_number_total             12828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05893a2.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 1560304--1560308.cif.'
_cod_original_formula_sum        'C70.50 H56 B Cl F24 N3 O3 P'
_cod_database_code               1560306
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: Cl2(0.5) C71(0.5) H71A(0.5) H71B(0.5) Cl1(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C71(H71A,H71B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C16(H16), C17(H17),
 C18(H18), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C40(H40), C42(H42),
  C44(H44), C48(H48), C50(H50), C52(H52), C56(H56), C58(H58), C60(H60),
 C64(H64), C66(H66), C68(H68)
3.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              23446
_shelx_hkl_checksum              41614
_olex2_submission_special_instructions 'No special instructions were received'