Electron-deficient cyclopropenium cations as Lewis acids in FLP chemistry
Mandal, Dipendu; Qu, Zheng-wang; Grimme, Stefan; Stephan, Douglas W.; Chemical Communications  (2023) –; doi:10.1039/D3CC02684A

data_7131963
_publ_section_title
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 Electron-deficient cyclopropenium cations as Lewis acids in FLP chemistry
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC02684A
_journal_year                    2023
_chemical_formula_moiety         'B C18 Cl F15, C33 H27 P'
_chemical_formula_sum            'C51 H27 B Cl F15 P'
_chemical_formula_weight         1002.009
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2022-12-01
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-04-25 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                97.878(9)
_cell_angle_beta                 90.337(8)
_cell_angle_gamma                109.858(8)
_cell_formula_units_Z            2
_cell_length_a                   12.216(4)
_cell_length_b                   12.340(4)
_cell_length_c                   15.353(5)
_cell_measurement_reflns_used    2817
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.44
_cell_measurement_theta_min      3.13
_cell_volume                     2152.8(12)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.9943
_diffrn_measured_fraction_theta_max 0.9943
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1936
_diffrn_reflns_av_unetI/netI     0.1922
_diffrn_reflns_Laue_measured_fraction_full 0.9943
_diffrn_reflns_Laue_measured_fraction_max 0.9943
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43510
_diffrn_reflns_point_group_measured_fraction_full 0.9943
_diffrn_reflns_point_group_measured_fraction_max 0.9943
_diffrn_reflns_theta_full        24.9990
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.38
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_T_max  0.7260
_exptl_absorpt_correction_T_min  0.6349
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1367 before and 0.1030 after correction.
The Ratio of minimum to maximum transmission is 0.8745.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1011.402
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.2917
_refine_diff_density_min         -1.4492
_refine_diff_density_rms         0.1901
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             6.0286
_refine_ls_goodness_of_fit_ref   1.0543
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    53
_refine_ls_number_parameters     622
_refine_ls_number_reflns         7547
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0543
_refine_ls_R_factor_all          0.1566
_refine_ls_R_factor_gt           0.0771
_refine_ls_shift/su_max          -0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1123P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1900
_refine_ls_wR_factor_ref         0.2466
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                4076
_reflns_number_total             7547
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3cc02684a2.cif
_cod_data_source_block           1_CCDC8
_cod_database_code               7131963
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C40(H40)
2.b Secondary CH2 refined with riding coordinates:
 C66(H66a,H66b)
2.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C27(H27), C28(H28), C30(H30), C37(H37), C39(H39), C41(H41),
 C48(H48), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57),
  C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64),
 C65(H65), C67(H67)
;
_olex2_submission_special_instructions 'No special instructions were received'