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_7131959
_publ_section_title
;
 Electron-deficient cyclopropenium cations as Lewis acids in FLP chemistry
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC02684A
_journal_year                    2023
_chemical_formula_moiety         'C72 H50 F4 P2, 2(B C24 F20)'
_chemical_formula_sum            'C118.5 H50 B2 F44 P2'
_chemical_formula_weight         2393.243
_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             2023-03-06
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2023-04-25 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                82.704(12)
_cell_angle_beta                 66.558(12)
_cell_angle_gamma                77.177(13)
_cell_formula_units_Z            1
_cell_length_a                   13.468(3)
_cell_length_b                   15.211(3)
_cell_length_c                   15.382(3)
_cell_measurement_reflns_used    3249
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      19.24
_cell_measurement_theta_min      2.36
_cell_volume                     2816.4(10)
_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 0.9988
_diffrn_measured_fraction_theta_max 0.9988
_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  0.1651
_diffrn_reflns_av_unetI/netI     0.2176
_diffrn_reflns_Laue_measured_fraction_full 0.9988
_diffrn_reflns_Laue_measured_fraction_max 0.9988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            52348
_diffrn_reflns_point_group_measured_fraction_full 0.9988
_diffrn_reflns_point_group_measured_fraction_max 0.9988
_diffrn_reflns_theta_full        24.9993
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.37
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1198.411
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.8889
_refine_diff_density_min         -0.8772
_refine_diff_density_rms         0.1932
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             14.8180
_refine_ls_extinction_coef       0.0066
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0339
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    50
_refine_ls_number_parameters     758
_refine_ls_number_reflns         9893
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0339
_refine_ls_R_factor_all          0.1864
_refine_ls_R_factor_gt           0.0714
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0856P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1524
_refine_ls_wR_factor_ref         0.2086
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              -14
_reflns_limit_k_max              18
_reflns_limit_k_min              -17
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                4219
_reflns_number_total             9893
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3cc02684a2.cif
_cod_data_source_block           1_CCDC3
_cod_database_code               7131959
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C32(H32), C40(H40), C42(H42), C44(H44), C45(H45), C46(H46), C52(H52),
 C55(H55), C62(H62), C63(H63), C65(H65), C68(H68), C69(H69), C70(H70), C71(H71),
  C74(H74), C78(H78), C79(H79), C80(H80), C81(H81), C83(H83), C84(H84),
 C85(H85), C88(H88), C89(H89)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 162 electrons were 
found in a volume of 479\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[CH2Cl2] per Asymmetric Unit 
which account for 84 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'