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_7131961
_publ_section_title
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 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         'B C24 F20, C21 H5 F10, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C45.5 H6 B Cl F30'
_chemical_formula_weight         1168.76
_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     iterative
_audit_creation_date             2023-04-25
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
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2023-04-25 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                64.316(5)
_cell_angle_beta                 75.794(5)
_cell_angle_gamma                78.866(6)
_cell_formula_units_Z            4
_cell_length_a                   10.8368(15)
_cell_length_b                   20.352(3)
_cell_length_c                   21.873(3)
_cell_measurement_reflns_used    1819
_cell_measurement_temperature    150.02
_cell_measurement_theta_max      18.10
_cell_measurement_theta_min      2.23
_cell_volume                     4193.7(10)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.02
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3688
_diffrn_reflns_av_unetI/netI     0.3406
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            97400
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.116
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.263
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             2284
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.011
_refine_diff_density_max         0.408
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_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1396
_refine_ls_number_reflns         14744
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_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.2982
_refine_ls_R_factor_gt           0.0867
_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^)+(0.0623P)^2^+3.4384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1466
_refine_ls_wR_factor_ref         0.2284
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4819
_reflns_number_total             14744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02684a2.cif
_cod_data_source_block           1_CCDC5
_cod_original_formula_sum        'C45.50 H6 B Cl F30'
_cod_database_code               7131961
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.902
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C92(H92), C98(H98), C120(H120), C135(H135), C142(H142), C59(H59), C80(H80),
 C131(H131), C147(H147), C150(H150)
;
_shelx_res_checksum              94531
_shelx_hkl_checksum              94347
_olex2_submission_special_instructions 'No special instructions were received'