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_7131965
_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_absolute_configuration unk
_chemical_formula_moiety         'C39 H20 F10 P, B C24 F20'
_chemical_formula_sum            'C63 H20 B F30 P'
_chemical_formula_weight         1388.611
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_Int_Tables_number      33
_audit_creation_date             2023-05-02
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
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2023-05-16 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
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_cell_angle_alpha                90
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_cell_angle_gamma                90
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_cell_length_b                   36.485(4)
_cell_length_c                   13.2044(15)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      19.73
_cell_measurement_theta_min      2.23
_cell_volume                     5877.6(11)
_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 0.9980
_diffrn_measured_fraction_theta_max 0.9980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1802
_diffrn_reflns_av_unetI/netI     0.1300
_diffrn_reflns_Laue_measured_fraction_full 0.9980
_diffrn_reflns_Laue_measured_fraction_max 0.9980
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            99111
_diffrn_reflns_point_group_measured_fraction_full 0.9980
_diffrn_reflns_point_group_measured_fraction_max 0.9980
_diffrn_reflns_theta_full        24.9988
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.76
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             2755.449
_refine_diff_density_max         0.4516
_refine_diff_density_min         -0.5773
_refine_diff_density_rms         0.1031
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   -0.06(12)
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             11.5705
_refine_ls_goodness_of_fit_ref   1.0564
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    40
_refine_ls_number_parameters     856
_refine_ls_number_reflns         10347
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0564
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0668
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+6.4626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1542
_reflns_Friedel_coverage         0.998
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              43
_reflns_limit_k_min              -43
_reflns_limit_l_max              15
_reflns_limit_l_min              -15
_reflns_number_gt                7636
_reflns_number_total             10347
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3cc02684a2.cif
_cod_data_source_block           dM126_a
_cod_original_sg_symbol_Hall     ' P 2c -2n'
_cod_original_formula_sum        'C63 H20 B1 F30 P1'
_cod_database_code               7131965
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C25(H25), C30(H30), C37(H37), C43(H43), C45(H45), C29(H29), C31(H31), C4(H4),
 C7(H7), C18(H18), C40(H40), C020(H020), C20(H20), C42(H42), C14(H14),
 C029(H029), C22(H22), C46(H46), C5(H5), C02J(H02J)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'