Double axial stabilization of a carbenium ion <i>via</i> convergent PO → C<sup>+</sup> tetrel bonding.
Litle, Elishua D.; Gabbaï, François P; Chemical communications (Cambridge, England) 60 (2024) 690–693; doi:10.1039/d3cc04729f

data_7132455
_publ_section_title
;
 Double axial stabilization of a carbenium ion <i>via</i> convergent
 P&#xe001;O &#x2192; C<sup>+</sup> tetrel bonding.
;
_journal_issue                   6
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              690
_journal_page_last               693
_journal_paper_doi               10.1039/d3cc04729f
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C45 H38 N O2 P2, B F4'
_chemical_formula_sum            'C45 H38 B F4 N O2 P2'
_chemical_formula_weight         773.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-08-17
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-09-20 deposited with the CCDC.	2023-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.755(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.224(2)
_cell_length_b                   25.959(5)
_cell_length_c                   12.870(2)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      68.210
_cell_measurement_theta_min      3.999
_cell_volume                     4082.0(12)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26069
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.241
_diffrn_reflns_theta_min         3.999
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.435
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.6229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0908 before and 0.0704 after correction. The Ratio of minimum to maximum transmission is 0.8272. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       block
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         3817
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0645P)^2^+5.0077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3522
_reflns_number_total             3817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04729f2.cif
_cod_data_source_block           eli163_0m_a
_cod_depositor_comments
'Adding full bibliography for 7132454--7132458.cif.'
_cod_original_cell_volume        4082.1(13)
_cod_database_code               7132455
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.891
_shelx_estimated_absorpt_t_min   0.753
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C2(H2), C5(H5), C3(H3), C18(H18), C4(H4), C14(H14),
 C8(H8), C12(H12), C17(H17), C16(H16), C15(H15), C10(H10), C11(H11), C9(H9)
2.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C)
;
_shelx_res_checksum              64906
_shelx_hkl_checksum              31824
_olex2_submission_special_instructions 'No special instructions were received'