Regulating iminophosphorane PN bond reactivity through geometric constraints with cage-shaped triarylphosphines.
Hu, Lei; Chakraborty, Sayandip; Tumanov, Nikolay; Wouters, Johan; Robiette, Raphaël; Berionni, Guillaume; Chemical communications (Cambridge, England) 60 (2024) 7073–7076; doi:10.1039/d4cc01868k

data_7133208
_publ_section_title
;
 Regulating iminophosphorane P&#xe001;N bond reactivity through geometric
 constraints with cage-shaped triarylphosphines.
;
_journal_issue                   55
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7073
_journal_page_last               7076
_journal_paper_doi               10.1039/d4cc01868k
_journal_volume                  60
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C44 H33 N P 1+, B F4 1-'
_chemical_formula_sum            'C44 H33 B F4 N P'
_chemical_formula_weight         693.49
_chemical_name_common
'N-(p-tritylphenyl)-9-phosphatriptycene-iminium tetrafluoroborate'
_chemical_name_systematic
'N-(p-tritylphenyl)-9-phosphatriptycene-iminium tetrafluoroborate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-04-10 deposited with the CCDC.	2024-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.867(4)
_cell_length_b                   13.069(4)
_cell_length_c                   21.505(6)
_cell_measurement_reflns_used    644
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      40.958
_cell_measurement_theta_min      4.112
_cell_volume                     3616.3(19)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.16'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_molecular_graphics    'Mercury 4.0 (Macrae et al, 2020)'
_computing_publication_material  'enCIFer (Allen et al, 2004)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.891
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w-scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.1093
_diffrn_reflns_Laue_measured_fraction_full 0.891
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3086
_diffrn_reflns_point_group_measured_fraction_full 0.715
_diffrn_reflns_point_group_measured_fraction_max 0.715
_diffrn_reflns_theta_full        48.240
_diffrn_reflns_theta_max         48.240
_diffrn_reflns_theta_min         4.111
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    1.113
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0907 before and 0.0581 after correction.
The Ratio of minimum to maximum transmission is 0.5680.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 330 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(7)
_refine_ls_extinction_coef       0.0008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         2459
_refine_ls_number_restraints     379
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1643
_refine_ls_R_factor_gt           0.0792
_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^)+(0.0780P)^2^+8.4136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1704
_refine_ls_wR_factor_ref         0.2302
_reflns_Friedel_coverage         0.547
_reflns_Friedel_fraction_full    0.525
_reflns_Friedel_fraction_max     0.525
_reflns_number_gt                1312
_reflns_number_total             2459
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01868k2.cif
_cod_data_source_block           nt1231_SMC037
_cod_depositor_comments
'Adding full bibliography for 7133202--7133219.cif.'
_cod_original_cell_volume        3616.2(18)
_cod_database_code               7133208
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.962
_shelx_estimated_absorpt_t_max   0.978
_shelx_res_checksum              1195
_shelx_hkl_checksum              52368