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_7133216
_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_formula_moiety         'C43 H18 B F15 N P, C H2 Cl2'
_chemical_formula_sum            'C44 H20 B Cl2 F15 N P'
_chemical_formula_weight         960.29
_chemical_name_common
;
(N-phenyl-9-phosphatriptycene-iminium)-2,3,5,6-tetrafluorophenyl]-
bis(2,3,4,5,6-pentafluorophenyl)-fluoroborate dichloromethane solvate
;
_chemical_name_systematic
;
(N-phenyl-9-phosphatriptycene-iminium)-2,3,5,6-tetrafluorophenyl]-
bis(2,3,4,5,6-pentafluorophenyl)-fluoroborate dichloromethane solvate
;
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_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                83.3900(10)
_cell_angle_beta                 78.0600(10)
_cell_angle_gamma                74.6010(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2365(2)
_cell_length_b                   12.2624(2)
_cell_length_c                   14.8185(3)
_cell_measurement_reflns_used    9798
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.2509
_cell_measurement_theta_min      3.7465
_cell_volume                     1921.98(6)
_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)'
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_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0538
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            71257
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.245
_diffrn_reflns_theta_min         3.054
_exptl_absorpt_coefficient_mu    2.915
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.616
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         7031
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+1.5189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0895
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6547
_reflns_number_total             7031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01868k2.cif
_cod_data_source_block           nt1332_SMC132_100K
_cod_depositor_comments
'Adding full bibliography for 7133202--7133219.cif.'
_cod_database_code               7133216
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.496
_shelx_estimated_absorpt_t_max   0.833
_shelx_res_checksum              90758
_shelx_hkl_checksum              51054