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_7133209
_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         'C25 H18 B F3 N P, 0.5(C H2 Cl2) '
_chemical_formula_sum            'C25.5 H19 B Cl F3 N P'
_chemical_formula_weight         473.65
_chemical_name_common
;
9-phosphatriptycene-N-phenyl imine trifluoroborane complex
 dichloromethane semisolvate
;
_chemical_name_systematic
;
N-phenyl-5gamma^5^-5,10-[1,2]benzenoacridophosphin-5(10H)-imine trifluoroborane
 complex dichloromethane semisolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 101.4060(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5904(2)
_cell_length_b                   16.0488(3)
_cell_length_c                   14.2154(3)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.2898
_cell_measurement_theta_min      4.2017
_cell_volume                     2144.74(8)
_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      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  0.0368
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21498
_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         68.285
_diffrn_reflns_theta_min         4.202
_exptl_absorpt_coefficient_mu    2.636
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5812
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       plate
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.018
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         3919
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0311P)^2^+3.6038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1154
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3813
_reflns_number_total             3919
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01868k2.cif
_cod_data_source_block           nt1194_SCM039_100K
_cod_depositor_comments
'Adding full bibliography for 7133202--7133219.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C25.50 H19 B Cl F3 N P'
_cod_database_code               7133209
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.442
_shelx_estimated_absorpt_t_max   0.954
_shelx_res_checksum              62703
_shelx_hkl_checksum              31470