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_7133206
_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         'C26 H20 N O2 P S'
_chemical_formula_sum            'C26 H20 N O2 P S'
_chemical_formula_weight         441.46
_chemical_name_common
;
N-(10H-5l5-5,10-[1,2]benzenoacridophosphin-5-ylidene)-4-
methylbenzenesulfonamide
;
_chemical_name_systematic
;
N-(10H-5l5-5,10-[1,2]benzenoacridophosphin-5-ylidene)-4-
methylbenzenesulfonamide
;
_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   dual
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-04-10 deposited with the CCDC.	2024-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.7093(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   13.9420(2)
_cell_length_c                   19.4641(3)
_cell_measurement_reflns_used    6607
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      66.9650
_cell_measurement_theta_min      3.9010
_cell_volume                     2192.04(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Mercury 4.0 (Macrae et al, 2020)'
_computing_publication_material  'enCIFer (Allen et al, 2004)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 5.1856
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur, Ruby, Gemini Ultra
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11121
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.067
_diffrn_reflns_theta_max         67.067
_diffrn_reflns_theta_min         3.919
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.186
_exptl_absorpt_correction_T_max  0.740
_exptl_absorpt_correction_T_min  0.508
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.910
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3893
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0632
_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^)+(0.0989P)^2^+1.8333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1784
_refine_ls_wR_factor_ref         0.1828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3579
_reflns_number_total             3893
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01868k2.cif
_cod_data_source_block           nt0718_LHB_Ts-N-p-trip
_cod_depositor_comments
'Adding full bibliography for 7133202--7133219.cif.'
_cod_original_cell_volume        2192.04(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7133206
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.433
_shelx_estimated_absorpt_t_max   0.735
_shelx_res_checksum              14998
_shelx_hkl_checksum              40757