Photochemical activation of pincer-ligated phosphoranides: mechanistic insight for reduction of aryl halides.
Escoudé, Emile; Pedrón, Manuel; Bourqui, Lilian; Gontard, Geoffrey; Vitale, Maxime R.; Ciofini, Ilaria; Lakhdar, Sami; Grimaud, Laurence; Chemical science 17 (2026) 579–584; doi:10.1039/d5sc06960b

data_1576205
_publ_section_title
;
 Photochemical activation of pincer-ligated phosphoranides: mechanistic
 insight for reduction of aryl halides.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              579
_journal_page_last               584
_journal_paper_doi               10.1039/d5sc06960b
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         'C47 H71 K N O8 P, C5 H12'
_chemical_formula_sum            'C52 H83 K N O8 P'
_chemical_formula_weight         920.26
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-07-02 deposited with the CCDC.	2025-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                79.756(1)
_cell_angle_beta                 79.904(1)
_cell_angle_gamma                79.803(1)
_cell_formula_units_Z            2
_cell_length_a                   9.2969(1)
_cell_length_b                   15.9116(2)
_cell_length_c                   18.7341(3)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    200(1)
_cell_measurement_theta_max      68.30
_cell_measurement_theta_min      4.02
_cell_volume                     2654.30(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SXGRAPH (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200(1)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_source         micro-source
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27484
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.590
_diffrn_reflns_theta_min         3.454
_exptl_absorpt_coefficient_mu    1.553
_exptl_absorpt_correction_T_max  0.867
_exptl_absorpt_correction_T_min  0.527
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 SADABS : 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    1.151
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
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_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         9328
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0630P)^2^+0.6365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                8480
_reflns_number_total             9328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc06960b3.cif
_cod_data_source_block           ee240716
_cod_depositor_comments
'Adding full bibliography for 1576202--1576209.cif.'
_cod_database_code               1576205
_shelx_shelxl_version_number     2019/3
_shelx_res_checksum              12436