The bismuth phosphanides Bi(PR<sub>2</sub>)<sub>3</sub>: sources of phosphanyl radicals, P-inversion, and reversible olefin insertion.
Reith, Sascha; Oberdorf, Kai; Martínez, Sebstián; Landgraf, Jann B.; Ahrens, Alena; Jakobi, Felix; Xie, Xiulan; Lichtenberg, Crispin; Chemical science 17 (2026) 5183–5191; doi:10.1039/d5sc07240a

data_1576865
_publ_section_title
;
 The bismuth phosphanides Bi(PR<sub>2</sub>)<sub>3</sub>: sources of
 phosphanyl radicals, P-inversion, and reversible olefin insertion.
;
_journal_issue                   10
_journal_name_full               'Chemical science'
_journal_page_first              5183
_journal_page_last               5191
_journal_paper_doi               10.1039/d5sc07240a
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         'C24 H54 Bi P3'
_chemical_formula_sum            'C24 H54 Bi P3'
_chemical_formula_weight         644.56
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-02-05
_audit_creation_method           'CrysAlisPro 1.171.41.96a (Rigaku OD, 2021)'
_audit_update_record
;
2025-11-11 deposited with the CCDC.	2025-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 108.020(3)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   11.5915(3)
_cell_length_b                   16.9444(4)
_cell_length_c                   16.3179(5)
_cell_measurement_reflns_used    14042
_cell_measurement_temperature    99.9(5)
_cell_measurement_theta_max      32.3750
_cell_measurement_theta_min      2.2240
_cell_volume                     3047.80(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.96a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.96a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.96a (Rigaku OD, 2021)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.8419
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     18.00  52.00   0.50    6.50    --    8.52-117.00 -75.00   68
  2  \w     28.00  75.00   0.50    6.50    --    8.52-160.00 132.00   94
  3  \w    -20.00   5.00   0.50    6.50    --    8.52 -19.00 -90.00   50
  4  \w    -65.00  -7.00   0.50    6.50    --    8.52 -19.00   0.00  116
  5  \w    -26.00   6.00   0.50    6.50    --    8.52 -99.00-120.00   64
  6  \w    -26.00  42.00   0.50    6.50    --    8.52 -99.00 150.00  136
  7  \w    -26.00  23.00   0.50    6.50    --   -9.46 -99.00-180.00   98
  8  \w     -2.00  23.00   0.50    6.50    --   -9.46 -99.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0249294000
_diffrn_orient_matrix_UB_12      -0.0353404000
_diffrn_orient_matrix_UB_13      0.0215712000
_diffrn_orient_matrix_UB_21      0.0495917000
_diffrn_orient_matrix_UB_22      0.0216645000
_diffrn_orient_matrix_UB_23      0.0271247000
_diffrn_orient_matrix_UB_31      -0.0325773000
_diffrn_orient_matrix_UB_32      0.0058567000
_diffrn_orient_matrix_UB_33      0.0298026000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.842
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36069
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.842
_diffrn_reflns_theta_full        26.3154
_diffrn_reflns_theta_max         32.2444
_diffrn_reflns_theta_min         2.2041
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.950
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;

CrysAlisPro 1.171.41.96a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       plate
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.063
_refine_diff_density_max         2.082
_refine_diff_density_min         -0.910
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         9096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+0.8217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0743
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7209
_reflns_number_total             9096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc07240a2.cif
_cod_data_source_block           KaOb025Mo_a
_cod_original_cell_volume        3047.82(15)
_cod_database_code               1576865
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.535
_shelx_estimated_absorpt_t_max   0.717
_shelx_res_checksum              83002
_cell_oxdiff_length_a            11.5922(3)
_cell_oxdiff_length_b            16.9431(3)
_cell_oxdiff_length_c            16.3221(4)
_cell_oxdiff_angle_alpha         89.9777(18)
_cell_oxdiff_angle_beta          108.061(2)
_cell_oxdiff_angle_gamma         90.0588(18)
_cell_oxdiff_volume              3047.82(11)
_cell_oxdiff_measurement_reflns_used 14042
_oxdiff_exptl_absorpt_empirical_full_min 0.884
_oxdiff_exptl_absorpt_empirical_full_max 1.132
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
01a5a067722bf776a66ae7548c061730d300676bb9f
;
_diffrn_oxdiff_digest_hkl
;
01a0d0c74bbd84f0bb9f9aee65810bda8123bd
;
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_theta     26.32
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'Bi C24 P3 H54'