Structural constraint at a P-P bond: phosphinophosphination of alkenes, alkynes, and carbonyls by a concerted mechanism.
You, Lijun; Roth, Daniel; Greb, Lutz; Chemical science 16 (2025) 1716–1721; doi:10.1039/d4sc06581f

data_1573049
_publ_section_title
;
 Structural constraint at a P-P bond: phosphinophosphination of alkenes,
 alkynes, and carbonyls by a concerted mechanism.
;
_journal_issue                   4
_journal_name_full               'Chemical science'
_journal_page_first              1716
_journal_page_last               1721
_journal_paper_doi               10.1039/d4sc06581f
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C46 H46 N O P2, C24 B F20, C H2 Cl2'
_chemical_formula_sum            'C71 H48 B Cl2 F20 N O P2'
_chemical_formula_weight         1454.75
_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     direct
_audit_creation_method
;FinalCif V130 by Daniel Kratzert, Freiburg 2024, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2024-05-22 deposited with the CCDC.	2024-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                82.59(2)
_cell_angle_beta                 77.118(18)
_cell_angle_gamma                64.527(16)
_cell_formula_units_Z            2
_cell_length_a                   14.195(7)
_cell_length_b                   15.574(7)
_cell_length_c                   16.591(8)
_cell_measurement_reflns_used    9733
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.401
_cell_measurement_theta_min      2.2935
_cell_volume                     3226(3)
_computing_cell_refinement       'SAINT V8.40B'
_computing_data_collection
'Bruker BIS V6.2.15/2021-03-15 and APEX4 2021.10-0'
_computing_data_reduction        'SAINT V8.40B'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0807
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            196656
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.047
_diffrn_reflns_theta_min         1.956
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.255
_exptl_absorpt_correction_T_max  0.7438
_exptl_absorpt_correction_T_min  0.7005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction: 
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 
(2015) 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       block
_exptl_crystal_F_000             1476
_exptl_crystal_recrystallization_method
;Single crystals suitable for X-ray diffraction were grown by gas phase diffusion
 of pentane into the solution of toluene and CH2Cl2 (1:1).
;
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.063
_refine_diff_density_max         0.756
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     948
_refine_ls_number_reflns         18332
_refine_ls_number_restraints     179
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0543P)^2^+2.2269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1345
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13616
_reflns_number_total             18332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06581f2.cif
_cod_data_source_block           ly129_a
_cod_depositor_comments
'Adding full bibliography for 1573045--1573053.cif.'
_cod_database_code               1573049
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.958
_shelx_estimated_absorpt_t_max   0.984
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_shelx_res_checksum              66660
_shelx_hkl_checksum              28933