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_1573046
_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         'C24 B F20, C38 H46 N O P2, C H2 Cl2'
_chemical_formula_sum            'C63 H48 B Cl2 F20 N O P2'
_chemical_formula_weight         1358.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 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                90
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_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1018(13)
_cell_length_b                   31.870(6)
_cell_length_c                   18.321(3)
_cell_measurement_reflns_used    9865
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.051
_cell_measurement_theta_min      2.4345
_cell_volume                     5892.1(17)
_computing_cell_refinement       'SAINT V8.40B'
_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
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_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.934
_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  0.0988
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            119817
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.243
_diffrn_reflns_theta_min         2.117
_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    0.273
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.6951
_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    1.532
_exptl_crystal_description       block
_exptl_crystal_F_000             2760
_exptl_crystal_recrystallization_method
'Single crystals suitable for X-ray diffraction were grown by gas phase diffusion of pentane into the CH2Cl2 solution.'
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.192
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 5365 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         19847
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0365P)^2^+2.4874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.1055
_reflns_Friedel_coverage         0.873
_reflns_Friedel_fraction_full    0.976
_reflns_Friedel_fraction_max     0.817
_reflns_number_gt                14223
_reflns_number_total             19847
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06581f2.cif
_cod_data_source_block           ly148_a
_cod_depositor_comments
'Adding full bibliography for 1573045--1573053.cif.'
_cod_original_cell_volume        5892.2(16)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               1573046
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.947
_shelx_estimated_absorpt_t_max   0.977
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_shelx_res_checksum              17608
_shelx_hkl_checksum              88619