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_1573053
_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         'C40 H42 N O2 P2, C24 B F20'
_chemical_formula_sum            'C64 H42 B F20 N O2 P2'
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_space_group_name_Hall           '-C 2yc'
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_atom_sites_solution_hydrogens   geom
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;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.
;
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.036
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_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)'
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_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
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_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
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_diffrn_measurement_method       '\w and \f scans'
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_diffrn_reflns_av_R_equivalents  0.0795
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_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            418640
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.262
_diffrn_reflns_theta_min         1.964
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_type              'Incoatec I\ms'
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_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_T_max  0.7458
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_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            colourless
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       block
_exptl_crystal_F_000             5312
_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          0.352
_exptl_crystal_size_mid          0.342
_exptl_crystal_size_min          0.194
_refine_diff_density_max         0.497
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_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     818
_refine_ls_number_reflns         16732
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0506P)^2^+16.0756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14084
_reflns_number_total             16732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06581f2.cif
_cod_data_source_block           ly163_a_sq
_cod_depositor_comments
'Adding full bibliography for 1573045--1573053.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1573053
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.941
_shelx_estimated_absorpt_t_max   0.967
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_shelx_res_checksum              67532
_shelx_hkl_checksum              98031
_shelx_fab_checksum              20479