Enthalpy-Controlled Insertion of a "Nonspectator" Tricoordinate Phosphorus Ligand into Group 10 Transition Metal-Carbon Bonds.
Hwang, Seung Jun; Tanushi, Akira; Radosevich, Alexander T.; Journal of the American Chemical Society 142 (2020) 21285–21291; doi:10.1021/jacs.0c11161

data_4135392
_publ_section_title
;
 Enthalpy-Controlled Insertion of a &quot;Nonspectator&quot; Tricoordinate
 Phosphorus Ligand into Group 10 Transition Metal-Carbon Bonds.
;
_journal_issue                   51
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              21285
_journal_page_last               21291
_journal_paper_doi               10.1021/jacs.0c11161
_journal_volume                  142
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_sum            'C40 H37 N3 O P2'
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_space_group_name_Hall           'P 2yb'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 107.1402(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9534(9)
_cell_length_b                   8.4688(4)
_cell_length_c                   21.9113(11)
_cell_measurement_reflns_used    9699
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.42
_cell_measurement_theta_min      2.25
_cell_volume                     3360.8(3)
_computing_cell_refinement       'SAINT 8.38A (Bruker-AXS, 2017)'
_computing_data_collection       'APEX3 v2017.3.0 (Bruker-AXS, 2017)'
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_computing_molecular_graphics    'Bruker SHELXTL'
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_diffrn_ambient_temperature      100(2)
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_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Photon2 CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0957
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            245534
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.033
_diffrn_reflns_theta_min         1.690
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  0.7214
_exptl_absorpt_correction_T_min  0.6610
_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.105
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_refine_diff_density_max         1.029
_refine_diff_density_min         -2.297
_refine_diff_density_rms         0.201
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.50(14)
_refine_ls_extinction_coef       0.084(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1339
_refine_ls_number_reflns         19638
_refine_ls_number_restraints     2872
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.0942
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1572P)^2^+2.1771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2307
_refine_ls_wR_factor_ref         0.2543
_reflns_Friedel_coverage         0.882
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                14985
_reflns_number_total             19638
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11161_si_002.cif
_cod_data_source_block           P18151
_cod_depositor_comments
'Adding full bibliography for 4135390--4135393.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4135392
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.944
_shelx_estimated_absorpt_t_max   0.993
_shelx_res_checksum              49911
_shelx_hkl_checksum              96559