Reductive Elimination from Phosphine-Ligated Alkylpalladium(II) Amido Complexes To Form sp<sup>3</sup> Carbon-Nitrogen Bonds.
Peacock, D. Matthew; Jiang, Quan; Hanley, Patrick S.; Cundari, Thomas R.; Hartwig, John F.; Journal of the American Chemical Society 140 (2018) 4893–4904; doi:10.1021/jacs.8b00928

data_4132044
_publ_section_title
;
 Reductive Elimination from Phosphine-Ligated Alkylpalladium(II) Amido
 Complexes To Form sp<sup>3</sup> Carbon-Nitrogen Bonds.
;
_journal_issue                   14
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4893
_journal_page_last               4904
_journal_paper_doi               10.1021/jacs.8b00928
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C42 H57 F N O2 P Pd'
_chemical_formula_weight         764.25
_chemical_name_common            8b
_chemical_name_systematic
'[(1-Ad)2(2-(OCH3)C6H4)P]Pd(syn-3-CH3norborn-2-yl)NH(4-F-2-(OCH3)C6H3)'
_space_group.centring_type       primitive
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                107.368(3)
_cell_angle_beta                 101.454(3)
_cell_angle_gamma                94.717(4)
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_cell_length_a                   10.5660(7)
_cell_length_b                   12.3759(9)
_cell_length_c                   14.7842(10)
_cell_measurement_reflns_used    9559
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.63
_cell_volume                     1787.5(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
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_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_refln_scan_rate          10
_diffrn_refln_scan_width         2.0
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            63247
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.393
_diffrn_reflns_theta_min         1.485
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       prism
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
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_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         6562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0291
_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^)+(0.0180P)^2^+3.0704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0687
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6013
_reflns_number_total             6562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b00928_si_003.cif
_cod_data_source_block           8b
_cod_database_code               4132044
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.964
_shelx_estimated_absorpt_t_max   0.976
_shelx_res_checksum              96444
_shelx_hkl_checksum              45009