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_4132046
_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            'C38 H57 F N O2 P Pd'
_chemical_formula_weight         716.21
_chemical_name_common            8e
_chemical_name_systematic
(1-Ad)2(CH3OCH2CH2)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                70.103(2)
_cell_angle_beta                 73.800(2)
_cell_angle_gamma                77.068(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1182(13)
_cell_length_b                   11.9143(14)
_cell_length_c                   14.2549(16)
_cell_measurement_reflns_used    9840
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.31
_cell_measurement_theta_min      2.19
_cell_volume                     1687.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  SHELXL-2016
_computing_structure_solution    SHELXT-2014
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_refln_scan_rate          20
_diffrn_refln_scan_width         1.0
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_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            57935
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.346
_diffrn_reflns_theta_min         1.558
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       prism
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.267
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.111
_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     400
_refine_ls_number_reflns         6182
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0552P)^2^+3.2911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5317
_reflns_number_total             6182
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b00928_si_004.cif
_cod_data_source_block           8e
_cod_database_code               4132046
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.969
_shelx_estimated_absorpt_t_max   0.981
_shelx_res_checksum              44666
_shelx_hkl_checksum              70295