Mechanistic Studies of Palladium-Catalyzed Aminocarbonylation of Aryl Chlorides with Carbon Monoxide and Ammonia.
Wang, Justin Y.; Strom, Alexandra E.; Hartwig, John F.; Journal of the American Chemical Society 140 (2018) 7979–7993; doi:10.1021/jacs.8b04073

data_4132453
_publ_section_title
;
 Mechanistic Studies of Palladium-Catalyzed Aminocarbonylation of Aryl
 Chlorides with Carbon Monoxide and Ammonia.
;
_journal_issue                   25
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7979
_journal_page_last               7993
_journal_paper_doi               10.1021/jacs.8b04073
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C29 H54 P2 Pd'
_chemical_formula_weight         571.06
_chemical_name_common            JYW-1-177
_chemical_name_systematic        hartwig126
_space_group.centring_type       primitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.0070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5521(3)
_cell_length_b                   9.1531(3)
_cell_length_c                   16.1386(5)
_cell_measurement_reflns_used    9807
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.22
_cell_measurement_theta_min      4.83
_cell_volume                     1410.80(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_refln_scan_rate          10
_diffrn_refln_scan_width         2.0
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
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_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
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_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         68.276
_diffrn_reflns_theta_min         5.340
_diffrn_source                   'microfocus rotating anode'
_exptl_absorpt_coefficient_mu    6.465
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
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_exptl_crystal_description       prism
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_exptl_crystal_size_min          0.030
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_refine_diff_density_min         -0.840
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         2563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.365
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0556
_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^)+5.8446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.1273
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2516
_reflns_number_total             2563
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04073_si_001.cif
_cod_data_source_block           hartwig126
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4132453
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.782
_shelx_estimated_absorpt_t_max   0.830
_shelx_res_checksum              89177
_shelx_hkl_checksum              39567