A Highly Active Palladium Catalyst for Intermolecular Hydroamination. Factors that Control Reactivity and Additions of Functionalized Anilines to Dienes and Vinylarenes
Adam M. Johns; Masaru Utsunomiya; Christopher D. Incarvito; John F. Hartwig; Journal of the American Chemical Society 128 (2006) 1828–1839; doi:10.1021/ja056003z

data_4110402
_publ_contact_author
;
     Prof. John F. Hartwig
     Department of Chemistry
     Yale University
     225 Prospect St
     PO Box 208107
     New Haven, CT 06520-8107
     USA
;
_publ_contact_author_email       john.hartwig@yale.edu
_publ_contact_author_fax         '+203 432 6144'
_publ_contact_author_phone       '+203 432 3917'
_publ_section_title
;
 A Highly Active Palladium Catalyst for Intermolecular Hydroamination.
 Factors that Control Reactivity and Additions of Functionalized Anilines
 to Dienes and Vinylarenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1828
_journal_page_last               1839
_journal_paper_doi               10.1021/ja056003z
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C45 H37 Cl2 F3 O4 P2 Pd S'
_chemical_formula_weight         970.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.76(3)
_cell_angle_beta                 67.63(3)
_cell_angle_gamma                70.75(3)
_cell_formula_units_Z            2
_cell_length_a                   11.451(2)
_cell_length_b                   14.314(3)
_cell_length_c                   14.412(3)
_cell_measurement_temperature    173(2)
_cell_volume                     2062.0(9)
_computing_cell_refinement       Denzo
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        Denzo
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_sigmaI/netI    0.1173
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17206
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_max  0.9413
_exptl_absorpt_correction_T_min  0.8619
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       blade
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         10129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0976
_reflns_number_gt                6237
_reflns_number_total             10129
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja056003zsi20050831_104911.cif
_cod_data_source_block           aj10
_cod_original_cell_volume        2062.0(7)
_cod_database_code               4110402