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_4110406
_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            'C42.5 H36 Cl F3 Fe O3 P2 Pd S'
_chemical_formula_weight         943.41
_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                63.91(3)
_cell_angle_beta                 81.69(3)
_cell_angle_gamma                77.45(3)
_cell_formula_units_Z            4
_cell_length_a                   10.426(2)
_cell_length_b                   20.056(4)
_cell_length_c                   21.214(4)
_cell_measurement_temperature    173(2)
_cell_volume                     3882.7(17)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0651
_diffrn_reflns_av_sigmaI/netI    0.1344
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            32734
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    1.096
_exptl_absorpt_correction_T_max  0.8983
_exptl_absorpt_correction_T_min  0.8528
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       block
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1006
_refine_ls_number_reflns         19196
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.101
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                10960
_reflns_number_total             19196
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja056003zsi20050831_105453.cif
_cod_data_source_block           aj08
_cod_original_cell_volume        3882.8(13)
_cod_original_formula_sum        'C42.50 H36 Cl F3 Fe O3 P2 Pd S'
_cod_database_code               4110406