Aerobic Oxidative Amination of Unactivated Alkenes Catalyzed by Palladium
Jodie L. Brice; Jenna E. Harang; Vitaliy I. Timokhin; Natia R. Anastasi; Shannon S. Stahl; Journal of the American Chemical Society 127 (2005) 2868–2869; doi:10.1021/ja0433020

data_4111480
_publ_section_title
;
 Aerobic Oxidative Amination of Unactivated Alkenes Catalyzed by Palladium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2868
_journal_page_last               2869
_journal_paper_doi               10.1021/ja0433020
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C21 H27 N O2 S'
_chemical_formula_weight         357.50
_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                76.737(3)
_cell_angle_beta                 88.019(3)
_cell_angle_gamma                88.673(3)
_cell_formula_units_Z            2
_cell_length_a                   6.2614(10)
_cell_length_b                   8.3523(14)
_cell_length_c                   17.417(3)
_cell_measurement_temperature    100(2)
_cell_volume                     885.9(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7037
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    0.198
_exptl_absorpt_correction_T_max  0.9710
_exptl_absorpt_correction_T_min  0.9129
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_meas      0
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.287
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3542
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.287
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.3702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1616
_refine_ls_wR_factor_ref         0.1661
_reflns_number_gt                2987
_reflns_number_total             3542
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0433020si20041106_025918.cif
_cod_data_source_block           stahl20
_cod_database_code               4111480