Intermolecular Migratory Insertion of Unactivated Olefins into Palladium-Nitrogen Bonds. Steric and Electronic Effects on the Rate of Migratory Insertion
Patrick S. Hanley; John F. Hartwig; Journal of the American Chemical Society 133 (2011) 15661–15673; doi:10.1021/ja205722f

data_4106876
_publ_section_title
;
 Intermolecular Migratory Insertion of Unactivated Olefins into
 Palladium-Nitrogen Bonds. Steric and Electronic Effects on the Rate of
 Migratory Insertion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15661
_journal_page_last               15673
_journal_paper_doi               10.1021/ja205722f
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C42 H59 N O P2 Pd2'
_chemical_formula_sum            'C42 H59 N O P2 Pd2'
_chemical_formula_weight         868.64
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
? 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.453(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.2843(15)
_cell_length_b                   9.3814(7)
_cell_length_c                   20.7994(14)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.89
_cell_measurement_theta_min      2.38
_cell_volume                     4140.6(5)
_computing_cell_refinement       'SAINT V7.68A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2010.11-3 (Bruker, 2010)'
_computing_data_reduction
; 
SAINT V7.68A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5 
(Bruker, 2005 & 2007) 
;
_computing_molecular_graphics
; 
SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  Complex5
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            58747
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.977
_exptl_absorpt_correction_T_max  0.9545
_exptl_absorpt_correction_T_min  0.6951
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1792
_exptl_crystal_id                Complex5
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-1 -1 3) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.564
_exptl_crystal_size_mid          0.309
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         9102
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0300P)^2^+3.6019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0802
_reflns_number_gt                6818
_reflns_number_total             9102
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja205722f_si_002.cif
_cod_data_source_block           Complex5
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4106876