Reductive Elimination of Alkylamines from Low-Valent, Alkylpalladium(II) Amido Complexes
Patrick S. Hanley; Seth L. Marquard; Thomas R. Cundari; John F. Hartwig; Journal of the American Chemical Society 134 (2012) 15281–15284; doi:10.1021/ja307558x

data_4118659
_publ_contact_author
; 
John F. Hartwig 
University of California, Berkeley 
Department of Chemistry  
718 Latimer Hall 
Berkeley, CA 94720-1460 
USA 
;
_publ_contact_author_email       jhartwig@berkeley.edu
_publ_contact_author_fax         '1  510-642-7714'
_publ_contact_author_phone       '1  510-642-2038'
_publ_section_title
;
 Reductive Elimination of Alkylamines from Low-Valent, Alkylpalladium(II)
 Amido Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15281
_journal_page_last               15284
_journal_paper_doi               10.1021/ja307558x
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C42 H59 N3 O Pd '
_chemical_formula_sum            'C42 H59 N3 O Pd'
_chemical_formula_weight         728.32
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 108.1840(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8298(3)
_cell_length_b                   15.9470(3)
_cell_length_c                   19.8577(4)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      67.43
_cell_measurement_theta_min      3.65
_cell_volume                     3859.92(14)
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_wavelength_id  bc21qas
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33291
_diffrn_reflns_theta_full        67.96
_diffrn_reflns_theta_max         67.96
_diffrn_reflns_theta_min         3.63
_exptl_absorpt_coefficient_mu    4.128
_exptl_absorpt_correction_T_max  0.8404
_exptl_absorpt_correction_T_min  0.3866
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_description       plate
_exptl_crystal_F_000             1544
_exptl_crystal_id                bc21qas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (0 4 1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.378
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.064
_refine_diff_density_max         1.499
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         6914
_refine_ls_number_restraints     385
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+3.0095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1056
_reflns_number_gt                6235
_reflns_number_total             6914
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja307558x_si_005.cif
_cod_data_source_block           bc21qas
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4118659