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_4118658
_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_absolute_configuration ad
_chemical_formula_moiety         'C35 H51 Cl N2 Pd , 0.5(C5 H12)'
_chemical_formula_sum            'C40 H63 Cl N2 Pd'
_chemical_formula_weight         713.77
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7615(3)
_cell_length_b                   13.4772(5)
_cell_length_c                   29.0572(13)
_cell_measurement_reflns_used    2050
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      51.44
_cell_measurement_theta_min      3.04
_cell_volume                     3822.7(3)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  bc99rasq
_diffrn_reflns_av_R_equivalents  0.1238
_diffrn_reflns_av_sigmaI/netI    0.0843
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30073
_diffrn_reflns_theta_full        67.54
_diffrn_reflns_theta_max         67.54
_diffrn_reflns_theta_min         4.47
_exptl_absorpt_coefficient_mu    4.753
_exptl_absorpt_correction_T_max  0.8439
_exptl_absorpt_correction_T_min  0.3790
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       prism
_exptl_crystal_F_000             1520
_exptl_crystal_id                bc99rasq
_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 1 -9) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.045
_platon_squeeze_details
; 
After the "squeeze" bypass routine, 46 electrons each were removed 
from two solvent accessible voids.  This is equivalent to approximately 
two pentane molecules per unit cell, which is consistant with that 
predicted from the highly disordered model. 
;
_refine_diff_density_max         0.709
_refine_diff_density_min         -1.677
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack (1983),  2906 Friedels'
_refine_ls_abs_structure_Flack   0.444(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         6751
_refine_ls_number_restraints     364
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1540
_reflns_number_gt                5571
_reflns_number_total             6751
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja307558x_si_004.cif
_cod_data_source_block           bc99rasq
_cod_original_sg_symbol_Hall     'P 2ac 2ab '
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               4118658