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_4118657
_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         '4(C42 H57 N3 Pd), C5 H12 '
_chemical_formula_sum            'C173 H240 N12 Pd4'
_chemical_formula_weight         2913.37
_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                 97.774(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.517(5)
_cell_length_b                   22.963(11)
_cell_length_c                   32.741(16)
_cell_measurement_reflns_used    7377
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      21.68
_cell_measurement_theta_min      2.16
_cell_volume                     7834(7)
_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      183(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Siemens Platform/ApexII CCD'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  bm54sasq
_diffrn_reflns_av_R_equivalents  0.0886
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            74015
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         1.09
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  0.9688
_exptl_absorpt_correction_T_min  0.8744
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       prism
_exptl_crystal_F_000             3092
_exptl_crystal_id                bm54sasq
_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 -3 -1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.099
_platon_squeeze_details
; 
After the "squeeze" bypass routine, 42 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 disordered model. 
;
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     949
_refine_ls_number_reflns         14240
_refine_ls_number_restraints     477
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1081
_reflns_number_gt                9761
_reflns_number_total             14240
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja307558x_si_003.cif
_cod_data_source_block           bm54sasq
_cod_original_cell_volume        7835(7)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4118657