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_4118656
_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         'C70 H98 Cl2 N4 Pd2, 1.5(C5H12)'
_chemical_formula_sum            'C85 H116 Cl2 N4 Pd2'
_chemical_formula_weight         1477.52
_chemical_name_systematic
; 
? 
;
_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
_audit_update_record
; 
? 
;
_cell_angle_alpha                102.478(3)
_cell_angle_beta                 92.417(3)
_cell_angle_gamma                109.701(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7161(5)
_cell_length_b                   14.8135(6)
_cell_length_c                   23.0484(13)
_cell_measurement_reflns_used    8502
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      67.55
_cell_measurement_theta_min      3.27
_cell_volume                     3648.2(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 0.959
_diffrn_measured_fraction_theta_max 0.959
_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  bc45sasq
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_sigmaI/netI    0.0763
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            12743
_diffrn_reflns_theta_full        67.93
_diffrn_reflns_theta_max         67.93
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    5.005
_exptl_absorpt_correction_T_max  0.8232
_exptl_absorpt_correction_T_min  0.3926
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       prism
_exptl_crystal_F_000             1560
_exptl_crystal_id                bc45sasq
_exptl_crystal_preparation
; 
The data crystal was mounted using ??oil (Parantone-N, Exxon) to a 
??0.3 mm cryo-loop (Hampton Research)?? 
??0.2 mm Kapton micromount (Thorne, 2003)?? 
with the (??) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.045
_platon_squeeze_details
; 
This amount of electrons squeezed out is consistant with the 1.5 pentane 
molecules per asymmetric unit predicted by the disordered model. 
;
_refine_diff_density_max         0.947
_refine_diff_density_min         -1.044
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         12743
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0677P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1205
_reflns_number_gt                9796
_reflns_number_total             12743
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja307558x_si_002.cif
_cod_data_source_block           bc45sasq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_ambient_temperature' value '193(2' was changed to '193(2)' -
precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4118656