Intermolecular Insertion of Ethylene and Octene into a Palladium-Amide Bond. Spectroscopic Evidence for an Ethylene Amido Intermediate
Patrick S. Hanley; Dean Marković; John F. Hartwig; Journal of the American Chemical Society 132 (2010) 6302–6303; doi:10.1021/ja102172m

data_4102398
_publ_contact_author
; 
Danielle L. Gray 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       dgray@illinois.edu
_publ_contact_author_fax         '1  217 244 8068'
_publ_contact_author_phone       '1  217 244 1708'
_publ_section_title
;
 Intermolecular Insertion of Ethylene and Octene into a Palladium-Amide
 Bond. Spectroscopic Evidence for an Ethylene Amido Intermediate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6302
_journal_page_last               6303
_journal_paper_doi               10.1021/ja102172m
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C54 H68 N2 P2 Pd2'
_chemical_formula_sum            'C54 H68 N2 P2 Pd2'
_chemical_formula_weight         1019.84
_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                 102.129(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9745(8)
_cell_length_b                   18.6987(11)
_cell_length_c                   20.4170(12)
_cell_measurement_reflns_used    9777
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.51
_cell_volume                     5216.0(5)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.0-1 (Bruker, 2004)'
_computing_data_reduction
; 
SAINT V7.23A, 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  ba23iasq
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            99103
_diffrn_reflns_theta_full        27.19
_diffrn_reflns_theta_max         27.19
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_T_max  0.8640
_exptl_absorpt_correction_T_min  0.8146
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_id                ba23iasq
_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 0 -1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.446
_exptl_crystal_size_mid          0.335
_exptl_crystal_size_min          0.306
_platon_squeeze_details
;
There are 2 symmetry related voids that were squeezed.  The number of electrons
squeezed per void were equivalent to approximately 1 pentane molecule/void.
;
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     665
_refine_ls_number_reflns         11568
_refine_ls_number_restraints     410
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0244
_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^)+(0.0328P)^2^+1.3138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0624
_reflns_number_gt                9858
_reflns_number_total             11568
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja102172m_si_003.cif
_cod_data_source_block           ba23iasq
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4102398