Ligandless, Anionic, Arylpalladium Halide Intermediates in the Heck Reaction
Brad P. Carrow; John. F. Hartwig; Journal of the American Chemical Society 132 (2010) 79–81; doi:10.1021/ja909306f

data_4101772
_publ_contact_author
; 
Scott R. Wilson 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       srwilson@uiuc.edu
_publ_contact_author_fax         '1  217 244 8068'
_publ_contact_author_phone       '1  217 244 1708'
_publ_section_title
;
 Ligandless, Anionic, Arylpalladium Halide Intermediates in the Heck
 Reaction
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              79
_journal_page_last               81
_journal_paper_doi               10.1021/ja909306f
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C14 H8 Br4 F6 Pd2, 2(C12 H28 P)'
_chemical_formula_sum            'C38 H64 Br4 F6 P2 Pd2'
_chemical_formula_weight         1229.27
_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
; 
2007-09-07   text and data added, srw 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.246(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.6562(4)
_cell_length_b                   9.0426(4)
_cell_length_c                   25.5092(11)
_cell_measurement_reflns_used    6174
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      23.65
_cell_measurement_theta_min      2.39
_cell_volume                     2447.76(18)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.0-1 (Bruker, 2004)'
_computing_data_reduction        'SAINT V7.23A (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL V6.12 (Bruker, 2005)'
_computing_publication_material  'XCIF (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  ga42vas
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            34711
_diffrn_reflns_theta_full        27.65
_diffrn_reflns_theta_max         27.65
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    4.112
_exptl_absorpt_correction_T_max  0.8252
_exptl_absorpt_correction_T_min  0.4238
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP (Bruker, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       columnar
_exptl_crystal_F_000             1216
_exptl_crystal_id                ga42vas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-5 -1 3) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         5623
_refine_ls_number_restraints     172
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+3.5084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.1040
_reflns_number_gt                3349
_reflns_number_total             5623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja909306f_si_002.cif
_cod_data_source_block           ga42vas
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               4101772