Generating Active "L-Pd(0)" via Neutral or Cationic π-Allylpalladium Complexes Featuring Biaryl/Bipyrazolylphosphines: Synthetic, Mechanistic, and Structure-Activity Studies in Challenging Cross-Coupling Reactions.
DeAngelis, A. J.; Gildner, Peter G.; Chow, Ruishan; Colacot, Thomas J.; The Journal of organic chemistry 80 (2015) 6794–6813; doi:10.1021/acs.joc.5b01005

data_4031116
_publ_section_title
;
 Generating Active &quot;L-Pd(0)&quot; via Neutral or Cationic
 \p-Allylpalladium Complexes Featuring Biaryl/Bipyrazolylphosphines:
 Synthetic, Mechanistic, and Structure-Activity Studies in Challenging
 Cross-Coupling Reactions.
;
_journal_issue                   13
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              6794
_journal_page_last               6813
_journal_paper_doi               10.1021/acs.joc.5b01005
_journal_volume                  80
_journal_year                    2015
_chemical_formula_sum            'C39 H54 F3 O3 P Pd S'
_chemical_formula_weight         797.25
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 97.703(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.8856(14)
_cell_length_b                   14.3360(11)
_cell_length_c                   31.032(3)
_cell_measurement_reflns_used    5013
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      21.22
_cell_measurement_theta_min      2.30
_cell_volume                     7885.1(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0796
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            57560
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_min         1.827
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       block
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.465
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.102
_refine_diff_density_max         1.133
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         8993
_refine_ls_number_restraints     468
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+10.4099P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1186
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5807
_reflns_number_total             8993
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo5b01005_si_006.cif
_cod_data_source_block           jmca028
_cod_depositor_comments
'Adding full bibliography for 4031112--4031118.cif.'
_cod_original_cell_volume        7885.0(11)
_cod_database_code               4031116
_shelx_estimated_absorpt_t_min   0.764
_shelx_estimated_absorpt_t_max   0.940
_shelxl_version_number           2013-2
_shelx_res_checksum              5156
_shelx_hkl_checksum              16853