Understanding the Unusual Reduction Mechanism of Pd(II) to Pd(I): Uncovery of Hidden Species and Implications in Catalytic Cross-Coupling Reactions.
Johansson Seechurn, Carin C. C.; Sperger, Theresa; Scrase, Thomas G.; Schoenebeck, Franziska; Colacot, Thomas J.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b01110

data_4125878
_publ_section_title
;
 Understanding the Unusual Reduction Mechanism of Pd(II) to Pd(I):
 Uncovery of Hidden Species and Implications in Catalytic Cross-Coupling
 Reactions.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b01110
_journal_year                    2017
_chemical_formula_moiety         '2(C12 H27 Br P +), Br6 Pd2 2-'
_chemical_formula_sum            'C24 H54 Br8 P2 Pd2'
_chemical_formula_weight         1256.69
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.8809(2)
_cell_length_b                   15.7708(2)
_cell_length_c                   28.0382(4)
_cell_measurement_reflns_used    48342
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.00
_cell_volume                     7906.66(17)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL-2013
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0915
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            60204
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.029
_diffrn_reflns_theta_min         3.521
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    9.091
_exptl_absorpt_correction_T_max  0.535
_exptl_absorpt_correction_T_min  0.354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.111
_exptl_crystal_description       plate
_exptl_crystal_F_000             4800
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.945
_refine_diff_density_min         -1.239
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0565P)^2^+14.3604P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1094
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5195
_reflns_number_total             6816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b01110_si_002.cif
_cod_data_source_block           jm1501
_cod_database_code               4125878
_shelx_estimated_absorpt_t_min   0.408
_shelx_estimated_absorpt_t_max   0.659
_shelxl_version_number           2013-4
_shelx_res_checksum              872
_shelx_hkl_checksum              40781