Mechanistic study on the reductive elimination of (aryl)(fluoroaryl)palladium complexes: a key step in regiospecific dehydrogenative cross-coupling.
Iida, Tomoki; Sato, Ryota; Yoshigoe, Yusuke; Kanbara, Takaki; Kuwabara, Junpei; Dalton transactions (Cambridge, England : 2003) 53 (2024) 13340–13347; doi:10.1039/d4dt01453g

data_7716482
_publ_section_title
;
 Mechanistic study on the reductive elimination of
 (aryl)(fluoroaryl)palladium complexes: a key step in regiospecific
 dehydrogenative cross-coupling.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13340
_journal_page_last               13347
_journal_paper_doi               10.1039/d4dt01453g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C66 H69 F15 N6 Pd3'
_chemical_formula_sum            'C66 H69 F15 N6 Pd3'
_chemical_formula_weight         1550.49
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2024-03-08 deposited with the CCDC.	2024-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                79.1470(10)
_cell_angle_beta                 88.9540(10)
_cell_angle_gamma                76.4020(10)
_cell_formula_units_Z            2
_cell_length_a                   10.6657(12)
_cell_length_b                   15.3472(17)
_cell_length_c                   20.4601(20)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    90
_cell_measurement_theta_max      27.20
_cell_measurement_theta_min      9904
_cell_volume                     3195.8(6)
_computing_cell_refinement       Unknown
_computing_data_collection       Unknown
_computing_data_reduction        Unknown
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2014 (Burla, et al., 2014)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            36797
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.197
_diffrn_reflns_theta_min         1.014
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.925
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6782
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            nONE
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       nONE
_exptl_crystal_F_000             1560.00
_exptl_crystal_size_max          0.346
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.61
_refine_diff_density_min         -1.29
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.338
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     844
_refine_ls_number_reflns         14132
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+12.1233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1036
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13554
_reflns_number_total             14132
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d4dt01453g3.cif
_cod_data_source_block           iid128_3_in_P-1
_cod_depositor_comments
'Adding full bibliography for 7716482--7716483.cif.'
_cod_database_code               7716482
_shelx_res_checksum              21053
_shelx_hkl_checksum              25676