Effects of PAr3Ligands on Direct Arylation of Heteroarenes with Isolated [Pd(2,6-Me2C6H3)(μ-O2CMe)(PAr3)]4Complexes
Wakioka, Masayuki; Nakamura, Yuki; Hihara, Yoshihiro; Ozawa, Fumiyuki; Sakaki, Shigeyoshi; Organometallics 33 (2014) 6247–; doi:10.1021/om500922n

data_4084463
_publ_section_title
;
 Effects of PAr3Ligands on Direct Arylation of Heteroarenes with Isolated
 [Pd(2,6-Me2C6H3)(\m-O2CMe)(PAr3)]4Complexes
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6247
_journal_paper_doi               10.1021/om500922n
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         '(C112 H96 F12 O8 P4 Pd4), 6(C4 H8 O)'
_chemical_formula_sum            'C136 H144 F12 O14 P4 Pd4'
_chemical_formula_weight         2779.99
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.712(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.313(7)
_cell_length_b                   14.755(3)
_cell_length_c                   28.978(6)
_cell_measurement_reflns_used    14578
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      4-046.cif
_cell_measurement_theta_min      3.0761
_cell_volume                     12844(5)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            53465
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.08
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.9050
_exptl_absorpt_correction_T_min  0.8120
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5696
_exptl_crystal_recrystallization_method THF/pentane
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.307
_refine_diff_density_min         -1.100
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         11913
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0713P)^2^+50.3354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1348
_reflns_number_gt                10601
_reflns_number_total             11913
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500922n_si_002.cif
_cod_data_source_block           1c
_cod_depositor_comments          'Adding full bibliography for 4084463.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4084463