Factors Controlling the Reactivity of Heteroarenes in Direct Arylation with Arylpalladium Acetate Complexes
Wakioka, Masayuki; Nakamura, Yuki; Hihara, Yoshihiro; Ozawa, Fumiyuki; Sakaki, Shigeyoshi; Organometallics 32 (2013) 4423–; doi:10.1021/om400636r

data_4081194
_publ_section_title
;
 Factors Controlling the Reactivity of Heteroarenes in Direct Arylation
 with Arylpalladium Acetate Complexes
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4423
_journal_paper_doi               10.1021/om400636r
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         '2(C35 H32 N O2 P Pd S), C4 H8 O'
_chemical_formula_sum            'C37 H36 N O2.5 P Pd S'
_chemical_formula_weight         704.10
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 106.4247(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.3110(10)
_cell_length_b                   28.404(2)
_cell_length_c                   19.4605(17)
_cell_measurement_reflns_used    21202
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      31.2666
_cell_measurement_theta_min      2.4121
_cell_volume                     6527.3(9)
_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      103(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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     0.71075
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45107
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.40
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  0.9650
_exptl_absorpt_correction_T_min  0.8939
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2896
_exptl_crystal_recrystallization_method THF/pentane
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.503
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     765
_refine_ls_number_reflns         11978
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+12.2001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                10721
_reflns_number_total             11978
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400636r_si_002.cif
_cod_data_source_block           2c_8
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4081194