Direct Arylation of 2-Methylthiophene with Isolated [PdAr(μ-O2CR)(PPh3)]nComplexes: Kinetics and Mechanism
Wakioka, Masayuki; Nakamura, Yuki; Wang, Qifeng; Ozawa, Fumiyuki; Organometallics 31 (2012) 4810–; doi:10.1021/om300367k

data_4078723
_publ_section_title
;
 Direct Arylation of 2-Methylthiophene with Isolated
 [PdAr(\m-O2CR)(PPh3)]nComplexes: Kinetics and Mechanism
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              4810
_journal_paper_doi               10.1021/om300367k
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C114 H112 Cl4 O8 P4 Pd4'
_chemical_formula_weight         2301.32
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      82
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.130(7)
_cell_length_b                   20.130(7)
_cell_length_c                   14.315(5)
_cell_measurement_reflns_used    6210
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4463
_cell_measurement_theta_min      3.1856
_cell_volume                     5801(3)
_computing_cell_refinement       'Rigaku AFC10/Saturn 70 CCD'
_computing_data_collection       'Rigaku AFC10/Saturn 70 CCD'
_computing_data_reduction        'Rigaku AFC10/Saturn 70 CCD'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'ORTEP3 for windows'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0800
_diffrn_reflns_av_sigmaI/netI    0.0867
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20008
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.19
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.808
_exptl_absorpt_correction_T_max  0.9762
_exptl_absorpt_correction_T_min  0.8297
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2344
_exptl_crystal_recrystallization_method dichloromethane/hexane
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.556
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.41(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         5397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0862
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1147P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2027
_refine_ls_wR_factor_ref         0.2147
_reflns_number_gt                4392
_reflns_number_total             5397
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300367k_si_002.cif
_cod_data_source_block           1c
_cod_original_cell_volume        5801(4)
_cod_database_code               4078723