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_4078722
_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            'C54 H51 O4.5 P2 Pd2'
_chemical_formula_weight         1046.69
_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                 91.846(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.884(6)
_cell_length_b                   17.730(9)
_cell_length_c                   23.000(11)
_cell_measurement_reflns_used    6706
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4612
_cell_measurement_theta_min      3.0172
_cell_volume                     4844(4)
_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  0.0757
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            40238
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.02
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.854
_exptl_absorpt_correction_T_max  0.9586
_exptl_absorpt_correction_T_min  0.8898
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2132
_exptl_crystal_recrystallization_method dichloromethane/pentane
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.853
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         8509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.0926
_refine_ls_shift/su_max          0.129
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1006P)^2^+16.1236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2220
_refine_ls_wR_factor_ref         0.2411
_reflns_number_gt                6555
_reflns_number_total             8509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300367k_si_002.cif
_cod_data_source_block           1b
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C54 H51 O4.50 P2 Pd2'
_cod_database_code               4078722