Oxidative Dinuclear Addition of a PdI-PdI Moiety to Arenes: Generation of μ-η3:η3-Arene-PdII2 Species
Tetsuro Murahashi; Kohei Takase; Masa-aki Oka; Sensuke Ogoshi; Journal of the American Chemical Society 133 (2011) 14908–14911; doi:10.1021/ja206076u

data_4106823
_publ_section_title
;
 Oxidative Dinuclear Addition of a PdI-PdI Moiety to Arenes: Generation of
 \m-\h3:\h3-Arene-PdII2 Species
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14908
_journal_page_last               14911
_journal_paper_doi               10.1021/ja206076u
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C49.50 H41 B2 F8 N4.50 O Pd2'
_chemical_formula_sum            'C49.5 H41 B2 F8 N4.5 O Pd2'
_chemical_formula_weight         1101.31
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 98.0275(12)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   17.4255(7)
_cell_length_b                   23.6328(10)
_cell_length_c                   21.2105(9)
_cell_measurement_reflns_used    27197
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.04
_cell_volume                     8649.2(6)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0939
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            79121
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_description       block
_exptl_crystal_F_000             4412.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.580
_refine_diff_density_min         -0.988
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1289
_refine_ls_number_reflns         10553
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.157
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
    Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
    4.6291    1.2093    3.6902
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0571
_reflns_number_gt                10553
_reflns_number_total             19201
_reflns_threshold_expression     F>3.0\s(F)
_cod_data_source_file            ja206076u_si_002.cif
_cod_data_source_block           takase14
_cod_original_formula_sum        'C49.50 H41 B2 F8 N4.50 O Pd2'
_cod_database_code               4106823