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_4106825
_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         'C32.50 H32.50 B2 F8 N4.50 O Pd2'
_chemical_formula_sum            'C32.5 H32.5 B2 F8 N4.5 O Pd2'
_chemical_formula_weight         888.55
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                89.2379(18)
_cell_angle_beta                 81.8766(19)
_cell_angle_gamma                78.1690(19)
_cell_formula_units_Z            4
_cell_length_a                   10.2184(7)
_cell_length_b                   13.8764(10)
_cell_length_c                   25.8461(18)
_cell_measurement_reflns_used    22251
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.00
_cell_volume                     3550.5(4)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.1161
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            53334
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.089
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_correction_T_min  0.468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            unknown
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1764.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.700
_refine_diff_density_min         -1.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     954
_refine_ls_number_reflns         6089
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.057
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
    Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
    6.5805    0.6492    4.7262
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0704
_reflns_number_gt                6089
_reflns_number_total             16181
_reflns_threshold_expression     F>3.0\s(F)
_cod_data_source_file            ja206076u_si_004.cif
_cod_data_source_block           takase3
_cod_original_cell_volume        3550.5(5)
_cod_original_formula_sum        'C32.50 H32.50 B2 F8 N4.50 O Pd2'
_cod_database_code               4106825