Amination of Aryl Iodides Catalyzed by a Palladium‒Copper Complex Supported by a Chelate-Bridging Ligand
Tsukada, Naofumi; Ohnishi, Nozomi; Aono, Shiori; Takahashi, Fusako; Organometallics 31 (2012) 7336–; doi:10.1021/om300902t

data_4079643
_publ_section_title
;
 Amination of Aryl Iodides Catalyzed by a Palladium--Copper Complex
 Supported by a Chelate-Bridging Ligand
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              7336
_journal_paper_doi               10.1021/om300902t
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C60 H53 N6 O0.50 P2 Pd2'
_chemical_formula_sum            'C60 H53 N6 O0.5 P2 Pd2'
_chemical_formula_weight         1140.87
_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                 98.0570
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   10.8651(5)
_cell_length_b                   14.8098(7)
_cell_length_c                   32.5690(13)
_cell_measurement_reflns_used    12933
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.03
_cell_volume                     5188.9(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            27804
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.802
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2324.00
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.620
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     633
_refine_ls_number_reflns         8958
_refine_ls_number_restraints     146
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0214P)^2^+9.3450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0880
_reflns_number_gt                8089
_reflns_number_total             8958
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om300902t_si_002.cif
_cod_data_source_block           complex1_Me2Pd2(dpqfam)2
_cod_original_formula_sum        'C60 H53 N6 O0.50 P2 Pd2'
_cod_database_code               4079643