Synthesis, Properties, and Reactivity of Palladium and Nickel NHC Complexes Supported by Combinations of Allyl, Cyclopentadienyl, and Indenyl Ligands
Bielinski, Elizabeth A.; Dai, Wei; Guard, Louise M.; Hazari, Nilay; Takase, Michael K.; Organometallics 32 (2013) 4025–; doi:10.1021/om4002632

data_4080954
_publ_section_title
;
 Synthesis, Properties, and Reactivity of Palladium and Nickel NHC
 Complexes Supported by Combinations of Allyl, Cyclopentadienyl, and
 Indenyl Ligands
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4025
_journal_paper_doi               10.1021/om4002632
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C40 H50 N2 Pd'
_chemical_formula_sum            'C40 H50 N2 Pd'
_chemical_formula_weight         665.25
_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                 101.956(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   10.6510(7)
_cell_length_b                   19.7236(13)
_cell_length_c                   17.6747(13)
_cell_measurement_reflns_used    24058
_cell_measurement_temperature    223
_cell_measurement_theta_max      24.52
_cell_measurement_theta_min      3.10
_cell_volume                     3632.5(4)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r12'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r12'
_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      223
_diffrn_detector_area_resol_mean 6.849
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku SCX mini'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28295
_diffrn_reflns_theta_full        24.41
_diffrn_reflns_theta_max         24.41
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1400.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.310
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     396
_refine_ls_number_reflns         5971
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0348P)^2^+2.9243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1050
_reflns_number_gt                4504
_reflns_number_total             5971
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om4002632_si_002.cif
_cod_data_source_block           '_IndAllPd'
_cod_original_cell_volume        3632.5(5)
_cod_database_code               4080954