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_4080949
_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_sum            'C43 H56 N2 Pd'
_chemical_formula_weight         707.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.757(7)
_cell_angle_beta                 96.156(7)
_cell_angle_gamma                91.899(7)
_cell_formula_units_Z            2
_cell_length_a                   10.1993(2)
_cell_length_b                   12.3405(3)
_cell_length_c                   15.3944(11)
_cell_measurement_reflns_used    49006
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.4
_cell_measurement_theta_min      3.0
_cell_volume                     1840.45(16)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 22.2
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'microfocus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1210
_diffrn_reflns_av_sigmaI/netI    0.0627
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            59912
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    4.287
_exptl_absorpt_correction_T_max  0.8822
_exptl_absorpt_correction_T_min  0.6738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.258
_refine_diff_density_min         -2.008
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+4.6745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1390
_reflns_number_gt                5810
_reflns_number_total             6556
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4002632_si_002.cif
_cod_data_source_block           '_CpAllPd'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4080949