Synthesis of Pincer-Type Bis(benzimidazolin-2-ylidene) Palladium Complexes and Their Application in C−C Coupling Reactions
Hahn, F. Ekkehardt; Jahnke, Mareike C.; Pape, Tania; Organometallics 26 (2007) 150–; doi:10.1021/om060882w

data_4072616
_publ_section_title
;
 Synthesis of Pincer-Type Bis(benzimidazolin-2-ylidene) Palladium
 Complexes and Their Application in C&#x2212;C Coupling Reactions
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              150
_journal_paper_doi               10.1021/om060882w
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C30 H33 Br N4 Pd'
_chemical_formula_weight         635.91
_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                102.4340(10)
_cell_angle_beta                 94.2730(10)
_cell_angle_gamma                113.3970(10)
_cell_formula_units_Z            2
_cell_length_a                   8.68300(10)
_cell_length_b                   10.7218(2)
_cell_length_c                   15.8253(3)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      75
_cell_measurement_theta_min      1
_cell_volume                     1299.22(4)
_computing_cell_refinement       'SAINT (Bruker AXS, 2000)'
_computing_data_collection       'SMART (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2000)'
_computing_molecular_graphics
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 0.856
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7478
_diffrn_reflns_theta_full        71.04
_diffrn_reflns_theta_max         71.04
_diffrn_reflns_theta_min         5.59
_exptl_absorpt_coefficient_mu    7.760
_exptl_absorpt_correction_T_max  0.8006
_exptl_absorpt_correction_T_min  0.2284
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Corrections were done with the SADABS program, utilizing the none merged
 raw data obtained from the integration process. Integration and final cell
 refinement were done with SAINT.

 SADABS reports  
 Maximum and minimum effective transmission:  1.000000  0.553044
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent plates'
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.417
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0853P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1221
_reflns_number_gt                3672
_reflns_number_total             4308
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060882wsi20060926_010501.cif
_cod_data_source_block           sad
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4072616