Synthesis of Palladium and Platinum Complexes with Phosphine-Functionalized Benzimidazolin-2-ylidene Ligands
Hahn, F. Ekkehardt; Jahnke, Mareike C.; Pape, Tania; Organometallics 25 (2006) 5927–; doi:10.1021/om060741u

data_4074544
_publ_section_title
;
 Synthesis of Palladium and Platinum Complexes with
 Phosphine-Functionalized Benzimidazolin-2-ylidene Ligands
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              5927
_journal_paper_doi               10.1021/om060741u
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C42.5 H43 B2 F8 N3 O0.5 P2 Pd'
_chemical_formula_weight         945.76
_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                101.099(2)
_cell_angle_beta                 95.263(2)
_cell_angle_gamma                93.406(2)
_cell_formula_units_Z            4
_cell_length_a                   11.3796(3)
_cell_length_b                   16.7644(5)
_cell_length_c                   22.7228(7)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70
_cell_measurement_theta_min      1
_cell_volume                     4222.7(2)
_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      100(2)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 0.874
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  goebel-mirror
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_sigmaI/netI    0.0953
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24679
_diffrn_reflns_theta_full        69.99
_diffrn_reflns_theta_max         69.99
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    4.883
_exptl_absorpt_correction_T_max  0.4572
_exptl_absorpt_correction_T_min  0.2123
_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  0.484290
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent prism'
_exptl_crystal_F_000             1924
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.301
_refine_diff_density_min         -1.051
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1104
_refine_ls_number_reflns         13986
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0836P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1474
_reflns_number_gt                9451
_reflns_number_total             13986
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060741usi20060815_021533.cif
_cod_data_source_block           sad_complex_22
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C42.50 H43 B2 F8 N3 O0.50 P2 Pd'
_cod_database_code               4074544