Synthesis of a Bis(N-heterocyclic carbene)palladium Complex via Oxidative Addition of a C-C Bond in a Biimidazolium Ion
Murray V. Baker; David H. Brown; Valerie J. Hesler; Brian W. Skelton; Allan H. White; Organometallics 26 (2007) 250–252; doi:10.1021/om0610546

data_4063242
_publ_section_title
;
 Synthesis of a Bis(N-heterocyclic carbene)palladium Complex via
 Oxidative Addition of a C-C Bond in a Biimidazolium Ion
;
_journal_name_full               Organometallics
_journal_page_first              250
_journal_page_last               252
_journal_paper_doi               10.1021/om0610546
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety
'C40 H35 Br N4 P Pd, C24 H20 B, 1.80(C H2 Cl2)'
_chemical_formula_sum            'C65.8 H58.6 B Br Cl3.6 N4 P Pd'
_chemical_formula_weight         1261.08
_chemical_name_systematic        ?
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2006-09-09T15:33:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   38.434(2)
_cell_length_b                   48.007(3)
_cell_length_c                   12.7080(7)
_cell_measurement_reflns_used    6624
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.35
_cell_measurement_theta_min      2.29
_cell_volume                     23448(2)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'xtal ADDREF SORTRF'
_computing_molecular_graphics    xtal
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_k_max       74
_diffrn_reflns_limit_k_min       -74
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22236
_diffrn_reflns_theta_full        33.9
_diffrn_reflns_theta_max         33.9
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    1.237
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  .91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             10298
_exptl_crystal_size_max          .48
_exptl_crystal_size_mid          .42
_exptl_crystal_size_min          .36
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.6
_refine_diff_density_rms         0.09
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.012(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         22236
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+46.6711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.084
_refine_ls_wR_factor_ref         0.0905
_reflns_number_gt                19090
_reflns_number_total             22236
_reflns_threshold_expression     I>2sigma(I)
_cod_original_sg_symbol_Hall     f_2_-2d
_cod_original_sg_symbol_H-M      F_d_d_2
_cod_original_formula_sum        'C65.80 H58.60 B Br Cl3.60 N4 P Pd'
_cod_database_code               4063242