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_4063240
_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         'C22 H20 N4, 2Br, C3 H6 O'
_chemical_formula_sum            'C25 H26 Br2 N4 O'
_chemical_formula_weight         558.32
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_cell_angle_alpha                80.957(3)
_cell_angle_beta                 86.821(3)
_cell_angle_gamma                75.278(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9690(10)
_cell_length_b                   10.2860(10)
_cell_length_c                   11.9850(10)
_cell_measurement_reflns_used    4372
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.5
_cell_measurement_theta_min      2.49
_cell_volume                     1173.7(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  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .038
_diffrn_reflns_av_sigmaI/netI    .124
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20859
_diffrn_reflns_theta_full        35.0
_diffrn_reflns_theta_max         35.
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.479
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  .70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.58
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             564
_exptl_crystal_size_max          .32
_exptl_crystal_size_mid          .22
_exptl_crystal_size_min          .15
_refine_diff_density_max         1.712
_refine_diff_density_min         -.978
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.038
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     289
_refine_ls_number_reflns         10267
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .093
_refine_ls_R_factor_gt           .045
_refine_ls_shift/su_max          .024
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/(sig^2^(F^2^) + 6F^2^)
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .114
_refine_ls_wR_factor_ref         .114
_reflns_d_resolution_high        .618
_reflns_d_resolution_low         11.807
_reflns_Friedel_coverage         0
_reflns_limit_h_max              16
_reflns_limit_h_min              0
_reflns_limit_k_max              16
_reflns_limit_k_min              -15
_reflns_limit_l_max              19
_reflns_limit_l_min              -19
_reflns_number_gt                6546
_reflns_number_total             10267
_reflns_threshold_expression     'I > 2.00 sig(I)'
_cod_original_sg_symbol_Hall     -p_1
_cod_original_sg_symbol_H-M      P_-1
_cod_original_formula_sum        'C25 H26 Br2 N4 O1'
_cod_database_code               4063240