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_4063241
_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         'C10 H16 N4, 2I'
_chemical_formula_sum            'C10 H16 I2 N4'
_chemical_formula_weight         446.1
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_cell_angle_alpha                90.00000
_cell_angle_beta                 104.6030(10)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   9.2022(5)
_cell_length_b                   15.0505(8)
_cell_length_c                   11.0279(6)
_cell_measurement_reflns_used    8846
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      37.5
_cell_measurement_theta_min      2.29
_cell_volume                     1478.00(14)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'Siemens SAINT'
_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  .026
_diffrn_reflns_av_sigmaI/netI    .024
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29258
_diffrn_reflns_theta_full        37.5
_diffrn_reflns_theta_max         37.5
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.239
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  .629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          .38
_exptl_crystal_size_mid          .18
_exptl_crystal_size_min          .18
_refine_diff_density_max         1.346
_refine_diff_density_min         -1.338
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.046
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     145
_refine_ls_number_reflns         7750
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .029
_refine_ls_R_factor_gt           .025
_refine_ls_shift/su_max          .003
_refine_ls_shift/su_mean         .0003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/(sig^2^(F^2^) + 7*F^2^)
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .056
_refine_ls_wR_factor_ref         .062
_reflns_d_resolution_high        .584
_reflns_d_resolution_low         8.69
_reflns_Friedel_coverage         0
_reflns_limit_h_max              15
_reflns_limit_h_min              0
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              -18
_reflns_number_gt                6948
_reflns_number_total             7750
_reflns_threshold_expression     'Fsqd >  .00 sig(Fsqd)'
_cod_original_sg_symbol_Hall     -p_2ybc
_cod_original_sg_symbol_H-M      P_1_21/c_1
_cod_database_code               4063241