Synthesis of Novel Chelating Benzimidazole-Based Carbenes and Their Nickel(II) Complexes: Activity in the Kumada Coupling Reaction
Berding, Joris; Lutz, Martin; Spek, Anthony L.; Bouwman, Elisabeth; Organometallics 28 (2009) 1845–; doi:10.1021/om8010596

data_4068731
_publ_section_title
;
 Synthesis of Novel Chelating Benzimidazole-Based Carbenes and Their
 Nickel(II) Complexes: Activity in the Kumada Coupling Reaction
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1845
_journal_paper_doi               10.1021/om8010596
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C31 H28 Br2 N4 Ni, C H2 Cl2'
_chemical_formula_sum            'C32 H30 Br2 Cl2 N4 Ni'
_chemical_formula_weight         760.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.788(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7277(4)
_cell_length_b                   15.0886(6)
_cell_length_c                   25.4183(9)
_cell_measurement_reflns_used    30644
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      1.59
_cell_volume                     3571.8(2)
_computing_cell_refinement       Peakref
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'EvalCCD, Sadabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            54246
_diffrn_reflns_theta_full        25.53
_diffrn_reflns_theta_max         25.53
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    2.955
_exptl_absorpt_correction_T_max  0.64
_exptl_absorpt_correction_T_min  0.29
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
;
_refine_diff_density_max         1.588
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0579
_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^)+(0.0332P)^2^+42.9633P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1472
_refine_ls_wR_factor_ref         0.1508
_reflns_number_gt                5564
_reflns_number_total             6591
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om8010596_si_002.cif
_cod_data_source_block           s3794a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4068731