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_4068730
_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         'C19 H20 Br2 N4 Ni, C H2 Cl2'
_chemical_formula_sum            'C20 H22 Br2 Cl2 N4 Ni'
_chemical_formula_weight         607.85
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 133.513(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.885(2)
_cell_length_b                   19.126(4)
_cell_length_c                   15.216(3)
_cell_measurement_reflns_used    13648
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.29
_cell_measurement_theta_min      2.15
_cell_volume                     2297.3(8)
_computing_cell_refinement       Peakref
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'EvalCCD, ABST, Mergehklf5'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.1140
_diffrn_reflns_av_sigmaI/netI    0.0554
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            41727
_diffrn_reflns_theta_full        25.79
_diffrn_reflns_theta_max         25.79
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    4.570
_exptl_absorpt_correction_T_max  0.76
_exptl_absorpt_correction_T_min  0.28
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.204
_refine_diff_density_min         -1.592
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         7247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+10.8193P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1681
_reflns_number_gt                5829
_reflns_number_total             7247
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8010596_si_002.cif
_cod_data_source_block           s3777a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4068730