Synthesis of complexes bearing NH,NMe-substituted NHCs by oxidative addition of 2-halogenato-N-methylbenzimidazoles to Ni0+
Tim Kosterke; Tania Pape; F. Ekkehardt Hahn; Chem.Commun. 47 (2011) 10773–; doi:10.1039/c1cc14243g

data_7106884
_publ_section_title
;
 Synthesis of complexes bearing NH,NMe-substituted NHCs by oxidative
 addition of 2-halogenato-N-methylbenzimidazoles to Ni0+
;
_journal_name_full               Chem.Commun.
_journal_page_first              10773
_journal_paper_doi               10.1039/c1cc14243g
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C37.5 H36 B0.5 Cl0.5 F2 I N2 Ni P2'
_chemical_formula_weight         823.36
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.7210(10)
_cell_angle_beta                 81.8170(10)
_cell_angle_gamma                69.2620(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5503(3)
_cell_length_b                   10.1764(3)
_cell_length_c                   20.2212(6)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1
_cell_volume                     1817.37(10)
_computing_cell_refinement       'APEX2(Bruker AXS, 2007)'
_computing_data_collection       'APEX2(Bruker AXS, 2007)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2007 )'
_computing_molecular_graphics
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_structure_refinement
;
SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_structure_solution
;
SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi 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  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            21343
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    1.547
_exptl_absorpt_correction_T_max  0.9551
_exptl_absorpt_correction_T_min  0.9129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Corrections were done with the SADABS program, utilizing the none merged
raw data obtained from the integration process. Integration and final cell
refinement were done with SAINT.

SADABS reports ratio of Tmin/Tmax = 0.758000

;
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent prism'
_exptl_crystal_F_000             830
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         4.147
_refine_diff_density_min         -2.690
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         10447
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0605
_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^)+(0.1108P)^2^+5.0743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1739
_refine_ls_wR_factor_ref         0.1899
_reflns_number_gt                8065
_reflns_number_total             10447
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc14243g.txt
_cod_data_source_block           sad1
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C37.50 H36 B0.50 Cl0.50 F2 I N2 Ni P2'
_cod_database_code               7106884