Enhanced Activity of [Ni(NHC)CpCl] Complexes in Arylamination Catalysis
Martin, Anthony R.; Makida, Yusuke; Meiries, Sébastien; Slawin, Alexandra M. Z.; Nolan, Steven P.; Organometallics 32 (2013) 6265–; doi:10.1021/om4004863

data_4081771
_publ_section_title
;
 Enhanced Activity of [Ni(NHC)CpCl] Complexes in Arylamination Catalysis
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6265
_journal_paper_doi               10.1021/om4004863
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C40 H57 Cl N2 Ni'
_chemical_formula_sum            'C40 H57 Cl N2 Ni'
_chemical_formula_weight         660.06
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 112.675(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   12.050(4)
_cell_length_b                   23.034(7)
_cell_length_c                   14.375(5)
_cell_measurement_reflns_used    5854
_cell_measurement_temperature    93
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.03
_cell_volume                     3682(2)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 rc13'
_computing_data_collection
'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 rc13'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11603
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.32
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1424.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.350
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  2195 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.66(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5552
_refine_ls_number_restraints     2
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0329P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1199
_reflns_number_gt                4210
_reflns_number_total             5552
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om4004863_si_002.cif
_cod_data_source_block           4
_cod_original_cell_volume        3681(2)
_cod_database_code               4081771