One-Pot, Single-Step, and Gram-Scale Synthesis of Mononuclear [(η6-arene)Ni(N-heterocyclic carbene)] Complexes: Useful Precursors of the Ni0‒NHC Unit
Hoshimoto, Yoichi; Hayashi, Yukari; Suzuki, Haruka; Ohashi, Masato; Ogoshi, Sensuke; Organometallics 33 (2014) 1276–; doi:10.1021/om500088p

data_4082691
_publ_section_title
;
 One-Pot, Single-Step, and Gram-Scale Synthesis of Mononuclear
 [(\h6-arene)Ni(N-heterocyclic carbene)] Complexes: Useful Precursors of
 the Ni0--NHC Unit
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1276
_journal_paper_doi               10.1021/om500088p
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C36 H44 N3 Ni'
_chemical_formula_sum            'C36 H44 N3 Ni'
_chemical_formula_weight         577.46
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   16.417(8)
_cell_length_b                   17.435(9)
_cell_length_c                   21.669(11)
_cell_measurement_reflns_used    11688
_cell_measurement_temperature    273
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.08
_cell_volume                     6202(5)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_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      273
_diffrn_detector_area_resol_mean 6.827
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            54188
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.57
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_correction_T_min  0.609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            gray
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2472.00
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.410
_exptl_crystal_size_min          0.360
_refine_diff_density_max         1.360
_refine_diff_density_min         -0.640
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     369
_refine_ls_number_reflns         7141
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1130P)^2^+2.3576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1961
_reflns_number_gt                5612
_reflns_number_total             7141
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om500088p_si_002.cif
_cod_data_source_block           complex1
_cod_original_cell_volume        6202(6)
_cod_database_code               4082691