N-Heterocyclic Dicarbene Iridium(III) Pincer Complexes Featuring Mixed NHC/Abnormal NHC Ligands and Their Applications in the Transfer Dehydrogenation of Cyclooctane
Zuo, Weiwei; Braunstein, Pierre; Organometallics 31 (2012) 2606–; doi:10.1021/om200444q

data_4077836
_publ_section_title
;
 N-Heterocyclic Dicarbene Iridium(III) Pincer Complexes Featuring Mixed
 NHC/Abnormal NHC Ligands and Their Applications in the Transfer
 Dehydrogenation of Cyclooctane
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2606
_journal_paper_doi               10.1021/om200444q
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C32 H40 N4,2(Br), 0.5(C H2 Cl2) '
_chemical_formula_sum            'C32.5 H41 Br2 Cl N4'
_chemical_formula_weight         682.96
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 104.184(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.3057(10)
_cell_length_b                   14.5628(9)
_cell_length_c                   12.9205(5)
_cell_measurement_reflns_used    6331
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     3156.9(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0560
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9934
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.80
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.681
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.205
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         5821
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0701P)^2^+1.8758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1316
_reflns_number_gt                4239
_reflns_number_total             5821
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200444q_si_002.cif
_cod_data_source_block           adamantane_di_imidazolium_Zuo2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C32.50 H41 Br2 Cl N4'
_cod_database_code               4077836