Cationic Iridium Complexes Containing Anionic Iridium Counterions Supported by Redox-Active N-Heterocyclic Carbenes
Arumugam, Kuppuswamy; Chang, Jinho; Lynch, Vincent M.; Bielawski, Christopher W.; Organometallics 32 (2013) 4334–; doi:10.1021/om4004829

data_4081147
_publ_section_title
;
 Cationic Iridium Complexes Containing Anionic Iridium Counterions
 Supported by Redox-Active N-Heterocyclic Carbenes
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4334
_journal_paper_doi               10.1021/om4004829
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety
'C23H24N2Fe1, Ir, C23H24N2Fe1, C2O2, Ir, Cl2, C2O2'
_chemical_formula_sum            'C50 H48 Cl2 Fe2 Ir2 N4 O4'
_chemical_formula_weight         1335.89
_chemical_name_common            '[(Fc-NHC)2Ir(CO)2][Ir(CO2)Cl2]'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.491(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.027(13)
_cell_length_b                   16.749(13)
_cell_length_c                   19.181(15)
_cell_measurement_reflns_used    5873
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     4962(7)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_solution
;
SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku SCX-Mini with Mercury CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21542
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    6.074
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Abscor. T. higashi (2001). The Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.191
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.055
_refine_diff_density_max         1.683
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.408(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         8707
_refine_ls_number_restraints     386
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+18.6514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0850
_reflns_number_gt                8005
_reflns_number_total             8707
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4004829_si_003.cif
_cod_data_source_block           compound[3][Ir(CO)2Cl2]
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               4081147