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_4081145
_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, C8H12, Cl, O, CH2Cl2'
_chemical_formula_sum            'C55 H62 Cl3 Fe2 Ir N4 O'
_chemical_formula_weight         1205.35
_chemical_name_common            '[(Fc-NHC)2Ir(COD)][Cl]'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(0)
_cell_angle_beta                 92.6051(95)
_cell_angle_gamma                90.000(0)
_cell_formula_units_Z            4
_cell_length_a                   17.991(10)
_cell_length_b                   10.641(6)
_cell_length_c                   26.749(15)
_cell_measurement_reflns_used    12246
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.0
_cell_volume                     5116(5)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ 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  0.1334
_diffrn_reflns_av_sigmaI/netI    0.0768
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            82732
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    3.355
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.384985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Abscor. T. higashi (2001). The Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.055
_refine_diff_density_max         2.938
_refine_diff_density_min         -1.994
_refine_diff_density_rms         0.161
_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     630
_refine_ls_number_reflns         9002
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0626P)^2^+16.2434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1315
_reflns_number_gt                7488
_reflns_number_total             9002
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4004829_si_003.cif
_cod_data_source_block           compound[2][Cl]
_cod_original_cell_volume        5115.7(4)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4081145