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_4081146
_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, Ir2, C23H24N2Fe1, C16H24, Cl2'
_chemical_formula_sum            'C62 H72 Cl2 Fe2 Ir2 N4'
_chemical_formula_weight         1440.24
_chemical_name_common            '[(Fc-NHC)2Ir(COD)][Ir(COD)Cl]'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.1836(12)
_cell_length_b                   24.1836(12)
_cell_length_c                   10.5165(5)
_cell_measurement_reflns_used    4016
_cell_measurement_temperature    233(2)
_cell_volume                     6150.5(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      233(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7046
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    4.902
_exptl_absorpt_correction_T_max  0.8281
_exptl_absorpt_correction_T_min  0.2865
_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    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
The unit cell contains solvent accessible voids 
which have been treated as a diffuse 
contribution to the overall 
scattering without specific atom positions by SQUEEZE/PLATON
;
_refine_diff_density_max         0.928
_refine_diff_density_min         -1.200
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.022(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         7046
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+10.7250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1005
_reflns_number_gt                5941
_reflns_number_total             7046
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4004829_si_003.cif
_cod_data_source_block           compound[2][Ir(COD)Cl2]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P41212
_cod_database_code               4081146