Stepwise and one-pot syntheses of Ir(iii) complexes with imidazolium-based carbene ligands
Chien, Chih-Hsien; Fujita, Singo; Yamoto, Suguru; Hara, Takeshi; Yamagata, Tsuneaki; Watanabe, Masami; Mashima, Kazushi; Dalton Transactions  (2008) 916–923; doi:10.1039/b712901g

data_7003127
_publ_section_title
;
 Stepwise and one-pot syntheses of Ir(iii) complexes with
 imidazolium-based carbene ligands
;
_journal_issue                   7
_journal_name_full               'Dalton Transactions'
_journal_page_first              916
_journal_page_last               923
_journal_paper_doi               10.1039/b712901g
_journal_year                    2008
_chemical_formula_moiety         '(C56, H44, Cl2, Ir2, N8, O4), 2.0(C H2 Cl2)'
_chemical_formula_sum            'C58 H48 Cl6 Ir2 N8 O4'
_chemical_formula_weight         1518.14
_chemical_name_systematic
;
?
;
_chemical_properties_physical    ' air-stable '
_chemical_temperature_decomposition_gt 553
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 100.2230(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.2338(6)
_cell_length_b                   21.0211(7)
_cell_length_c                   25.5914(7)
_cell_measurement_reflns_used    88758
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.0
_cell_volume                     11241.6(6)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'teXan (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997) and modified'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Maria et al., 2005)'
_diffrn_ambient_temperature      120(1)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_details
;
RAPID: Eulerian 3-circle
;
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_collimation    ' 0.5 mm double pinhole '
_diffrn_radiation_detector       'imaging plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.2027
_diffrn_reflns_av_sigmaI/netI    0.1069
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            241575
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.99
_diffrn_source_current           40
_diffrn_source_power             50
_exptl_absorpt_coefficient_mu    5.071
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_correction_T_min  0.221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, H. (1995), ABSCOR: Program for Absorption
Correction, Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            ' platelet '
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ' yellow '
_exptl_crystal_F_000             5920
_exptl_crystal_preparation
'mounted on the CryoLoop with mineral oil and placed in N2 stream at 120(1) K'
_exptl_crystal_recrystallization_method
'Crystallized from a solution of CH2Cl2/hexane at ambient temperature under Ar'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.703
_refine_diff_density_min         -2.402
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1405
_refine_ls_number_reflns         25625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0595
_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^)+(0.0644P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1427
_reflns_number_gt                16874
_reflns_number_total             25625
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b712901g.txt
_cod_data_source_block           CCDC656909(compd2b)
_cod_original_sg_symbol_Hall     ' -P 2yn '
_cod_original_sg_symbol_H-M      ' P21/n '
_cod_database_code               7003127