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_7003128
_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_iupac          ' [Ir (C13 H9 N2)3] '
_chemical_formula_moiety         'Ir, 3(C13 H9 N2)'
_chemical_formula_structural     ' (C13 H9 N2)3 Ir '
_chemical_formula_sum            'C39 H27 Ir N6'
_chemical_formula_weight         771.87
_chemical_name_common
;
racemic-mer-tris(kappa$2!C3,C2'-2-phenyl-pyrido(1,2-c)
imidazo-3-ylidene)iridium(iii)
;
_chemical_name_systematic
; racemic-mer-tris(\k^2^C3,C2'-2-phenyl-pyrido[1,2-c]
imidazo-3-ylidene)iridium(III)
;
_chemical_properties_physical    ' emission luminescence '
_chemical_temperature_decomposition_gt 509
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      88
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             ' 2006-02-24T19:18:14 '
_audit_update_record             ' 2006-04-19T15:24:35 '
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   19.109(2)
_cell_length_b                   19.109(2)
_cell_length_c                   35.200(4)
_cell_measurement_reflns_used    69903
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.02
_cell_volume                     12853(2)
_computing_cell_refinement       'Rigaku/RAPID Diffractometer Control'
_computing_data_collection       'Rigaku/RAPID Diffractometer Control'
_computing_data_reduction        'teXsan: PROCESS (MSC)'
_computing_structure_solution    DIRDIF-99
_diffrn_ambient_temperature      120(2)
_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    ' 0.8 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  0.0914
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            123986
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.02
_diffrn_source_current           40
_diffrn_source_power             50
_exptl_absorpt_coefficient_mu    4.193
_exptl_absorpt_correction_T_max  0.729
_exptl_absorpt_correction_T_min  0.239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). ABSCOR - Program for Absorption Correction, Rigaku
Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            ' yellow '
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ' needle '
_exptl_crystal_F_000             6080
_exptl_crystal_preparation
'mounted on the CryoLoop with mineral oil and placed in N2 stream at 120(2) K'
_exptl_crystal_recrystallization_method
'crystallized from a solution of CHCl3/hexsan at ambient temperature'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.151
_refine_diff_density_min         -2.679
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         9323
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.1394
_refine_ls_R_factor_gt           0.1137
_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^)+(0.0129P)^2^+624.0211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2202
_refine_ls_wR_factor_ref         0.2301
_reflns_number_gt                7082
_reflns_number_total             9323
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b712901g.txt
_cod_data_source_block           CCDC656910(mer-3a)
_cod_original_cell_volume        12853(3)
_cod_original_sg_symbol_Hall     ' -I 4ad '
_cod_original_sg_symbol_H-M      ' I41/a '
_cod_database_code               7003128