Palladium-Catalyzed Direct Arylation of Luminescent Bis-Cyclometalated Iridium(III) Complexes Incorporating C^N- or O^O-Coordinating Thiophene-Based Ligands: an Efficient Method for Color Tuning
Kassem Beydoun; Moussa Zaarour; J. A. Gareth Williams; Thierry Roisnel; Vincent Dorcet; Aurélien Planchat; Abdou Boucekkine; Denis Jacquemin; Henri Doucet; Véronique Guerchais; Inorganic Chemistry 52 (2013) 12416–12428; doi:10.1021/ic401208p

data_4336521
_publ_section_title
;
 Palladium-Catalyzed Direct Arylation of Luminescent Bis-Cyclometalated
 Iridium(III) Complexes Incorporating C^N- or O^O-Coordinating
 Thiophene-Based Ligands: an Efficient Method for Color Tuning
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12416
_journal_page_last               12428
_journal_paper_doi               10.1021/ic401208p
_journal_volume                  52
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C41 H25 Ir N4 O2 S4, C1 H2 Cl2'
_chemical_formula_sum            'C42 H27 Cl2 Ir N4 O2 S4'
_chemical_formula_weight         1011.02
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2012-02-13T17:33:53-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                112.030(2)
_cell_angle_beta                 106.407(3)
_cell_angle_gamma                111.969(3)
_cell_formula_units_Z            2
_cell_length_a                   12.4712(8)
_cell_length_b                   12.6001(7)
_cell_length_c                   16.7180(9)
_cell_measurement_reflns_used    9432
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.55
_cell_measurement_wavelength     0.71073
_cell_volume                     1966.4(2)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
           WinGX publication routines (Farrugia, 1999),
           CRYSCAL (T. Roisnel, local program)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32082
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    3.786
_exptl_absorpt_correction_T_max  0.685
_exptl_absorpt_correction_T_min  0.452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_description       prism
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         8925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.025
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+0.3854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.055
_reflns_number_gt                8264
_reflns_number_total             8925
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401208p_si_002.cif
_cod_data_source_block           K1011
_cod_database_code               4336521