Efficient Synthesis of Tris-Heteroleptic Iridium(III) Complexes Based on the Zn(2+)-Promoted Degradation of Tris-Cyclometalated Iridium(III) Complexes and Their Photophysical Properties.
Tamura, Yuichi; Hisamatsu, Yosuke; Kumar, Sarvendra; Itoh, Taiki; Sato, Kyouhei; Kuroda, Reiko; Aoki, Shin; Inorganic chemistry 56 (2017) 812–833; doi:10.1021/acs.inorgchem.6b02270

data_4344980
_publ_section_title
;
 Efficient Synthesis of Tris-Heteroleptic Iridium(III) Complexes Based on
 the Zn(2+)-Promoted Degradation of Tris-Cyclometalated Iridium(III)
 Complexes and Their Photophysical Properties.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              812
_journal_page_last               833
_journal_paper_doi               10.1021/acs.inorgchem.6b02270
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C35 H26 F2 Ir N3'
_chemical_formula_sum            'C35 H26 F2 Ir N3'
_chemical_formula_weight         718.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.710(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.105(16)
_cell_length_b                   9.227(4)
_cell_length_c                   17.928(8)
_cell_measurement_reflns_used    6116
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.29
_cell_volume                     5561(4)
_computing_cell_refinement       'SMART V5.625 (Bruker, 2000)'
_computing_data_collection       'SMART V5.625 (Bruker, 2000)'
_computing_data_reduction        'SAINT v6.28A (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL V6.10 (Bruker, 2000)'
_computing_publication_material  'SHELXTL V6.10 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16326
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    4.845
_exptl_absorpt_correction_T_max  0.8683
_exptl_absorpt_correction_T_min  0.2744
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS v.2.03 (Bruker,2001)'
_exptl_crystal_colour            'yellowish green'
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.643
_refine_diff_density_min         -1.801
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         6249
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0428P)^2^+49.8838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1094
_reflns_number_gt                5437
_reflns_number_total             6249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02270_si_003.cif
_cod_data_source_block           yt3_2
_cod_depositor_comments
'Adding full bibliography for 4344979--4344983.cif.'
_cod_original_cell_volume        5561(5)
_cod_original_sg_symbol_H-M      C12/c1
_cod_database_code               4344980