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_4344983
_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_sum            'C35 H25 Br F2 Ir N3 O1.5'
_chemical_formula_weight         821.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                70.7450(10)
_cell_angle_beta                 86.1520(10)
_cell_angle_gamma                84.7100(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5171(7)
_cell_length_b                   12.9204(9)
_cell_length_c                   13.0846(10)
_cell_measurement_reflns_used    7956
_cell_measurement_temperature    175(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.63
_cell_volume                     1511.32(19)
_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      175(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8662
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    5.787
_exptl_absorpt_correction_T_max  0.4223
_exptl_absorpt_correction_T_min  0.1718
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS v.2.03 (Bruker,2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.171
_refine_diff_density_min         -1.729
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         5992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0545P)^2^+3.7445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0893
_reflns_number_gt                5767
_reflns_number_total             5992
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02270_si_007.cif
_cod_data_source_block           yt11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4344979--4344983.cif.
;
_cod_original_sg_symbol_H-M      'P-1  '
_cod_original_formula_sum        'C35 H25 Br F2 Ir N3 O1.50'
_cod_database_code               4344983