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_4344981
_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            'C48 H40 Br2 Ir2 N4'
_chemical_formula_weight         1217.06
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.241(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6206(6)
_cell_length_b                   14.8110(7)
_cell_length_c                   25.0132(13)
_cell_measurement_reflns_used    8759
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.45
_cell_volume                     4279.6(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0746
_diffrn_reflns_av_sigmaI/netI    0.0823
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            25592
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    8.118
_exptl_absorpt_correction_T_max  0.197
_exptl_absorpt_correction_T_min  0.055
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.889
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.898
_refine_diff_density_min         -2.885
_refine_diff_density_rms         0.288
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         7525
_refine_ls_number_restraints     336
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_gt           0.0650
_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^)+(0.0004P)^2^+185.8601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1570
_reflns_number_gt                5375
_reflns_number_total             7525
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic6b02270_si_002.cif
_cod_data_source_block           fkn1_p21n
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      P2(1)/n
_cod_database_code               4344981