Stable Blue Phosphorescence Iridium(III) Cyclometalated Complexes Prompted by Intramolecular Hydrogen Bond in Ancillary Ligand.
Yi, Seungjun; Kim, Jin-Hyoung; Cho, Yang-Jin; Lee, Jiwon; Choi, Tae-Sup; Cho, Dae Won; Pac, Chyongjin; Han, Won-Sik; Son, Ho-Jin; Kang, Sang Ook; Inorganic chemistry 55 (2016) 3324–3331; doi:10.1021/acs.inorgchem.5b02511

data_4346988
_publ_section_title
;
 Stable Blue Phosphorescence Iridium(III) Cyclometalated Complexes
 Prompted by Intramolecular Hydrogen Bond in Ancillary Ligand.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3324
_journal_page_last               3331
_journal_paper_doi               10.1021/acs.inorgchem.5b02511
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C29 H22 Ir N3 O3'
_chemical_formula_weight         652.54
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.277(4)
_cell_length_b                   24.613(11)
_cell_length_c                   25.517(11)
_cell_measurement_reflns_used    7477
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.404
_cell_measurement_theta_min      2.339
_cell_volume                     5826(4)
_computing_cell_refinement       'SMART (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1999)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1816
_diffrn_reflns_av_unetI/netI     0.1525
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            78096
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.468
_diffrn_reflns_theta_min         1.149
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.614
_exptl_absorpt_correction_T_max  0.874
_exptl_absorpt_correction_T_min  0.439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2543
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.219
_refine_diff_density_min         -1.753
_refine_diff_density_rms         0.167
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.887
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         14543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0521P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1744
_reflns_Friedel_coverage         0.814
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                7787
_reflns_number_total             14543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02511_si_002.cif
_cod_data_source_block           2b
_cod_database_code               4346988
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.607
_shelx_estimated_absorpt_t_max   0.874
_shelx_res_checksum              19231
_shelx_hkl_checksum              13780