Near-Infrared Phosphorescent Iridium(III) Benzonorrole Complexes Possessing Pyridine-based Axial Ligands.
Maurya, Yogesh Kumar; Ishikawa, Takahiro; Kawabe, Yasunori; Ishida, Masatoshi; Toganoh, Motoki; Mori, Shigeki; Yasutake, Yuhsuke; Fukatsu, Susumu; Furuta, Hiroyuki; Inorganic chemistry 55 (2016) 6223–6230; doi:10.1021/acs.inorgchem.6b00853

data_4348016
_publ_section_title
;
 Near-Infrared Phosphorescent Iridium(III) Benzonorrole Complexes
 Possessing Pyridine-based Axial Ligands.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6223
_journal_page_last               6230
_journal_paper_doi               10.1021/acs.inorgchem.6b00853
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C51 H20 F15 Ir N6, C7 H16'
_chemical_formula_sum            'C58 H36 F15 Ir N6'
_chemical_formula_weight         1294.13
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   36.913(10)
_cell_length_b                   36.913(10)
_cell_length_c                   15.452(4)
_cell_measurement_reflns_used    29948
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.46
_cell_measurement_theta_min      1.56
_cell_volume                     21054(10)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.2.1 (Rigaku, 2016)'
_computing_publication_material  'CrystalStructure 4.2.1'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            220790
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.429
_exptl_absorpt_coefficient_mu    2.635
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10208
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.716
_refine_diff_density_min         -1.951
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.219
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         12683
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      1.240
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+368.2935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1524
_refine_ls_wR_factor_ref         0.1540
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12216
_reflns_number_total             12683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00853_si_002.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        21055(13)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4348016
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.693
_shelx_estimated_absorpt_t_max   0.902
_shelx_res_checksum              60278
_shelx_hkl_checksum              10921
_shelx_fab_checksum              65900