Pentacyclic Ladder-Heteraborin Emitters Exhibiting High-Efficiency Blue Thermally Activated Delayed Fluorescence with an Ultrashort Emission Lifetime
Agou, Tomohiro; Matsuo, Kyohei; Kawano, Rei; Park, In Seob; Hosoya, Takaaki; Fukumoto, Hiroki; Kubota, Toshio; Mizuhata, Yoshiyuki; Tokitoh, Norihiro; Yasuda, Takuma; ACS Materials Letters  (2019) 28–; doi:10.1021/acsmaterialslett.9b00433

data_4517290
_publ_section_title
;
 Pentacyclic Ladder-Heteraborin Emitters Exhibiting High-Efficiency Blue
 Thermally Activated Delayed Fluorescence with an Ultrashort Emission
 Lifetime
;
_journal_name_full               'ACS Materials Letters'
_journal_page_first              28
_journal_paper_doi               10.1021/acsmaterialslett.9b00433
_journal_year                    2019
_chemical_formula_moiety         'C64 H71 B2 N O2, 3 (C H Cl3)'
_chemical_formula_sum            'C67 H74 B2 Cl9 N O2'
_chemical_formula_weight         1265.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-06-21 deposited with the CCDC.	2019-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.291(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8786(14)
_cell_length_b                   10.1453(6)
_cell_length_c                   32.4284(19)
_cell_measurement_reflns_used    8128
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.029
_cell_measurement_theta_min      2.21
_cell_volume                     6625.8(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'Rigaku CrystalClear-SM Expert 2.1'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Yadokari-XG 2016'
_computing_publication_material  'Yadokari-XG 2016'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  ccd
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1054
_diffrn_reflns_av_unetI/netI     0.0931
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            49235
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         1.847
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.424
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.65969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       block
_exptl_crystal_F_000             2648
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: CHCl3'
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         12344
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1264
_refine_ls_R_factor_gt           0.0729
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0967P)^2^+5.6306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1804
_refine_ls_wR_factor_ref         0.2251
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7422
_reflns_number_total             12344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tz9b00433_si_002.cif
_cod_data_source_block           MCz-BOBO
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4517290
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.845
_shelx_estimated_absorpt_t_max   0.931
_oxdiff_exptl_absorpt_empirical_full_min 0.808
_oxdiff_exptl_absorpt_empirical_full_max 1.355
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              9260
_shelx_hkl_checksum              82433