Elevating the upconversion performance of a multiple resonance thermally activated delayed fluorescence emitter via an embedded azepine approach
Chen, Yi-Kuan; Lei, Jian; Wu, Tien-Lin; Chemical Science 15 (2024) 10146–10154; doi:10.1039/D4SC02351J

data_1571719
_publ_section_title
;
 Elevating the upconversion performance of a multiple resonance thermally
 activated delayed fluorescence emitter via an embedded azepine approach
;
_journal_issue                   26
_journal_name_full               'Chemical Science'
_journal_page_first              10146
_journal_page_last               10154
_journal_paper_doi               10.1039/D4SC02351J
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C48 H36 B N3'
_chemical_formula_sum            'C48 H36 B N3'
_chemical_formula_weight         665.61
_chemical_name_systematic        TAzBN
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-06
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-04-09 deposited with the CCDC.	2024-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.72780(13)
_cell_length_b                   13.75053(9)
_cell_length_c                   25.09061(16)
_cell_measurement_reflns_used    20916
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.1210
_cell_measurement_theta_min      3.5250
_cell_volume                     7151.28(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -125.00 -41.00   0.50    0.97    --  -75.21 -15.00 -60.00  168
  2  \w   -115.00 -85.00   0.50    0.97    --  -75.21 -15.00  90.00   60
  3  \w    -69.00 -44.00   0.50    0.97    --  -75.21 -15.00  90.00   50
  4  \w     41.00 123.00   0.50    0.97    --   75.83  15.00 -60.00  164
  5  \w     53.00 128.00   0.50    0.97    --   83.87  15.00 -30.00  150
  6  \w    109.00 134.00   0.50    0.97    --   83.87  15.00  30.00   50
  7  \w     52.00  77.00   0.50    0.97    --   83.87  15.00  30.00   50
  8  \w     52.00  80.00   0.50    0.97    --   83.87 -95.00 -90.00   56
  9  \w     23.00  55.00   0.50    0.97    --   69.42-125.00-120.00   64
 10  \w     28.00  53.00   0.50    0.97    --   69.42 -95.00 -90.00   50
 11  \w     22.00  47.00   0.50    0.97    --   56.26 -95.00-120.00   50
 12  \w     34.00  83.00   0.50    0.97    --   75.83 -95.00-180.00   98
 13  \w     14.00  39.00   0.50    0.97    --   56.26 -95.00   0.00   50
 14  \w     33.00  70.00   0.50    0.97    --   75.83 -95.00   0.00   74
 15  \w     36.00  65.00   0.50    0.97    --   75.83 -95.00-120.00   58
 16  \w     33.00  76.00   0.50    0.97    --   75.83 -95.00  30.00   86
 17  \w     41.00  92.00   0.50    0.97    --   83.87 -95.00 -30.00  102
 18  \w     33.00  84.00   0.50    0.97    --   56.26-125.00 120.00  102
 19  \w     21.00  56.00   0.50    0.97    --   56.26 -95.00 150.00   70
 20  \w     35.00  60.00   0.50    0.97    --   75.83 -95.00 150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0474342000
_diffrn_orient_matrix_UB_12      0.0753727000
_diffrn_orient_matrix_UB_13      -0.0230419000
_diffrn_orient_matrix_UB_21      0.0276751000
_diffrn_orient_matrix_UB_22      0.0175187000
_diffrn_orient_matrix_UB_23      0.0561461000
_diffrn_orient_matrix_UB_31      0.0500699000
_diffrn_orient_matrix_UB_32      -0.0810676000
_diffrn_orient_matrix_UB_33      -0.0092236000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            42604
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         3.523
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.548
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.58a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       plate
_exptl_crystal_F_000             2800
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method Sublimation
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.00012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         6377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0573P)^2^+3.8626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1125
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5693
_reflns_number_total             6377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02351j2.cif
_cod_data_source_block           221276lt2_auto
_cod_depositor_comments
'Adding full bibliography for 1571718--1571719.cif.'
_cod_database_code               1571719
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.913
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C30(H30A,H30B), C31(H31A,H31B), C45(H45A,H45B),
 C46(H46A,H46B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C15(H15), C17(H17), C20(H20), C21(H21),
 C22(H22), C25(H25), C26(H26), C27(H27), C28(H28), C33(H33), C34(H34), C35(H35),
  C36(H36), C41(H41), C42(H42), C43(H43), C48(H48), C49(H49), C50(H50), C51(H51)
;
_shelx_res_checksum              47851
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.242
_oxdiff_exptl_absorpt_empirical_full_min 0.837