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_1571718
_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 H42 B N3'
_chemical_formula_sum            'C48 H42 B N3'
_chemical_formula_weight         671.65
_chemical_name_systematic        TTABN
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-10
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2024-04-09 deposited with the CCDC.	2024-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.7230(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.7232(2)
_cell_length_b                   9.88890(10)
_cell_length_c                   51.6585(6)
_cell_measurement_reflns_used    25541
_cell_measurement_temperature    99.98(12)
_cell_measurement_theta_max      73.0580
_cell_measurement_theta_min      2.9930
_cell_volume                     7495.74(15)
_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      99.98(12)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     24.00  64.00   0.50    3.08    --   61.89 -95.00  30.00   80
  2  \w     24.00  70.00   0.50    3.08    --   61.89 -95.00   0.00   92
  3  \w     24.00  64.00   0.50    3.08    --   61.89 -95.00-150.00   80
  4  \w     24.00  67.00   0.50    3.08    --   61.89 -95.00 -60.00   86
  5  \w     57.00  99.00   0.50    3.08    --   61.89   0.00 -30.00   84
  6  \w     44.00  69.00   0.50    3.08    --   61.89 -95.00  90.00   50
  7  \w     27.00  64.00   0.50    3.08    --   61.89 -95.00-120.00   74
  8  \w     24.00  64.00   0.50    3.08    --   61.89 -95.00 120.00   80
  9  \w     32.00  58.00   0.50    3.08    --   61.89 -95.00-180.00   52
 10  \w    -95.00 -36.00   0.50    3.08    --  -64.95   0.00 -90.00  118
 11  \w    -70.00 -45.00   0.50    3.08    --  -64.95 -15.00  30.00   50
 12  \w   -105.00 -74.00   0.50    3.08    --  -64.95 -15.00  30.00   62
 13  \w     52.00  82.00   0.50    3.08    --   73.73 -95.00-150.00   60
 14  \w     37.00  77.00   0.50    3.08    --   74.76-125.00 150.00   80
 15  \w     57.00  82.00   0.50    3.08    --   74.76 -95.00 120.00   50
 16  \w     37.00  77.00   0.50    3.08    --   74.76 -95.00-120.00   80
 17  \w     36.00  98.00   0.50    3.08    --   74.76-125.00  30.00  124
 18  \w     38.00  64.00   0.50    3.08    --   74.76 -95.00 -90.00   52
 19  \w     56.00  81.00   0.50    3.08    --   74.76 -95.00-180.00   50
 20  \w     39.00  64.00   0.50    3.08    --   74.76-125.00 -60.00   50
 21  \w   -120.00 -78.00   0.50    3.08    --  -77.70-125.00 -60.00   84
 22  \w   -117.00 -75.00   0.50    3.08    --  -77.70-125.00-120.00   84
 23  \w   -118.00 -92.00   0.50    3.08    --  -77.70-125.00 150.00   52
 24  \w   -102.00 -75.00   0.50    3.08    --  -77.70-125.00 -30.00   54
 25  \w   -115.00 -79.00   0.50    3.08    --  -77.70   0.00  90.00   72
;
_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      -0.0518159000
_diffrn_orient_matrix_UB_12      0.1353940000
_diffrn_orient_matrix_UB_13      -0.0020107000
_diffrn_orient_matrix_UB_21      0.0451659000
_diffrn_orient_matrix_UB_22      0.0420794000
_diffrn_orient_matrix_UB_23      0.0267596000
_diffrn_orient_matrix_UB_31      0.0793429000
_diffrn_orient_matrix_UB_32      0.0645390000
_diffrn_orient_matrix_UB_33      -0.0132564000
_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  0.0282
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            54420
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.075
_diffrn_reflns_theta_max         67.075
_diffrn_reflns_theta_min         3.012
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87563
_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    1.190
_exptl_crystal_description       plate
_exptl_crystal_F_000             2848
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method Sublimation
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.00057(4)
_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   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     950
_refine_ls_number_reflns         13332
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0506P)^2^+6.8119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11515
_reflns_number_total             13332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02351j2.cif
_cod_data_source_block           230312lt_auto
_cod_depositor_comments
;
Adding full bibliography for 1571718--1571719.cif.

2025-06-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C96 H84 B2 N6'
_cod_original_formula_weight         1343.31
_cod_original_formula_moiety         '2(C48 H42 B N3)'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        7495.75(15)
_cod_database_code               1571718
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.959
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C9(H9), C11(H11), C12(H12), C17(H17), C18(H18), C20(H20),
 C21(H21), C23(H23), C24(H24), C26(H26), C27(H27), C31(H31), C32(H32), C34(H34),
  C35(H35), C39(H39), C40(H40), C42(H42), C45(H45), C46(H46), C48(H48),
 C49(H49), C54(H54), C56(H56), C61(H61), C63(H63), C64(H64), C69(H69), C70(H70),
  C72(H72), C73(H73), C75(H75), C76(H76), C78(H78), C79(H79), C83(H83),
 C84(H84), C86(H86), C87(H87), C91(H91), C93(H93), C94(H94), C97(H97), C98(H98),
  C100(H100), C101(H101)
2.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C36(H36A,H36B,H36C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C80(H80A,H80B,H80C), C81(H81A,
 H81B,H81C), C88(H88A,H88B,H88C), C102(H10A,H10B,H10C), C103(H10D,H10E,H10F),
 C104(H10G,H10H,H10I)
;
_shelx_res_checksum              59120
_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 1.248
_oxdiff_exptl_absorpt_empirical_full_min 0.863