Thermally activated delayed fluorescence in a mechanically soft charge-transfer complex: role of the locally excited state.
Kalita, Kalyan Jyoti; Mondal, Saikat; Reddy, C. Malla; Vijayaraghavan, Ratheesh K.; Chemical science 14 (2023) 13870–13878; doi:10.1039/d3sc03267a

data_1570295
_publ_section_title
;
 Thermally activated delayed fluorescence in a mechanically soft
 charge-transfer complex: role of the locally excited state.
;
_journal_issue                   47
_journal_name_full               'Chemical science'
_journal_page_first              13870
_journal_page_last               13878
_journal_paper_doi               10.1039/d3sc03267a
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         '2(C5 H N2), C14 H13 N'
_chemical_formula_sum            'C24 H15 N5'
_chemical_formula_weight         373.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-05-04 deposited with the CCDC.	2023-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.6360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.2576(2)
_cell_length_b                   29.1258(4)
_cell_length_c                   9.46920(10)
_cell_measurement_reflns_used    5505
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      67.9460
_cell_measurement_theta_min      3.4440
_cell_volume                     3924.30(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.984
_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    -37.00  25.00   0.50    3.00    --  -41.33  32.00   0.00  124
  2  \w    -27.00  67.00   0.50    3.00    --   41.33 -72.00  42.00  188
  3  \w     26.00  80.00   0.50    3.00    --   41.33-104.00 -30.00  108
  4  \w     75.00 100.00   0.50    3.00    --   41.33-138.00   0.00   50
  5  \w     44.00 127.00   0.50   18.00    --   96.67-145.00 -90.00  166
  6  \w     36.00  83.00   0.50   18.00    --   96.67 -68.00 -30.00   94
  7  \w     30.00  57.00   0.50   18.00    --   96.67 -50.00   0.00   54
  8  \w     31.00  56.00   0.50   18.00    --   96.67 -50.00 -30.00   50
  9  \w     29.00  54.00   0.50   18.00    --   96.67 -59.00 -60.00   50
 10  \w     28.00  96.00   0.50   18.00    --   96.67 -77.00 -90.00  136
 11  \w     30.00 107.00   0.50   18.00    --   96.67-117.00 -90.00  154
 12  \w     28.00  91.00   0.50   18.00    --   96.67 -72.00  42.00  126
 13  \w     31.00  56.00   0.50   18.00    --   96.67 -50.00 120.00   50
 14  \w     32.00  83.00   0.50   18.00    --   96.67 -68.00  90.00  102
 15  \w     30.00  55.00   0.50   18.00    --   96.67 -50.00 150.00   50
 16  \w     32.00  58.00   0.50   18.00    --   96.67 -59.00 120.00   52
 17  \w     31.00  56.00   0.50   18.00    --   96.67 -50.00  90.00   50
 18  \w     34.00  60.00   0.50   18.00    --   96.67 -59.00  60.00   52
 19  \w     83.00 159.00   0.50   18.00    --   96.67  50.00  90.00  152
 20  \w    106.00 132.00   0.50   18.00    --   96.67  96.00   0.00   52
 21  \w     99.00 164.00   0.50   18.00    --   96.67 117.00  30.00  130
 22  \w    122.00 148.00   0.50   18.00    --   96.67 117.00-120.00   52
 23  \w     16.00 111.00   0.50    3.00    --   41.33  72.00 172.00  190
 24  \w     71.00 163.00   0.50   18.00    --   96.67  72.00 172.00  184
 25  \w     -4.00  22.00   0.50    3.00    --  -41.33  72.00 172.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0324780000
_diffrn_orient_matrix_UB_12      -0.0137117000
_diffrn_orient_matrix_UB_13      -0.1524631000
_diffrn_orient_matrix_UB_21      0.0566203000
_diffrn_orient_matrix_UB_22      0.0402038000
_diffrn_orient_matrix_UB_23      -0.0573509000
_diffrn_orient_matrix_UB_31      0.0863639000
_diffrn_orient_matrix_UB_32      -0.0315209000
_diffrn_orient_matrix_UB_33      -0.0067817000
_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  0.0162
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9209
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.194
_diffrn_reflns_theta_min         3.035
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         3541
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0963P)^2^+0.5007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1420
_refine_ls_wR_factor_ref         0.1497
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2953
_reflns_number_total             3541
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03267a4.cif
_cod_data_source_block           kjk-tcnb_1
_cod_depositor_comments
'Adding full bibliography for 1570291--1570296.cif.'
_cod_database_code               1570295
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N'
_chemical_oxdiff_usercomment     @RT
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.886
_reflns_odcompleteness_completeness 99.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C1(0.5) C3(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C00U(H00A,H00B)
3.b Aromatic/amide H refined with riding coordinates:
 C003(H003), C005(H005), C00C(H00F), C00E(H00G), C00M(H00M), C00N(H00N),
 C00O(H00O), C00Q(H00Q), C2(H2)
3.c Idealised Me refined as rotating group:
 C00V(H00C,H00D,H00E)
;
_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 1.431
_oxdiff_exptl_absorpt_empirical_full_min 0.789