An ultralong room-temperature phosphorescent material based on the combination of small singlet-triplet splitting energy and H-aggregation.
Zhang, Liang; Li, Meng; Gao, Qing-Yu; Chen, Chuan-Feng; Chemical communications (Cambridge, England) 56 (2020) 4296–4299; doi:10.1039/c9cc09636a

data_7126183
_publ_section_title
;
 An ultralong room-temperature phosphorescent material based on the
 combination of small singlet-triplet splitting energy and H-aggregation.
;
_journal_issue                   31
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4296
_journal_page_last               4299
_journal_paper_doi               10.1039/c9cc09636a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C H2 Cl2, C38 H23 N3 O2'
_chemical_formula_sum            'C39 H25 Cl2 N3 O2'
_chemical_formula_weight         638.52
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-29 deposited with the CCDC.	2020-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                91.7300(10)
_cell_angle_beta                 103.5750(10)
_cell_angle_gamma                110.2320(10)
_cell_formula_units_Z            2
_cell_length_a                   9.44150(10)
_cell_length_b                   11.5767(2)
_cell_length_c                   15.2148(2)
_cell_measurement_reflns_used    23442
_cell_measurement_temperature    170.00(11)
_cell_measurement_theta_max      75.3140
_cell_measurement_theta_min      4.0720
_cell_volume                     1505.45(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.964
_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    -85.00   4.00   0.50    0.30    --  -47.20 107.00  15.00  178
  2  \w      2.00  85.00   0.50    0.30    --   47.20-107.00 -81.00  166
  3  \w   -168.00 -80.00   0.50    0.80    --  -99.00-107.00 -81.00  176
  4  \w   -111.00 -26.00   0.50    0.80    --  -99.00 107.00  15.00  170
  5  \w     87.00 169.00   0.50    0.80    --  103.25 107.00  15.00  164
  6  \w     31.00 111.00   0.50    0.80    --  103.25-107.00 -81.00  160
  7  \w    -62.00  25.00   0.50    0.30    --  -47.20  57.00 120.00  174
  8  \w   -120.00 -71.00   0.50    0.30    --  -47.20-125.00   0.00   98
  9  \w   -120.00 -71.00   0.50    0.30    --  -47.20-125.00  60.00   98
 10  \w    -24.00  62.00   0.50    0.30    --   47.20 -57.00 -90.00  172
 11  \w     25.00 120.00   0.50    0.30    --   47.20  77.00  30.00  190
 12  \w   -168.00 -81.00   0.50    0.80    --  -99.00 -94.00-150.00  174
 13  \w   -115.00 -26.00   0.50    0.80    --  -99.00  61.00  90.00  178
 14  \w   -168.00 -82.00   0.50    0.80    --  -99.00 -61.00 -30.00  172
 15  \w   -168.00 -86.00   0.50    0.80    --  -99.00 -45.00 -60.00  164
 16  \w     31.00 117.00   0.50    0.80    --  103.25-125.00 -90.00  172
 17  \w     31.00 126.00   0.50    0.80    --  103.25 -77.00 -90.00  190
 18  \w     31.00 109.00   0.50    0.80    --  103.25 -94.00  30.00  156
 19  \w     91.00 169.00   0.50    0.80    --  103.25  45.00-180.00  156
 20  \w     31.00 109.00   0.50    0.80    --  103.25 -94.00 120.00  156
 21  \w     32.00 116.00   0.50    0.80    --  103.25 -45.00  60.00  168
 22  \w     77.00 169.00   0.50    0.80    --  103.25 125.00 -30.00  184
 23  \w     28.00 117.00   0.50    0.80    --  103.25 -15.00 -30.00  178
 24  \w     31.00 120.00   0.50    0.80    --  103.25 -61.00  90.00  178
 25  \w     25.00 120.00   0.50    0.30    --   47.20  77.00 -90.00  190
 26  \w     25.00 120.00   0.50    0.30    --   47.20  77.00-180.00  190
 27  \w     32.00 120.00   0.50    0.30    --   47.20  57.00   0.00  176
 28  \w     32.00 120.00   0.50    0.30    --   47.20  57.00 120.00  176
 29  \w     25.00 120.00   0.50    0.30    --   47.20  77.00-120.00  190
 30  \w     25.00 120.00   0.50    0.30    --   47.20  77.00   0.00  190
 31  \w     32.00 120.00   0.50    0.30    --   47.20  57.00 150.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0747933000
_diffrn_orient_matrix_UB_12      -0.0474755000
_diffrn_orient_matrix_UB_13      0.0854994000
_diffrn_orient_matrix_UB_21      -0.0447919000
_diffrn_orient_matrix_UB_22      -0.1267484000
_diffrn_orient_matrix_UB_23      -0.0554997000
_diffrn_orient_matrix_UB_31      0.1576652000
_diffrn_orient_matrix_UB_32      0.0458192000
_diffrn_orient_matrix_UB_33      -0.0249796000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25723
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.374
_diffrn_reflns_theta_min         4.101
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.276
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.423
_exptl_crystal_size_mid          0.321
_exptl_crystal_size_min          0.311
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+0.8134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1120
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5857
_reflns_number_total             6008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09636a2.cif
_cod_data_source_block           tx198
_cod_depositor_comments
'Adding full bibliography for 7126183--7126184.cif.'
_cod_database_code               7126183
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         CHNO
_reflns_odcompleteness_completeness 99.70
_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
2.a Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C14(H14), C16(H16),
 C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25), C28(H28),
  C29(H29), C30(H30), C31(H31), C34(H34), C35(H35), C36(H36), C37(H37)
;
_shelx_res_checksum              35066
_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 3.589
_oxdiff_exptl_absorpt_empirical_full_min 0.535