An umpolung strategy for rapid access to thermally activated delayed fluorescence (TADF) materials based on phenazine
Zhang, Huaxing; Guo, Qiang; Cheng, Hu; Ran, Chunhao; Wu, Di; Lan, Jingbo; Chemical Communications  (2022) –; doi:10.1039/D1CC06705B

data_7129559
_publ_section_title
;
 An umpolung strategy for rapid access to thermally activated delayed
 fluorescence (TADF) materials based on phenazine
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06705B
_journal_year                    2022
_chemical_formula_moiety         'C12 H7 N3 O2'
_chemical_formula_sum            'C12 H7 N3 O2'
_chemical_formula_weight         225.21
_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     direct
_audit_creation_date             2020-09-09
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2020-10-30 deposited with the CCDC.	2021-12-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.235(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8370(4)
_cell_length_b                   22.4145(11)
_cell_length_c                   7.1605(4)
_cell_measurement_reflns_used    1588
_cell_measurement_temperature    296.4(8)
_cell_measurement_theta_max      70.4490
_cell_measurement_theta_min      5.7320
_cell_volume                     1000.62(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (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      air
_diffrn_ambient_temperature      296.4(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_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    -53.00  33.00   1.00    4.49    --  -34.98  57.00  30.00   86
  2  \w    -34.00  64.00   1.00    4.49    --   34.98 -77.00-150.00   98
  3  \w     16.00 103.00   1.00    4.49    --   34.98  57.00  60.00   87
  4  \w    -34.00  64.00   1.00    4.49    --   34.98 -77.00 -60.00   98
  5  \w      1.00  75.00   1.00    4.49    --   34.98 -99.00  90.00   74
  6  \w    100.00 178.00   1.00   17.97    --  106.90 111.00-120.00   78
  7  \w     78.00 176.00   1.00   17.97    --  106.90  77.00-120.00   98
  8  \w    100.00 178.00   1.00   17.97    --  106.90 111.00 -30.00   78
  9  \w     61.00 178.00   1.00   17.97    --  106.90  15.00 -60.00  117
 10  \w    100.00 178.00   1.00   17.97    --  106.90 111.00 120.00   78
 11  \w     36.00 113.00   1.00   17.97    --  106.90-111.00-180.00   77
 12  \w     37.00 110.00   1.00   17.97    --  106.90 -94.00  30.00   73
 13  \w    100.00 178.00   1.00   17.97    --  106.90 111.00   0.00   78
 14  \w   -103.00 -16.00   1.00    4.49    --  -34.98 -57.00-120.00   87
 15  \w     16.00 103.00   1.00    4.49    --   34.98  57.00 150.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0233045000
_diffrn_orient_matrix_UB_12      -0.0668973000
_diffrn_orient_matrix_UB_13      -0.0541163000
_diffrn_orient_matrix_UB_21      0.1568401000
_diffrn_orient_matrix_UB_22      0.0070730000
_diffrn_orient_matrix_UB_23      -0.1034164000
_diffrn_orient_matrix_UB_31      0.1895876000
_diffrn_orient_matrix_UB_32      -0.0140289000
_diffrn_orient_matrix_UB_33      0.2049786000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5414
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.269
_diffrn_reflns_theta_min         3.944
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       plate
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         1917
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0702
_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^)+(0.1413P)^2^+0.1300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2204
_refine_ls_wR_factor_ref         0.2332
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1510
_reflns_number_total             1917
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06705b2.cif
_cod_data_source_block           zhx-no2
_cod_original_cell_volume        1000.63(10)
_cod_database_code               7129559
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00C(H00C), C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G),
 C00H(H00H)
;
_shelx_res_checksum              56061
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2020-09-08
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.623
_oxdiff_exptl_absorpt_empirical_full_min 0.520