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_7129552
_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         'C31 H18 N2'
_chemical_formula_sum            'C31 H18 N2'
_chemical_formula_weight         418.47
_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     direct
_audit_creation_date             2020-10-12
_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                73.340(5)
_cell_angle_beta                 87.044(4)
_cell_angle_gamma                72.220(5)
_cell_formula_units_Z            2
_cell_length_a                   8.2871(4)
_cell_length_b                   9.5533(5)
_cell_length_c                   14.9700(8)
_cell_measurement_reflns_used    3706
_cell_measurement_temperature    292.8(8)
_cell_measurement_theta_max      71.2530
_cell_measurement_theta_min      5.0630
_cell_volume                     1080.34(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      292.8(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.970
_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   -106.00 -13.00   1.00    1.82    --  -35.23 -38.00  30.00   93
  2  \w    -57.00  35.00   1.00    1.82    --  -35.23  38.00-150.00   92
  3  \w     23.00  90.00   1.00    1.82    --   35.23-125.00-120.00   67
  4  \w     17.00 104.00   1.00    1.82    --   35.23  57.00   0.00   87
  5  \w    -34.00  64.00   1.00    1.82    --   35.23 -77.00  90.00   98
  6  \w     17.00 104.00   1.00    1.82    --   35.23  57.00-120.00   87
  7  \w     23.00  90.00   1.00    1.82    --   35.23-125.00  30.00   67
  8  \w     17.00 104.00   1.00    1.82    --   35.23  57.00 -60.00   87
  9  \w     36.00 113.00   1.00    7.28    --  106.90-111.00-150.00   77
 10  \w     61.00 178.00   1.00    7.28    --  106.90  15.00-180.00  117
 11  \w     81.00 178.00   1.00    7.28    --  106.90  30.00  60.00   97
 12  \w     87.00 177.00   1.00    7.28    --  106.90  45.00 -30.00   90
 13  \w    100.00 178.00   1.00    7.28    --  106.90 111.00-120.00   78
 14  \w     37.00 127.00   1.00    7.28    --  106.90 -45.00-120.00   90
 15  \w     35.00 133.00   1.00    7.28    --  106.90 -30.00 150.00   98
 16  \w     37.00 110.00   1.00    7.28    --  106.90 -94.00 -90.00   73
 17  \w     37.00 110.00   1.00    7.28    --  106.90 -94.00  60.00   73
 18  \w     37.00 110.00   1.00    7.28    --  106.90 -94.00   0.00   73
 19  \w     61.00 178.00   1.00    7.28    --  106.90  15.00-180.00  117
 20  \w     37.00 127.00   1.00    7.28    --  106.90 -45.00 -30.00   90
 21  \w     37.00 110.00   1.00    7.28    --  106.90 -94.00-120.00   73
 22  \w     17.00 104.00   1.00    1.82    --   35.23  57.00 150.00   87
 23  \w    -33.00 -21.00   1.00    1.82    --   35.23 -57.00   0.00   12
;
_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      0.1149156000
_diffrn_orient_matrix_UB_12      -0.0951843000
_diffrn_orient_matrix_UB_13      -0.0594421000
_diffrn_orient_matrix_UB_21      0.0135054000
_diffrn_orient_matrix_UB_22      -0.1480197000
_diffrn_orient_matrix_UB_23      0.0791916000
_diffrn_orient_matrix_UB_31      -0.1574270000
_diffrn_orient_matrix_UB_32      -0.0155885000
_diffrn_orient_matrix_UB_33      -0.0418590000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9414
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.544
_diffrn_reflns_theta_min         5.072
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48680
_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    1.286
_exptl_crystal_description       block
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0644
_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^)+(0.1315P)^2^+0.0284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1739
_refine_ls_wR_factor_ref         0.1916
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3359
_reflns_number_total             4092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06705b2.cif
_cod_data_source_block           zhx-4054
_cod_original_cell_volume        1080.34(10)
_cod_database_code               7129552
_reflns_odcompleteness_completeness 99.30
_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:
 C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G), C00I(H00I), C00K(H00K),
 C00L(H00L), C00M(H00M), C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R),
 C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X)
;
_shelx_res_checksum              50923
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2020-10-12
_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 1.831
_oxdiff_exptl_absorpt_empirical_full_min 0.725