A novel thermally activated delayed fluorescence macrocycle
Zhou, He-Ye; Zhang, Da-Wei; Han, Xiao-Ni; Han, Ying; Chen, Chuan-Feng; Chemical Communications  (2022) –; doi:10.1039/D2CC04618K

data_7130858
_publ_section_title
;
 A novel thermally activated delayed fluorescence macrocycle
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04618K
_journal_year                    2022
_chemical_formula_moiety         'C37 H28 N4, C2 H4'
_chemical_formula_sum            'C37 H28 N4'
_chemical_formula_weight         528.63
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-06-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-07-26 deposited with the CCDC.	2022-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   24.5261(4)
_cell_length_b                   24.5261(4)
_cell_length_c                   17.8430(2)
_cell_measurement_reflns_used    16297
_cell_measurement_temperature    169.99(13)
_cell_measurement_theta_max      74.4870
_cell_measurement_theta_min      2.2530
_cell_volume                     9295.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.956
_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    -25.00  47.00   0.50    0.73    --   47.57 -38.00-120.00  144
  2  \w     48.00 111.00   0.50    7.94    --  103.25-125.00  30.00  126
  3  \w    144.00 169.00   0.50    7.94    --  103.25 120.00 -91.00   50
  4  \w    138.00 167.00   0.50    7.94    --  103.25 125.00 -60.00   58
  5  \w     90.00 131.00   0.50    7.94    --  103.25 120.00 -91.00   82
  6  \w     85.00 133.00   0.50    7.94    --  103.25 125.00 -60.00   96
  7  \w    -65.00 -32.00   0.50    7.94    --  -99.00  61.00  30.00   66
  8  \w    -55.00 -26.00   0.50    7.94    --  -99.00  61.00 -60.00   58
  9  \w    -66.00 -40.00   0.50    7.94    --  -99.00  61.00-180.00   52
 10  \w   -109.00 -33.00   0.50    7.94    --  -99.00 118.00 -71.00  152
 11  \w   -165.00 -88.00   0.50    7.94    --  -99.00 -77.00-150.00  154
 12  \w   -119.00 -94.00   0.50    0.73    --  -47.57-125.00 -30.00   50
 13  \w   -116.00 -68.00   0.50    0.73    --  -47.57-156.00  88.00   96
;
_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      -0.0499771000
_diffrn_orient_matrix_UB_12      -0.0704783000
_diffrn_orient_matrix_UB_13      0.0025068000
_diffrn_orient_matrix_UB_21      -0.0519103000
_diffrn_orient_matrix_UB_22      0.0171419000
_diffrn_orient_matrix_UB_23      0.0112260000
_diffrn_orient_matrix_UB_31      -0.0081298000
_diffrn_orient_matrix_UB_32      0.0001420000
_diffrn_orient_matrix_UB_33      -0.0856002000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37936
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.114
_diffrn_reflns_theta_min         2.476
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    0.567
_exptl_crystal_description       plate
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.161
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.342
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         12246
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.342
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0971
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3003
_refine_ls_wR_factor_ref         0.3156
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9616
_reflns_number_total             12246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04618k2.cif
_cod_data_source_block           tx5870_sq
_cod_original_cell_volume        9295.1(3)
_cod_database_code               7130858
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHON
_reflns_odcompleteness_completeness 99.74
_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.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C0AA(H0AA,H0AB), C1AA(H1AA,H1AB)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C3(H3), C12(H12), C19(H19), C13(H13), C20(H20), C4(H4), C6(H6),
 C16(H16), C17(H17), C32(H32), C28(H28), C31(H31), C29(H29), C30(H30), C34(H34),
  C38(H38), C35(H35), C36(H36), C37(H37)
2.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              77095
_shelx_hkl_checksum              38060
_shelx_fab_checksum              92379
_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 2.528
_oxdiff_exptl_absorpt_empirical_full_min 0.467