Novel oxacalix[2]arene[2]triazines with thermally activated delayed fluorescence and aggregation-induced emission properties.
Wang, Yin-Feng; Lu, Hai-Yan; Shen, Yi-Fan; Li, Meng; Chen, Chuan-Feng; Chemical communications (Cambridge, England) 55 (2019) 9559–9562; doi:10.1039/c9cc04995a

data_7125389
_publ_section_title
;
 Novel oxacalix[2]arene[2]triazines with thermally activated delayed
 fluorescence and aggregation-induced emission properties.
;
_journal_issue                   64
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9559
_journal_page_last               9562
_journal_paper_doi               10.1039/c9cc04995a
_journal_volume                  55
_journal_year                    2019
_chemical_formula_moiety         'C36 H28 N4 O2'
_chemical_formula_sum            'C36 H28 N4 O2'
_chemical_formula_weight         548.62
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-03-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-12 deposited with the CCDC.	2019-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.45750(10)
_cell_length_b                   10.69620(10)
_cell_length_c                   27.0458(2)
_cell_measurement_reflns_used    22436
_cell_measurement_temperature    170.01(10)
_cell_measurement_theta_max      75.2760
_cell_measurement_theta_min      3.8830
_cell_volume                     3314.51(5)
_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      170.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.953
_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    -60.00  25.00   0.50    0.05    --  -47.20  46.00-128.00  170
  2  \w   -120.00 -34.00   0.50    0.05    --  -47.20 -46.00  81.00  172
  3  \w     35.00 120.00   0.50    0.05    --   47.20  46.00-128.00  170
  4  \w    -24.00  60.00   0.50    0.05    --   47.20 -46.00  81.00  168
  5  \w   -112.00 -26.00   0.50    0.08    --  -99.00  46.00-128.00  172
  6  \w   -168.00 -86.00   0.50    0.08    --  -99.00 -46.00  81.00  164
  7  \w     31.00 116.00   0.50    0.08    --  103.25 -46.00  81.00  170
  8  \w     91.00 169.00   0.50    0.08    --  103.25  46.00-128.00  156
  9  \w   -120.00 -71.00   0.50    0.05    --  -47.20-125.00-180.00   98
 10  \w     16.00  95.00   0.50    0.05    --   47.20-125.00 -60.00  158
 11  \w   -113.00 -24.00   0.50    0.08    --  -99.00  15.00  90.00  178
 12  \w   -112.00 -24.00   0.50    0.08    --  -99.00  30.00  30.00  176
 13  \w   -115.00 -26.00   0.50    0.08    --  -99.00  61.00 120.00  178
 14  \w   -168.00 -90.00   0.50    0.08    --  -99.00 -30.00 -30.00  156
 15  \w   -160.00 -86.00   0.50    0.08    --  -99.00 -45.00 120.00  148
 16  \w   -112.00 -45.00   0.50    0.08    --  -99.00  45.00  60.00  134
 17  \w     92.00 158.00   0.50    0.08    --  103.25  15.00  30.00  132
;
_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      0.0701978000
_diffrn_orient_matrix_UB_12      0.0553368000
_diffrn_orient_matrix_UB_13      -0.0433988000
_diffrn_orient_matrix_UB_21      -0.0300799000
_diffrn_orient_matrix_UB_22      0.1329845000
_diffrn_orient_matrix_UB_23      0.0177794000
_diffrn_orient_matrix_UB_31      0.1106477000
_diffrn_orient_matrix_UB_32      0.0011203000
_diffrn_orient_matrix_UB_33      0.0323276000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0098
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            30875
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.336
_diffrn_reflns_theta_min         4.445
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64137
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.355
_exptl_crystal_size_mid          0.345
_exptl_crystal_size_min          0.324
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.184
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         3289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0648P)^2^+0.8321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1217
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3090
_reflns_number_total             3289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04995a2.cif
_cod_data_source_block           tx401
_cod_database_code               7125389
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         CHNO
_reflns_odcompleteness_completeness 99.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_shelx_res_checksum              61309
_shelx_fab_checksum              29661
_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 1.318
_oxdiff_exptl_absorpt_empirical_full_min 0.725