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_7125390
_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         'C60 H44 N8 O4'
_chemical_formula_sum            'C60 H44 N8 O4'
_chemical_formula_weight         941.03
_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     dual
_audit_creation_date             2019-03-14
_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                 101.9258(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.64598(5)
_cell_length_b                   27.23322(15)
_cell_length_c                   18.74004(10)
_cell_measurement_reflns_used    24203
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      75.1960
_cell_measurement_theta_min      2.8990
_cell_volume                     4816.59(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      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.952
_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    -61.00  12.00   0.50    0.20    --  -47.20  54.00  89.00  146
  2  \w     -5.00  37.00   0.50    0.20    --   47.20 -54.00 -54.00   84
  3  \w     38.00  87.00   0.50    0.20    --   47.20  54.00  89.00   98
  4  \w    -70.00 -45.00   0.50    1.00    --  -99.00  54.00  89.00   50
  5  \w   -164.00-105.00   0.50    1.00    --  -99.00 -54.00 -54.00  118
  6  \w    144.00 169.00   0.50    1.00    --  103.25  54.00  89.00   50
  7  \w     92.00 118.00   0.50    1.00    --  103.25  54.00  89.00   52
  8  \w     31.00 117.00   0.50    1.00    --  103.25 -54.00 -54.00  172
  9  \w   -119.00 -72.00   0.50    0.20    --  -47.20-125.00  90.00   94
 10  \w   -100.00 -35.00   0.50    0.20    --  -47.20 -54.00 -54.00  130
 11  \w   -116.00 -91.00   0.50    0.20    --  -47.20-125.00  60.00   50
 12  \w   -146.00 -85.00   0.50    1.00    --  -99.00 -15.00-150.00  122
 13  \w   -167.00-101.00   0.50    1.00    --  -99.00 -45.00 -30.00  132
 14  \w   -112.00 -28.00   0.50    1.00    --  -99.00  30.00 -90.00  168
 15  \w   -160.00 -85.00   0.50    1.00    --  -99.00 -15.00 -30.00  150
 16  \w     32.00  79.00   0.50    1.00    --  103.25 -94.00-180.00   94
 17  \w     91.00 163.00   0.50    1.00    --  103.25  30.00-150.00  144
 18  \w     69.00  95.00   0.50    1.00    --  103.25 -30.00  30.00   52
 19  \w     28.00  53.00   0.50    1.00    --  103.25 -30.00  30.00   50
 20  \w     60.00  95.00   0.50    1.00    --  103.25 -45.00  90.00   70
;
_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      -0.0907458000
_diffrn_orient_matrix_UB_12      -0.0352831000
_diffrn_orient_matrix_UB_13      -0.0548394000
_diffrn_orient_matrix_UB_21      -0.0926609000
_diffrn_orient_matrix_UB_22      -0.0112268000
_diffrn_orient_matrix_UB_23      0.0558357000
_diffrn_orient_matrix_UB_31      -0.0990616000
_diffrn_orient_matrix_UB_32      0.0427851000
_diffrn_orient_matrix_UB_33      -0.0305502000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34940
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.506
_diffrn_reflns_theta_min         2.905
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61164
_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    1.298
_exptl_crystal_description       plate
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.041
_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     653
_refine_ls_number_reflns         9511
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0662P)^2^+2.0275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1355
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8570
_reflns_number_total             9511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04995a2.cif
_cod_data_source_block           tx457_sq
_cod_original_cell_volume        4816.58(5)
_cod_database_code               7125390
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         CHONCl
_reflns_odcompleteness_completeness 99.76
_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. Rigid bond restraints
 C33, C34
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3.a Aromatic/amide H refined with riding coordinates:
 C44(H44), C45(H45), C41(H41), C21(H21), C20(H20), C16(H16), C5(H5), C42(H42),
 C18(H18), C47(H47), C14(H14), C23(H23), C57(H57), C24(H24), C26(H26), C36(H36),
  C35(H35), C15(H15), C48(H48), C34(H34), C50(H50), C7(H7), C54(H54), C33(H33),
 C27(H27), C29(H29), C28(H28), C56(H56), C9(H9), C49(H49), C8(H8), C55(H55)
3.b Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C), C39(H39A,H39B,H39C), C38(H38A,H38B,H38C), C60(H60A,H60B,
 H60C)
;
_shelx_res_checksum              57628
_shelx_fab_checksum              51005
_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 1.344
_oxdiff_exptl_absorpt_empirical_full_min 0.647