Enhancing corannulene chemiluminescence, electrochemiluminescence and photoluminescence by means of an azabora-helicene to slow down its bowl inversion.
Qin, Xiaoli; Huang, Lin; Zhan, Ziying; Fu, Peng; Wang, Qing; Zhang, Congyang; Huang, Jianhui; Ding, Zhifeng; Chemical science 15 (2024) 9657–9668; doi:10.1039/d4sc01524j

data_1571633
_publ_section_title
;
 Enhancing corannulene chemiluminescence, electrochemiluminescence and
 photoluminescence by means of an azabora-helicene to slow down its bowl
 inversion.
;
_journal_issue                   25
_journal_name_full               'Chemical science'
_journal_page_first              9657
_journal_page_last               9668
_journal_paper_doi               10.1039/d4sc01524j
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C33 H24 B N'
_chemical_formula_sum            'C33 H24 B N'
_chemical_formula_weight         445.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-11-27
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-03-05 deposited with the CCDC.	2024-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.2760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.69340(10)
_cell_length_b                   21.4946(4)
_cell_length_c                   12.5425(2)
_cell_measurement_reflns_used    6902
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.2230
_cell_measurement_theta_min      4.0980
_cell_volume                     2337.18(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.941
_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    -63.00 -38.00   0.50    1.50    --  -46.28 132.00  53.00   50
  2  \w   -102.00 -50.00   0.50    1.50    --  -46.28 137.00-130.00  104
  3  \w     36.00  61.00   0.50    1.50    --   46.28-132.00 -16.00   50
  4  \w     70.00 109.00   0.50    1.50    --   46.28 137.00-130.00   78
  5  \w     76.00 109.00   0.50    1.50    --   46.28 132.00  53.00   66
  6  \w     39.00  64.00   0.50    1.50    --   46.28-137.00 166.00   50
  7  \w   -116.00 -89.00   0.50    6.00    -- -100.00 132.00  53.00   54
  8  \w   -149.00-124.00   0.50    6.00    -- -100.00-132.00 -16.00   50
  9  \w   -147.00-121.00   0.50    6.00    -- -100.00-137.00 166.00   52
 10  \w   -114.00 -30.00   0.50    6.00    -- -100.00 137.00-130.00  168
 11  \w     70.00 155.00   0.50    6.00    --  105.53 137.00-130.00  170
 12  \w     51.00  76.00   0.50    6.00    --  105.53-132.00 -16.00   50
 13  \w     22.00 118.00   0.50    1.50    --   46.28  77.00 150.00  192
 14  \w     -6.00  24.00   0.50    1.50    --   46.28 -19.00-150.00   60
 15  \w    -27.00  11.00   0.50    1.50    --   46.28 -37.00-150.00   76
 16  \w    -71.00 -40.00   0.50    6.00    -- -100.00  61.00-180.00   62
 17  \w   -170.00 -82.00   0.50    6.00    -- -100.00 -61.00   0.00  176
 18  \w    -65.00 -33.00   0.50    6.00    -- -100.00  61.00 -90.00   64
 19  \w    -60.00 -34.00   0.50    6.00    -- -100.00  61.00  90.00   52
 20  \w    -53.00 -28.00   0.50    6.00    -- -100.00  45.00-120.00   50
 21  \w     60.00 103.00   0.50    6.00    --  105.53 -94.00-180.00   86
 22  \w     85.00 174.00   0.50    6.00    --  105.53  15.00-120.00  178
 23  \w     75.00 102.00   0.50    6.00    --  105.53 -94.00-150.00   54
 24  \w     39.00 111.00   0.50    6.00    --  105.53-125.00-150.00  144
 25  \w    125.00 150.00   0.50    6.00    --  105.53  45.00-150.00   50
 26  \w     32.00  67.00   0.50    6.00    --  105.53 -61.00 -60.00   70
 27  \w     79.00 104.00   0.50    6.00    --  105.53 -94.00   0.00   50
 28  \w     93.00 118.00   0.50    6.00    --  105.53  45.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0180320000
_diffrn_orient_matrix_UB_12      0.0679351000
_diffrn_orient_matrix_UB_13      0.0380855000
_diffrn_orient_matrix_UB_21      -0.0610101000
_diffrn_orient_matrix_UB_22      0.0228309000
_diffrn_orient_matrix_UB_23      -0.1116761000
_diffrn_orient_matrix_UB_31      -0.1659142000
_diffrn_orient_matrix_UB_32      -0.0010287000
_diffrn_orient_matrix_UB_33      0.0353475000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16092
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.475
_diffrn_reflns_theta_min         4.089
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.63a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'fluorescent light yellow'
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4554
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0542
_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^)+(0.1212P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.1709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3485
_reflns_number_total             4554
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01524j2.cif
_cod_data_source_block           hl-cor-11b-2ben_auto
_cod_depositor_comments          'Adding full bibliography for 1571633.cif.'
_cod_database_code               1571633
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.947
_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:
 C6(H6A,H6B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C43(H43), C20(H20), C24(H24), C50(H50), C48(H48), C56(H56),
 C46(H46), C40(H40), C44(H44), C7(H7), C3(H3), C53(H53), C38(H38)
2.c Idealised Me refined as rotating group:
 C57(H57A,H57B,H57C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              13965
_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 4.098
_oxdiff_exptl_absorpt_empirical_full_min 0.271