Interfacial self-assembly of a chiral pyrene exciplex into a superhelix with enhanced circularly polarized luminescence.
Yang, Yang; Yang, Chenchen; Zhu, Xuefeng; Zhang, Li; Liu, Minghua; Chemical communications (Cambridge, England) 60 (2024) 6631–6634; doi:10.1039/d4cc01820f

data_7133104
_publ_section_title
;
 Interfacial self-assembly of a chiral pyrene exciplex into a superhelix
 with enhanced circularly polarized luminescence.
;
_journal_issue                   52
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6631
_journal_page_last               6634
_journal_paper_doi               10.1039/d4cc01820f
_journal_volume                  60
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C26 H25 N O5'
_chemical_formula_sum            'C26 H25 N O5'
_chemical_formula_weight         431.47
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-04-17 deposited with the CCDC.	2024-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.0705(2)
_cell_length_b                   19.7168(7)
_cell_length_c                   21.8610(10)
_cell_measurement_reflns_used    3893
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      74.0770
_cell_measurement_theta_min      2.9990
_cell_volume                     2185.53(15)
_computing_cell_refinement       'CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.921
_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   -119.00 -52.00   0.50    2.00    --  -46.42-157.00-162.00  134
  2  \w     58.00 119.00   0.50    2.00    --   46.42 157.00-126.00  122
  3  \w   -106.00 -31.00   0.50   10.00    -- -104.50  91.00-174.00  150
  4  \w   -174.00 -90.00   0.50   10.00    -- -104.50 -33.00-149.00  168
  5  \w     40.00 110.00   0.50   10.00    --  108.85-119.00  -7.00  140
  6  \w    -23.00  29.00   0.50    2.00    --  -46.42  19.00-150.00  104
  7  \w    -22.00  24.00   0.50    2.00    --  -46.42  19.00 -90.00   92
  8  \w    -90.00 -34.00   0.50   10.00    -- -104.50 125.00  60.00  112
  9  \w    -66.00 -32.00   0.50   10.00    -- -104.50  61.00 150.00   68
 10  \w   -174.00-144.00   0.50   10.00    -- -104.50 -94.00  60.00   60
 11  \w   -173.00-147.00   0.50   10.00    -- -104.50 -15.00 120.00   52
 12  \w   -119.00 -93.00   0.50   10.00    -- -104.50 -15.00 120.00   52
 13  \w   -111.00 -85.00   0.50   10.00    -- -104.50 -94.00  60.00   52
 14  \w     78.00 105.00   0.50   10.00    --  108.85 -94.00-120.00   54
 15  \w     36.00  61.00   0.50   10.00    --  108.85 -61.00 120.00   50
 16  \w     39.00 106.00   0.50   10.00    --  108.85 -77.00 150.00  134
 17  \w     38.00  64.00   0.50   10.00    --  108.85 -61.00 -90.00   52
 18  \w     36.00  74.00   0.50   10.00    --  108.85 -61.00 -30.00   76
 19  \w     37.00  73.00   0.50   10.00    --  108.85 -61.00-120.00   72
;
_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      -0.2464911000
_diffrn_orient_matrix_UB_12      -0.0117273000
_diffrn_orient_matrix_UB_13      -0.0399229000
_diffrn_orient_matrix_UB_21      -0.1748748000
_diffrn_orient_matrix_UB_22      0.0296208000
_diffrn_orient_matrix_UB_23      0.0510402000
_diffrn_orient_matrix_UB_31      0.0320600000
_diffrn_orient_matrix_UB_32      0.0713130000
_diffrn_orient_matrix_UB_33      -0.0277088000
_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  0.0650
_diffrn_reflns_av_unetI/netI     0.0717
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12326
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         81.966
_diffrn_reflns_theta_min         3.018
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.96a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       needle
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 1177 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0646
_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^)+(0.0902P)^2^+0.7078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1630
_refine_ls_wR_factor_ref         0.1788
_reflns_Friedel_coverage         0.691
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.888
_reflns_number_gt                3622
_reflns_number_total             4400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01820f2.cif
_cod_data_source_block           tx15307
_cod_depositor_comments          'Adding full bibliography for 7133104.cif.'
_cod_database_code               7133104
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNO
_reflns_odcompleteness_completeness 98.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C18(H18)
2.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C12(H12),
 C13(H13)
2.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              72554
_shelx_hkl_checksum              88178
_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 1.928
_oxdiff_exptl_absorpt_empirical_full_min 0.427