Regulating the Excited State Chirality to Fabricate High-Performance-Solid-State Circularly Polarized Luminescence Materials
Han, Jianlei; Shi, Yonghong; Jin, Xue; Yang, Xuefeng; Duan, Pengfei; Chemical Science  (2022) –; doi:10.1039/D2SC01846B

data_1566881
_publ_section_title
;
 Regulating the Excited State Chirality to Fabricate
 High-Performance-Solid-State Circularly Polarized Luminescence Materials
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC01846B
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C51 H32 O4, C H4 O'
_chemical_formula_sum            'C52 H36 O5'
_chemical_formula_weight         740.81
_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             2021-07-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-20 deposited with the CCDC.	2022-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.2123(2)
_cell_length_b                   17.9092(4)
_cell_length_c                   27.4926(5)
_cell_measurement_reflns_used    10059
_cell_measurement_temperature    169.99(16)
_cell_measurement_theta_max      75.0210
_cell_measurement_theta_min      3.1750
_cell_volume                     3551.12(14)
_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 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(16)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.966
_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    -22.00  20.00   0.50    1.50    --  -47.45  19.00 -30.00   84
  2  \w    -59.00 -32.00   0.50    4.00    --  -99.00  63.00 -14.00   54
  3  \w    -53.00 -26.00   0.50    4.00    --  -99.00  61.00  60.00   54
  4  \w    -56.00 -28.00   0.50    4.00    --  -99.00  58.00 153.00   56
  5  \w   -116.00 -89.00   0.50    4.00    --  -99.00 -15.00 120.00   54
  6  \w   -125.00 -87.00   0.50    4.00    --  -99.00 -30.00  60.00   76
  7  \w   -100.00 -74.00   0.50    1.50    --  -47.45-125.00   0.00   52
  8  \w   -115.00 -76.00   0.50    4.00    --  -99.00-125.00   0.00   78
  9  \w   -116.00 -82.00   0.50    1.50    --  -47.45-125.00-180.00   68
 10  \w    -13.00  29.00   0.50    1.50    --   47.45 -19.00-120.00   84
 11  \w     31.00  57.00   0.50    4.00    --  103.25 -63.00-151.00   52
 12  \w     35.00  75.00   0.50    4.00    --  103.25 -61.00-120.00   80
 13  \w     42.00  68.00   0.50    4.00    --  103.25 -58.00  12.00   52
 14  \w     35.00  69.00   0.50    4.00    --  103.25-120.00 138.00   68
 15  \w     33.00  60.00   0.50    4.00    --  103.25 -61.00 150.00   54
 16  \w     32.00 119.00   0.50    1.50    --   47.45  58.00 153.00  174
 17  \w    -97.00 -26.00   0.50    4.00    --  -99.00  77.00-120.00  142
 18  \w   -167.00-134.00   0.50    4.00    --  -99.00 -15.00 120.00   66
 19  \w   -168.00-127.00   0.50    4.00    --  -99.00 -30.00  60.00   82
 20  \w   -164.00-135.00   0.50    4.00    --  -99.00-125.00   0.00   58
 21  \w     60.00 131.00   0.50    4.00    --  103.25 155.00  19.00  142
 22  \w     87.00 168.00   0.50    4.00    --  103.25  63.00 -14.00  162
;
_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      0.2118920000
_diffrn_orient_matrix_UB_12      0.0072599000
_diffrn_orient_matrix_UB_13      0.0051136000
_diffrn_orient_matrix_UB_21      -0.0003232000
_diffrn_orient_matrix_UB_22      -0.0628373000
_diffrn_orient_matrix_UB_23      0.0382470000
_diffrn_orient_matrix_UB_31      0.0265771000
_diffrn_orient_matrix_UB_32      -0.0583064000
_diffrn_orient_matrix_UB_33      -0.0406403000
_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  0.0404
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            21470
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.426
_diffrn_reflns_theta_min         2.945
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.700
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67068
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       needle
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 2416 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         6941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0871P)^2^+0.1286P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1236
_reflns_Friedel_coverage         0.725
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.917
_reflns_number_gt                6239
_reflns_number_total             6941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01846b5.cif
_cod_data_source_block           tx5985
_cod_database_code               1566881
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHO
_reflns_odcompleteness_completeness 99.97
_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, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C10(H10A,H10B), C11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C13(H13), C14(H14), C15(H15), C21(H21), C22(H22),
 C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C31(H31), C32(H32), C37(H37),
  C38(H38), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45), C47(H47), C48(H48)
2.c Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C)
2.d Idealised tetrahedral OH refined as rotating group:
 O5(H5A)
;
_shelx_res_checksum              40850
_shelx_hkl_checksum              98855
_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 2.056
_oxdiff_exptl_absorpt_empirical_full_min 0.462