Amplified circularly polarized luminescence of chiral lanthanide-based chains through helical assembly
Wang, Xue-Ting; Lv, Fang-Wen; Qin, Hang; Dai, Xin-Tong; Jin, Shan; Zheng, Xiu-Ying; CrystEngComm 26 (2024) 6676–6682; doi:10.1039/D4CE00957F

data_7249508
_publ_section_title
;
 Amplified circularly polarized luminescence of chiral lanthanide-based
 chains through helical assembly
;
_journal_issue                   47
_journal_name_full               CrystEngComm
_journal_page_first              6676
_journal_page_last               6682
_journal_paper_doi               10.1039/D4CE00957F
_journal_volume                  26
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C138 H126 Eu4 N8 O32, 2(Cl O4), H2 O'
_chemical_formula_sum            'C138 H128 Cl2 Eu4 N8 O41'
_chemical_formula_weight         3233.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2024-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-08-27 deposited with the CCDC.	2024-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.5968(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6925(2)
_cell_length_b                   28.1386(4)
_cell_length_c                   17.4098(2)
_cell_measurement_reflns_used    20930
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      77.4230
_cell_measurement_theta_min      3.0770
_cell_volume                     6613.91(16)
_computing_cell_refinement       'CrysAlisPro 1.171.43.100a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 42.93a 64-bit (release 05-06-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.100a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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    -38.00 -13.00   0.50    0.32    --  -49.71 110.00 156.00   50
  2  \w      9.00  36.00   0.50    0.32    --   49.71-110.00  61.00   54
  3  \w     52.00  85.00   0.50    0.32    --   49.71-110.00  61.00   66
  4  \w   -134.00-108.00   0.50    1.27    -- -104.50-110.00  61.00   52
  5  \w     82.00 107.00   0.50    1.27    --  106.85-110.00  61.00   50
  6  \w     49.00  77.00   0.50    1.27    --  106.85-110.00  61.00   56
  7  \w    -84.00 -37.00   0.50    0.32    --  -49.71 -57.00 120.00   94
  8  \w    -56.00   8.00   0.50    0.32    --  -49.71  57.00 150.00  128
  9  \w    -37.00  20.00   0.50    0.32    --  -49.71  38.00  90.00  114
 10  \w   -113.00 -76.00   0.50    0.32    --  -49.71-125.00  90.00   74
 11  \w   -122.00 -97.00   0.50    0.32    --  -49.71 -57.00 120.00   50
 12  \w   -119.00 -79.00   0.50    0.32    --  -49.71-125.00-150.00   80
 13  \w    -91.00 -13.00   0.50    0.32    --  -49.71 125.00-120.00  156
 14  \w     29.00 109.00   0.50    0.32    --   49.71  77.00-150.00  160
 15  \w    -71.00 -35.00   0.50    1.27    -- -104.50 125.00 -60.00   72
 16  \w    -96.00 -71.00   0.50    1.27    -- -104.50 110.00 156.00   50
 17  \w   -172.00-147.00   0.50    1.27    -- -104.50 -38.00-150.00   50
 18  \w   -108.00 -83.00   0.50    1.27    -- -104.50 111.00  61.77   50
 19  \w    -71.00 -39.00   0.50    1.27    -- -104.50  77.00 -60.00   64
 20  \w   -123.00 -77.00   0.50    1.27    -- -104.50 147.00-154.00   92
 21  \w    -62.00 -35.00   0.50    1.27    -- -104.50  57.00-120.00   54
 22  \w    -62.00 -37.00   0.50    1.27    -- -104.50  57.00 -30.00   50
 23  \w    -61.00 -36.00   0.50    1.27    -- -104.50 108.00 153.08   50
 24  \w   -108.00 -74.00   0.50    1.27    -- -104.50 111.00-116.38   68
 25  \w    -61.00 -33.00   0.50    1.27    -- -104.50  57.00 -90.00   56
 26  \w    -66.00 -37.00   0.50    1.27    -- -104.50 147.00-154.00   58
 27  \w   -108.00 -82.00   0.50    1.27    -- -104.50 125.00 -60.00   52
 28  \w    -62.00 -37.00   0.50    1.27    -- -104.50  57.00 150.00   50
 29  \w   -108.00 -82.00   0.50    1.27    -- -104.50 108.00 153.08   52
 30  \w   -143.00 -98.00   0.50    1.27    -- -104.50 -38.00-150.00   90
 31  \w    106.00 168.00   0.50    1.27    --  106.85  38.00   0.00  124
 32  \w     56.00 106.00   0.50    1.27    --  106.85 -99.00  90.00  100
 33  \w    102.00 178.00   0.50    1.27    --  106.85  19.00 -60.00  152
 34  \w     37.00  89.00   0.50    1.27    --  106.85 -99.00-150.00  104
 35  \w     38.00  73.00   0.50    1.27    --  106.85 -99.00   0.00   70
 36  \w     37.00 104.00   0.50    1.27    --  106.85 -99.00-180.00  134
 37  \w     37.00  69.00   0.50    1.27    --  106.85 -57.00 -90.00   64
 38  \w     41.00  67.00   0.50    1.27    --  106.85 -57.00  60.00   52
 39  \w     36.00  68.00   0.50    1.27    --  106.85 -57.00-150.00   64
 40  \w     37.00  69.00   0.50    1.27    --  106.85 -57.00-120.00   64
 41  \w     37.00  65.00   0.50    1.27    --  106.85 -57.00  90.00   56
 42  \w     99.00 129.00   0.50    1.27    --  106.85  57.00-120.00   60
 43  \w    108.00 133.00   0.50    1.27    --  106.85 110.00 156.00   50
;
_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      0.0752498000
_diffrn_orient_matrix_UB_12      -0.0176587000
_diffrn_orient_matrix_UB_13      -0.0502391000
_diffrn_orient_matrix_UB_21      0.0438787000
_diffrn_orient_matrix_UB_22      0.0504422000
_diffrn_orient_matrix_UB_23      0.0000677000
_diffrn_orient_matrix_UB_31      0.0736035000
_diffrn_orient_matrix_UB_32      -0.0119642000
_diffrn_orient_matrix_UB_33      0.0743769000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1579
_diffrn_reflns_av_unetI/netI     0.1473
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            65693
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        64.991
_diffrn_reflns_theta_max         64.991
_diffrn_reflns_theta_min         2.574
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.479
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.100a (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    1.624
_exptl_crystal_description       block
_exptl_crystal_F_000             3252
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.397
_refine_diff_density_min         -2.462
_refine_diff_density_rms         0.198
_refine_ls_abs_structure_details
;
 Flack x determined using 5932 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1747
_refine_ls_number_reflns         21356
_refine_ls_number_restraints     1286
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0727
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1240P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1823
_refine_ls_wR_factor_ref         0.2058
_reflns_Friedel_coverage         0.873
_reflns_Friedel_fraction_full    0.906
_reflns_Friedel_fraction_max     0.906
_reflns_number_gt                17558
_reflns_number_total             21356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00957f2.cif
_cod_data_source_block           S-Eu-phen
_cod_depositor_comments
'Adding full bibliography for 7249504--7249511.cif.'
_cod_original_cell_volume        6613.88(16)
_cod_database_code               7249508
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.671
_shelx_estimated_absorpt_t_min   0.477
_reflns_odcompleteness_completeness 99.03
_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, All O(H,H) groups
2. Restrained distances
 C62-C122 = C62-C125 = C138-C125 = C138-C129 = C129-C127 = C127-C122 = C84-C82
 = C88-C84 = C90-C88 = C90-C73 = C90-C85 = C94-C85 = C94-C71 = C71-C63 = C73-
 C63 = C93-C71 = C93-C75 = C75-C65 = C54-C45 = C50-C45 = C50-C113 = C117-C113 =
 C117-C114 = C54-C114 = C99-C58 = C99-C47 = C66-C47 = C66-C64 = C64-C59 = C59-
 C58 = C20-C16 = C22-C20 = C5-C22 = C5-C34 = C26-C23 = C7-C34 = C7-C25 = C26-
 C25 = C37-C35 = C37-C25 = C35-C19 = C79-C78 = C79-C72 = C72-C69 = C69-C135 =
 C81-C135 = C81-C78 = C123-C110 = C123-C107 = C107-C106 = C70-C106 = C70-C68 =
 C68-C110 = C55-C111 = C97-C128 = C97-C55 = C121-C118 = C121-C111 = C128-C118 =
 C32-C12 = C9-C32 = C9-C2 = C27-C18 = C18-C13 = C13-C11 = C2-C1 = C27-C2 = C11-
 C1 = C86-C13 = C86-C10 = C24-C10 = C92-C61 = C89-C87 = C92-C89 = C87-C83 = C83-
 C57 = C61-C57 = C120-C115 = C120-C103 = C53-C103 = C53-C108 = C119-C108 = C119-
 C115 = C130-C100 = C134-C130 = C136-C134 = C96-C136 = C96-C95 = C95-C100 =
 C124-C104 = C124-C112 = C98-C112 = C98-C131 = C131-C109 = C109-C104 = C33-C29 =
  C8-C33 = C8-C17 = C3-C17 = C21-C17 = C30-C3 = C30-C15 = C36-C21 = C36-C15 =
 C31-C15 = C31-C28 = C6-C28
 1.38 with sigma of 0.0002
 C49-C48 = C49-C45 = C52-C47 = C52-C38 = C67-C41 = C67-C62 = C81-C80 = C80-C76
 = C68-C40 = C40-C39 = C51-C46 = C55-C46 = C133-C131 = C137-C133 = C43-C42 =
 C95-C42 = C53-C14 = C4-C14 = C60-C56 = C60-C57
 1.5 with sigma of 0.0002
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.004 and sigma
for terminal atoms of 0.008
Uanis(O39) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Riding coordinates:
 O32(H32A,H32B), O33(H33A,H33B), O41(H41A,H41B)
4.b Ternary CH refined with riding coordinates:
 C14(H14), C40(H40), C42(H42), C46(H46), C49(H49), C52(H52), C60(H60),
 C67(H67), C80(H80), C133(H133)
4.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C9(H9), C10(H10), C12(H12), C16(H16), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28),
  C29(H29), C31(H31), C32(H32), C33(H33), C35(H35), C36(H36), C37(H37),
 C50(H50), C54(H54), C58(H58), C59(H59), C61(H61), C64(H64), C65(H65), C66(H66),
  C69(H69), C70(H70), C72(H72), C75(H75), C78(H78), C79(H79), C82(H82),
 C83(H83), C84(H84), C85(H85), C86(H86), C87(H87), C88(H88), C89(H89), C92(H92),
  C93(H93), C94(H94), C96(H96), C97(H97), C98(H98), C99(H99), C100(H100),
 C103(H103), C104(H104), C106(H106), C107(H107), C108(H108), C109(H109),
 C110(H110), C111(H111), C112(H112), C113(H113), C114(H114), C115(H115),
 C117(H117), C118(H118), C119(H119), C120(H120), C121(H121), C122(H122),
 C123(H123), C124(H124), C125(H125), C127(H127), C128(H128), C129(H129),
 C130(H130), C134(H134), C135(H135), C136(H136), C138(H138)
4.d Idealised Me refined with riding coordinates:
 C116(H11A,H11B,H11C)
4.e Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C74(H74A,H74B,H74C), C77(H77A,H77B,H77C), C91(H91A,H91B,
 H91C), C101(H10A,H10B,H10C), C102(H10D,H10E,H10F), C105(H10G,H10H,H10I),
 C126(H12A,H12B,H12C), C132(H13A,H13B,H13C)
;
_shelx_res_checksum              8921
_shelx_hkl_checksum              68166
_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 3.821
_oxdiff_exptl_absorpt_empirical_full_min 0.136