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_7249507
_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         '0.5(C138 H126 Eu4 N8 O32), Cl O4, 0.5(H2 O)'
_chemical_formula_sum            'C69 H64 Cl Eu2 N4 O20.5'
_chemical_formula_weight         1616.61
_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
_audit_creation_date             2024-07-19
_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                 99.673(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7229(8)
_cell_length_b                   28.1271(19)
_cell_length_c                   17.3870(10)
_cell_measurement_reflns_used    25742
_cell_measurement_temperature    120
_cell_measurement_theta_max      69.50
_cell_measurement_theta_min      3.02
_cell_volume                     6615.7(7)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)
;
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
 1114 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38793
_diffrn_reflns_point_group_measured_fraction_full 0.785
_diffrn_reflns_point_group_measured_fraction_max 0.785
_diffrn_reflns_theta_full        64.997
_diffrn_reflns_theta_max         64.997
_diffrn_reflns_theta_min         3.019
_exptl_absorpt_coefficient_mu    14.475
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3252
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.462
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details
;
 Flack x determined using 4727 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1746
_refine_ls_number_reflns         17660
_refine_ls_number_restraints     1278
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+51.3541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1278
_reflns_Friedel_coverage         0.562
_reflns_Friedel_fraction_full    0.578
_reflns_Friedel_fraction_max     0.578
_reflns_number_gt                15507
_reflns_number_total             17660
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00957f2.cif
_cod_data_source_block           R-Eu-phen
_cod_depositor_comments
'Adding full bibliography for 7249504--7249511.cif.'
_cod_original_formula_sum        'C69 H64 Cl Eu2 N4 O20.50'
_cod_database_code               7249507
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.761
_shelx_estimated_absorpt_t_min   0.595
_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
 C9-C5 = C93-C5 = C68-C44 = C44-C38 = C90-C31 = C90-C22 = C8-C2 = C8-C13 = C88-
 C16 = C94-C16 = C45-C102 = C45-C37 = C29-C21 = C54-C29 = C65-C1 = C7-C65 = C49-
 C24 = C49-C35 = C43-C23 = C42-C23
 1.5 with sigma of 0.0002
 C27-C13 = C76-C13 = C76-C128 = C128-C127 = C131-C127 = C27-C131 = C31-C18 =
 C18-C123 = C123-C111 = C111-C104 = C66-C104 = C66-C31 = C94-C64 = C64-C106 =
 C117-C106 = C117-C114 = C130-C114 = C94-C130 = C71-C102 = C96-C102 = C96-C92 =
 C92-C120 = C41-C120 = C71-C41 = C77-C116 = C78-C77 = C69-C116 = C69-C26 = C98-
 C10 = C3-C10 = C34-C26 = C34-C3 = C3-C25 = C62-C25 = C62-C14 = C38-C15 = C122-
 C101 = C38-C101 = C133-C122 = C133-C115 = C15-C115 = C79-C50 = C79-C53 = C84-
 C12 = C84-C80 = C84-C53 = C80-C32 = C52-C32 = C52-C19 = C81-C73 = C73-C63 = C6-
 C11 = C36-C11 = C4-C36 = C4-C30 = C4-C39 = C51-C39 = C51-C105 = C87-C105 = C87-
 C30 = C112-C105 = C112-C107 = C107-C103 = C7-C48 = C82-C48 = C82-C56 = C56-C17
 = C40-C17 = C7-C40 = C86-C61 = C129-C113 = C86-C100 = C129-C100 = C21-C113 =
 C61-C21 = C59-C28 = C59-C110 = C33-C110 = C70-C33 = C46-C33 = C58-C46 = C83-
 C70 = C58-C55 = C97-C55 = C83-C55 = C97-C57 = C67-C57 = C42-C121 = C135-C121 =
 C135-C134 = C134-C119 = C124-C119 = C42-C124 = C91-C85 = C93-C91 = C93-C132 =
 C132-C126 = C81-C52 = C126-C108 = C85-C108 = C95-C118 = C95-C24 = C60-C24 =
 C99-C60 = C99-C136 = C136-C118
 1.38 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
4. Others
 Fixed Y: C84(0.499269) C97(0.376529)
5.a Riding coordinates:
 O4(H4A,H4B), O14(H14A,H14B), O41(H41A,H41B)
5.b Ternary CH refined with riding coordinates:
 C5(H5), C8(H8), C16(H16), C23(H23), C29(H29), C44(H44), C45(H45), C49(H49),
 C65(H65), C90(H90)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C10(H10), C11(H11), C14(H14), C15(H15), C17(H17), C18(H18), C25(H25),
 C27(H27), C28(H28), C32(H32), C36(H36), C39(H39), C40(H40), C41(H41), C46(H46),
  C48(H48), C50(H50), C51(H51), C53(H53), C56(H56), C57(H57), C58(H58),
 C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C66(H66), C67(H67),
  C71(H71), C73(H73), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80),
 C81(H81), C82(H82), C85(H85), C86(H86), C91(H91), C92(H92), C95(H95), C96(H96),
  C97(H97), C98(H98), C99(H99), C100(H100), C101(H101), C103(H103), C104(H104),
 C106(H106), C107(H107), C108(H108), C110(H110), C111(H111), C112(H112),
 C113(H113), C114(H114), C115(H115), C116(H116), C117(H117), C118(H118),
 C119(H119), C120(H120), C121(H121), C122(H122), C123(H123), C124(H124),
 C126(H126), C127(H127), C128(H128), C129(H129), C130(H130), C131(H131),
 C132(H132), C133(H133), C134(H134), C135(H135), C136(H136)
5.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C47(H47A,H47B,H47C), C72(H72A,H72B,H72C), C74(H74A,H74B,
 H74C), C75(H75A,H75B,H75C), C89(H89A,H89B,H89C), C109(H10A,H10B,H10C),
 C125(H12A,H12B,H12C), C137(H13A,H13B,H13C), C138(H13D,H13E,H13F)
;
_shelx_res_checksum              27544
_shelx_hkl_checksum              38760
_olex2_submission_special_instructions 'No special instructions were received'