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_7249509
_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 N8 O32 Tb4), Cl O4, 0.5(H2 O)'
_chemical_formula_sum            'C69 H64 Cl N4 O20.5 Tb2'
_chemical_formula_weight         1630.53
_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                 99.903(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6917(7)
_cell_length_b                   28.1150(14)
_cell_length_c                   17.3468(9)
_cell_measurement_reflns_used    35514
_cell_measurement_temperature    120
_cell_measurement_theta_max      69.75
_cell_measurement_theta_min      3.14
_cell_volume                     6578.0(6)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.153.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.74.2.0 (STOE, 2018)
X-Area LANA 1.75.3.0 (STOE, 2018)
;
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
 1928 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  0.0611
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            61886
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.500
_diffrn_reflns_theta_min         3.026
_exptl_absorpt_coefficient_mu    11.481
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3771
_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    1.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3268
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.645
_refine_diff_density_min         -1.606
_refine_diff_density_rms         0.251
_refine_ls_abs_structure_details
;
 Flack x determined using 6867 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1741
_refine_ls_number_reflns         21994
_refine_ls_number_restraints     1300
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0880
_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^)+(0.0436P)^2^+268.4871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2205
_refine_ls_wR_factor_ref         0.2318
_reflns_Friedel_coverage         0.866
_reflns_Friedel_fraction_full    0.900
_reflns_Friedel_fraction_max     0.900
_reflns_number_gt                18728
_reflns_number_total             21994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00957f2.cif
_cod_data_source_block           S-Tb-phen
_cod_depositor_comments
'Adding full bibliography for 7249504--7249511.cif.'
_cod_original_formula_sum        'C69 H64 Cl N4 O20.50 Tb2'
_cod_database_code               7249509
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.803
_shelx_estimated_absorpt_t_min   0.657
_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
 C51-C120 = C61-C120 = C61-C59 = C59-C28 = C67-C59 = C67-C118 = C48-C118 = C28-
 C26 = C48-C26 = C93-C47 = C93-C48 = C47-C102 = C66-C136 = C136-C124 = C124-
 C116 = C83-C116 = C66-C50 = C83-C50 = C78-C130 = C78-C62 = C62-C109 = C121-
 C109 = C125-C121 = C130-C125 = C52-C41 = C87-C41 = C87-C43 = C43-C39 = C97-C43
 = C97-C7 = C7-C31 = C31-C16 = C39-C16 = C58-C31 = C64-C58 = C64-C54 = C8-C60 =
 C8-C131 = C138-C131 = C138-C129 = C98-C129 = C98-C60 = C35-C18 = C9-C18 = C9-
 C114 = C114-C106 = C75-C106 = C75-C35 = C57-C3 = C57-C49 = C95-C49 = C95-C27 =
 C27-C22 = C3-C22 = C77-C134 = C134-C132 = Cl1-O35 = C68-C115 = C132-C115 = C77-
 C20 = C68-C20 = C85-C11 = C85-C126 = C126-C122 = C70-C122 = C70-C37 = C37-C11 =
  C90-C30 = C90-C76 = C76-C104 = C96-C104 = C72-C104 = C72-C21 = C6-C21 = C6-
 C23 = C96-C23 = C6-C44 = C53-C44 = C53-C17 = C34-C103 = C89-C34 = C110-C103 =
 C128-C110 = C82-C128 = C89-C82 = C84-C14 = C84-C71 = C71-C117 = C117-C113 =
 C69-C113 = C69-C14 = C94-C107 = C94-C46 = C46-C123 = C127-C123 = C137-C127 =
 C137-C107 = C73-C29 = C73-C65 = C86-C29 = C86-C79 = C79-C108 = C13-C108 = C99-
 C13 = C99-C45 = C86-C45 = C91-C13 = C91-C38 = C42-C38
 1.38 with sigma of 0.0002
 C89-C2 = C2-C15 = C37-C25 = C81-C25 = C4-C33 = C33-C22 = C74-C32 = C94-C32 =
 C69-C40 = C56-C40 = C18-C101 = C101-C1 = C66-C12 = C12-C10 = C20-C19 = C5-C19 =
  C63-C100 = C60-C100 = C130-C111 = C36-C111
 1.5 with sigma of 0.0002
3. Rigid bond restraints
 C101, C1, O1, O26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. 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(O6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O26) = Uanis(O1)
5.a Riding coordinates:
 O12(H12A,H12B), O13(H13A,H13B), O41(H41A,H41B)
5.b Ternary CH refined with riding coordinates:
 C2(H2), C12(H12), C19(H19), C25(H25), C32(H32), C33(H33), C40(H40),
 C100(H100), C101(H101), C111(H111)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C8(H8), C9(H9), C11(H11), C14(H14), C17(H17), C21(H21),
 C27(H27), C29(H29), C30(H30), C34(H34), C35(H35), C38(H38), C41(H41), C42(H42),
  C44(H44), C46(H46), C47(H47), C49(H49), C50(H50), C51(H51), C52(H52),
 C53(H53), C54(H54), C57(H57), C58(H58), C61(H61), C62(H62), C64(H64), C65(H65),
  C67(H67), C68(H68), C70(H70), C71(H71), C72(H72), C73(H73), C75(H75),
 C76(H76), C77(H77), C78(H78), C79(H79), C82(H82), C83(H83), C84(H84), C85(H85),
  C87(H87), C90(H90), C91(H91), C93(H93), C95(H95), C97(H97), C98(H98),
 C102(H102), C103(H103), C106(H106), C107(H107), C108(H108), C109(H109),
 C110(H110), C113(H113), C114(H114), C115(H115), C116(H116), C117(H117),
 C118(H118), C120(H120), C121(H121), C122(H122), C123(H123), C124(H124),
 C125(H125), C126(H126), C127(H127), C128(H128), C129(H129), C131(H131),
 C132(H132), C134(H134), C136(H136), C137(H137), C138(H138)
5.d Idealised Me refined with riding coordinates:
 C55(H55A,H55B,H55C)
5.e Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C80(H80A,H80B,H80C), C88(H88A,H88B,H88C), C92(H92A,H92B,
 H92C), C105(H10A,H10B,H10C), C112(H11A,H11B,H11C), C119(H11D,H11E,H11F),
 C133(H13C,H13D,H13E), C135(H13F,H13G,H13H)
;
_shelx_res_checksum              47147
_shelx_hkl_checksum              60155
_olex2_submission_special_instructions 'No special instructions were received'