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_7249510
_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                 99.823(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7334(5)
_cell_length_b                   28.0916(7)
_cell_length_c                   17.3794(6)
_cell_measurement_reflns_used    29921
_cell_measurement_temperature    120
_cell_measurement_theta_max      69.52
_cell_measurement_theta_min      3.62
_cell_volume                     6606.6(4)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)
;
_computing_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_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 0.991
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
 2091 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  0.0943
_diffrn_reflns_av_unetI/netI     0.1117
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            72197
_diffrn_reflns_point_group_measured_fraction_full 0.786
_diffrn_reflns_point_group_measured_fraction_max 0.770
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         69.621
_diffrn_reflns_theta_min         3.626
_exptl_absorpt_coefficient_mu    11.432
_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    1.639
_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         1.417
_refine_diff_density_min         -1.080
_refine_diff_density_rms         0.172
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.021(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1747
_refine_ls_number_reflns         19131
_refine_ls_number_restraints     1285
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0815
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1583P)^2^+7.3802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1966
_refine_ls_wR_factor_ref         0.2268
_reflns_Friedel_coverage         0.540
_reflns_Friedel_fraction_full    0.572
_reflns_Friedel_fraction_max     0.552
_reflns_number_gt                14476
_reflns_number_total             19131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00957f2.cif
_cod_data_source_block           R-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               7249510
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.804
_shelx_estimated_absorpt_t_min   0.658
_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
 C31-C10 = C95-C125 = C31-C125 = C96-C95 = C96-C57 = C57-C10 = C123-C122 = C44-
 C38 = C91-C38 = C91-C122 = C98-C123 = C98-C44 = C8-C109 = C8-C58 = C58-C124 =
 C121-C109 = C138-C121 = C138-C124 = C77-C128 = C128-C101 = C126-C101 = C64-
 C133 = C77-C64 = C133-C126 = C97-C40 = C97-C113 = C67-C113 = C67-C15 = C59-
 C102 = C67-C102 = C59-C56 = C56-C22 = C22-C15 = C80-C14 = C80-C53 = C56-C53 =
 C79-C115 = C33-C115 = C33-C107 = C71-C107 = C83-C107 = C83-C66 = C66-C111 =
 C49-C111 = C71-C49 = C7-C118 = C137-C118 = C137-C131 = C92-C131 = C7-C18 = C92-
 C18 = C99-C130 = C135-C130 = C136-C135 = C136-C127 = C47-C127 = C99-C47 = C55-
 C114 = C120-C114 = C120-C103 = C85-C103 = C85-C65 = C65-C55 = C73-C37 = C37-
 C35 = C129-C119 = C35-C119 = C74-C129 = C74-C73 = C24-C16 = C24-C104 = C134-
 C104 = C112-C110 = C16-C110 = C134-C112 = C21-C20 = C50-C20 = C50-C45 = C45-
 C27 = C27-C25 = C25-C21 = C88-C86 = C86-C100 = C36-C100 = C42-C36 = C87-C36 =
 C87-C116 = C46-C116 = C78-C46 = C78-C42 = C89-C46 = C89-C61 = C61-C12 = C93-
 C117 = C60-C117 = C34-C26 = C34-C29 = C26-C2 = C32-C2 = C72-C2 = C90-C72 = C90-
 C70 = C82-C70 = C70-C108 = C94-C108 = C94-C54 = C82-C32
 1.38 with sigma of 0.0002
 C17-C10 = C28-C17 = C5-C4 = C8-C4 = C44-C13 = C76-C128 = C76-C19 = C68-C18 =
 C9-C68 = C47-C11 = C52-C11 = C55-C3 = C6-C3 = C62-C30 = C30-C16 = C41-C1 = C41-
 C27 = C48-C35 = C48-C23 = C51-C13
 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(O41) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Y: O41(0.27158)
5.a Riding coordinates:
 O4(H4A,H4B), O17(H17A,H17B), O41(H41A,H41B)
5.b Ternary CH refined with riding coordinates:
 C3(H3), C4(H4), C11(H11), C13(H13), C17(H17), C30(H30), C41(H41), C48(H48),
 C68(H68), C76(H76)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C12(H12), C14(H14), C20(H20), C21(H21), C24(H24), C25(H25), C26(H26),
 C29(H29), C31(H31), C33(H33), C34(H34), C37(H37), C38(H38), C40(H40), C45(H45),
  C50(H50), C53(H53), C54(H54), C57(H57), C58(H58), C59(H59), C60(H60),
 C61(H61), C64(H64), C65(H65), C66(H66), C72(H72), C73(H73), C74(H74), C77(H77),
  C79(H79), C80(H80), C83(H83), C85(H85), C86(H86), C87(H87), C88(H88),
 C89(H89), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94), C95(H95), C96(H96),
  C97(H97), C98(H98), C99(H99), C100(H100), C101(H101), C102(H102), C103(H103),
 C104(H104), C108(H108), C109(H109), C110(H110), 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), C125(H125),
 C126(H126), C127(H127), C129(H129), C130(H130), C131(H131), C133(H133),
 C134(H134), C135(H135), C136(H136), C137(H137), C138(H138)
5.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C43(H43A,H43B,H43C), C63(H63A,H63B,H63C), C69(H69A,H69B,
 H69C), C75(H75A,H75B,H75C), C81(H81A,H81B,H81C), C84(H84A,H84B,H84C),
 C105(H10A,H10B,H10C), C106(H10D,H10E,H10F), C132(H13A,H13B,H13C)
;
_shelx_res_checksum              43965
_shelx_hkl_checksum              93092
_olex2_submission_special_instructions 'No special instructions were received'