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_7249505
_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         'C18 H22 O8 Tb, Cl O4'
_chemical_formula_sum            'C18 H22 Cl O12 Tb'
_chemical_formula_weight         624.72
_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   mixed
_atom_sites_solution_primary     dual
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7651(8)
_cell_length_b                   18.9706(10)
_cell_length_c                   6.2102(3)
_cell_measurement_reflns_used    12317
_cell_measurement_temperature    120
_cell_measurement_theta_max      70.01
_cell_measurement_theta_min      4.67
_cell_volume                     2210.74(18)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            10260
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        66.471
_diffrn_reflns_theta_max         66.471
_diffrn_reflns_theta_min         4.662
_exptl_absorpt_coefficient_mu    17.410
_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    1.877
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.194
_refine_diff_density_min         -1.407
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details
;
 Flack x determined using 1426 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         3837
_refine_ls_number_restraints     292
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+15.5146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1242
_reflns_Friedel_coverage         0.700
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                3670
_reflns_number_total             3837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00957f2.cif
_cod_data_source_block           R-Tb
_cod_depositor_comments
'Adding full bibliography for 7249504--7249511.cif.'
_cod_database_code               7249505
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.722
_shelx_estimated_absorpt_t_min   0.543
_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
 C17-C13 = C17-C9 = C9-C8 = C8-C2 = C13-C10 = C10-C2 = C11-C5 = C6-C5 = C16-C6
 = C18-C16 = C18-C15 = C15-C11
 1.38 with sigma of 0.0002
 C14-C1 = C5-C1 = C7-C2 = C7-C3
 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(O3) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O12)
\\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: O10(0.5) O11(0.5) O12(0.5) O13(0.5) O14(0.5) O15(0.5)
5.a Riding coordinates:
 O5(H5A,H5B), O8(H8A,H8B)
5.b Ternary CH refined with riding coordinates:
 C1(H1), C7(H7)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C15(H15), C16(H16),
 C17(H17), C18(H18)
5.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              11163
_shelx_hkl_checksum              55946
_olex2_submission_special_instructions 'No special instructions were received'