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_7249504
_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 Eu O8, Cl O4'
_chemical_formula_sum            'C18 H22 Cl Eu O12'
_chemical_formula_weight         617.76
_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                   6.2461(2)
_cell_length_b                   18.7509(5)
_cell_length_c                   19.0329(4)
_cell_measurement_reflns_used    8626
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      77.1320
_cell_measurement_theta_min      3.2820
_cell_volume                     2229.13(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.975
_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    -64.00  22.00   0.50    0.05    --  -49.58  62.00-105.00  172
  2  \w    -23.00  24.00   0.50    0.05    --  -49.58  19.00   0.00   94
  3  \w    -23.00  24.00   0.50    0.05    --  -49.58  19.00  30.00   94
  4  \w    -81.00 -32.00   0.50    0.06    -- -104.50  69.00 112.00   98
  5  \w    -62.00 -32.00   0.50    0.06    -- -104.50  57.00  90.00   60
  6  \w    -62.00 -32.00   0.50    0.06    -- -104.50  57.00  60.00   60
  7  \w    -62.00 -32.00   0.50    0.06    -- -104.50  57.00 -30.00   60
  8  \w    -62.00 -32.00   0.50    0.06    -- -104.50  57.00-150.00   60
  9  \w     42.00  90.00   0.50    0.05    --   49.58  38.00-120.00   96
 10  \w     92.00 178.00   0.50    0.06    --  106.85  62.00-105.00  172
 11  \w     42.00 121.00   0.50    0.05    --   49.58  38.00 -30.00  158
 12  \w     35.00 106.00   0.50    0.06    --  106.85 -94.00-117.00  142
 13  \w     35.00  69.00   0.50    0.06    --  106.85 -57.00 -90.00   68
 14  \w     35.00  69.00   0.50    0.06    --  106.85 -57.00 -60.00   68
 15  \w     35.00  88.00   0.50    0.06    --  106.85 -69.00 -20.00  106
 16  \w     35.00  69.00   0.50    0.06    --  106.85 -57.00   0.00   68
;
_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      0.1056129000
_diffrn_orient_matrix_UB_12      0.0446999000
_diffrn_orient_matrix_UB_13      0.0584833000
_diffrn_orient_matrix_UB_21      -0.2032149000
_diffrn_orient_matrix_UB_22      0.0461973000
_diffrn_orient_matrix_UB_23      0.0052101000
_diffrn_orient_matrix_UB_31      -0.0911013000
_diffrn_orient_matrix_UB_32      -0.0512035000
_diffrn_orient_matrix_UB_33      0.0557628000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0941
_diffrn_reflns_av_unetI/netI     0.0728
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12000
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.784
_diffrn_reflns_theta_min         3.309
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.806
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (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    1.841
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.316
_refine_diff_density_min         -3.206
_refine_diff_density_rms         0.267
_refine_ls_abs_structure_details
;
 Flack x determined using 1320 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         4229
_refine_ls_number_restraints     238
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0693
_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^)+(0.1565P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1876
_refine_ls_wR_factor_ref         0.1933
_reflns_Friedel_coverage         0.589
_reflns_Friedel_fraction_full    0.864
_reflns_Friedel_fraction_max     0.778
_reflns_number_gt                3895
_reflns_number_total             4229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00957f2.cif
_cod_data_source_block           R-Eu
_cod_depositor_comments
'Adding full bibliography for 7249504--7249511.cif.'
_cod_database_code               7249504
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.670
_shelx_estimated_absorpt_t_min   0.476
_diffrn_oxdiff_digest_frames
;
0153d2a09829c391b598a501c1559423e400109577c
;
_diffrn_oxdiff_digest_hkl
;
018245f95d311ce8e2384acd24889bda67efd3
;
_reflns_odcompleteness_completeness 100.00
_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
 C5-C17 = C18-C17 = C18-C15 = C15-C13 = C3-C13 = C5-C3 = C2-C1 = C7-C1 = C7-C4
 = C4-C14 = C14-C12 = C2-C12
 1.38 with sigma of 0.0002
 C8-C1 = C8-C6 = C3-C10 = C16-C10
 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 0.04 and sigma
for terminal atoms of 0.08
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:
 O6(H6A,H6B)
5.b Rotating group:
 O5(H5A,H5B)
5.c Ternary CH refined with riding coordinates:
 C8(H8), C10(H10)
5.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C7(H7), C12(H12), C13(H13), C14(H14), C15(H15),
 C17(H17), C18(H18)
5.e Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              20918
_shelx_hkl_checksum              94212
_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 4.088
_oxdiff_exptl_absorpt_empirical_full_min 0.381