Tuning the visible circularly polarized luminescence in highly emissive chiral terbium and europium chlorides.
Chen, Congcong; Luo, Zhongshiqi; Zhang, Mengke; Li, Xiaojing; Zhang, Tonghuan; Chen, Jian; Dalton transactions (Cambridge, England : 2003) 54 (2025) 12658–12666; doi:10.1039/d5dt01465d

data_7719134
_publ_section_title
;
 Tuning the visible circularly polarized luminescence in highly emissive
 chiral terbium and europium chlorides.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12658
_journal_page_last               12666
_journal_paper_doi               10.1039/d5dt01465d
_journal_volume                  54
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety         '3(Cl6 Tb), Cl, 5(C5 H14 N2)'
_chemical_formula_sum            'C25 H70 Cl19 N10 Tb3'
_chemical_formula_weight         1661.22
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-04
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-04 deposited with the CCDC.	2025-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8967(13)
_cell_length_b                   16.1383(16)
_cell_length_c                   27.412(3)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      27.453
_cell_measurement_theta_min      2.509
_cell_volume                     5705.3(10)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            34278
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.459
_diffrn_reflns_theta_min         1.949
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.600
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0830 before and 0.0734 after correction.
The Ratio of minimum to maximum transmission is 0.8919.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.934
_exptl_crystal_description       block
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.086
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.164
_refine_ls_abs_structure_details
;
 Flack x determined using 4227 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(6)
_refine_ls_extinction_coef       0.00024(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         12923
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0625
_reflns_Friedel_coverage         0.805
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                11219
_reflns_number_total             12923
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01465d2.cif
_cod_data_source_block           STb
_cod_depositor_comments
'Adding full bibliography for 7719134--7719137.cif.'
_cod_database_code               7719134
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.820
_shelx_estimated_absorpt_t_min   0.693
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C4(H4), C24(H24), C9(H9), C19(H19), C14(H14)
2.b Secondary CH2 refined with riding coordinates:
 N9(H9A,H9B), C1(H1A,H1B), N8(H8A,H8B), N1(H1C,H1D), N4(H4A,H4B), N3(H3C,H3D),
 N2(H2A,H2B), C21(H21A,H21B), N7(H7A,H7B), N5(H5D,H5E), N6(H6C,H6D), N10(H10A,
 H10B), C22(H22A,H22B), C8(H8C,H8D), C2(H2C,H2D), C12(H12A,H12B), C23(H23A,
 H23B), C13(H13A,H13B), C6(H6A,H6B), C18(H18A,H18B), C17(H17A,H17B), C3(H3A,
 H3B), C7(H7C,H7D), C11(H11A,H11B), C16(H16A,H16B)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C25(H25A,H25B,H25C), C10(H10C,H10D,H10E), C20(H20A,H20B,
 H20C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              19507
_shelx_hkl_checksum              11569
_olex2_submission_special_instructions 'No special instructions were received'