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_7719136
_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), 5(C5 H14 N2), Cl'
_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                   12.8744(8)
_cell_length_b                   16.1274(10)
_cell_length_c                   27.3771(16)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      25.346
_cell_measurement_theta_min      2.171
_cell_volume                     5684.3(6)
_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 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0833
_diffrn_reflns_av_unetI/netI     0.0713
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            45909
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.369
_diffrn_reflns_theta_min         1.748
_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    4.617
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1220 before and 0.0865 after correction.
The Ratio of minimum to maximum transmission is 0.7700.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.941
_exptl_crystal_description       block
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.175
_refine_ls_abs_structure_details
;
 Flack x determined using 3579 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(7)
_refine_ls_extinction_coef       0.000080(16)
_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   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         10392
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0369
_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^)+0.3349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0618
_reflns_Friedel_coverage         0.806
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                9150
_reflns_number_total             10392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01465d2.cif
_cod_data_source_block           RTb
_cod_depositor_comments
'Adding full bibliography for 7719134--7719137.cif.'
_cod_database_code               7719136
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.826
_shelx_estimated_absorpt_t_min   0.668
_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. Uiso/Uaniso restraints and constraints
N1 \\sim N2 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim N9 \\sim N10
\\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 1.7A
N1 \\sim N2 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
Uanis(C9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C14) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C11) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Ternary CH refined with riding coordinates:
 C14(H14), C4(H4), C9(H9), C19(H19), C24(H24)
3.b Secondary CH2 refined with riding coordinates:
 N5(H5A,H5B), N6(H6A,H6B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 N1(H1A,H1B), N2(H2A,H2B), C1(H1C,H1D), C2(H2C,H2D), C3(H3A,H3B), N3(H3C,H3D),
 N4(H4A,H4B), C6(H6C,H6D), C7(H7A,H7B), C8(H8A,H8B), N7(H7C,H7D), N8(H8C,H8D),
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), N9(H9A,H9B), N10(H10D,H10E),
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B)
3.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C5(H5C,H5D,H5E), C10(H10A,H10B,H10C), C20(H20A,H20B,
 H20C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              92618
_shelx_hkl_checksum              32015
_olex2_submission_special_instructions 'No special instructions were received'