Efficient circularly polarized luminescence from zero-dimensional terbium- and europium-based hybrid metal halides.
Zhang, Yan; Wei, Yi; Li, Chen; Wang, Yuxuan; Liu, Yulian; He, Meiying; Luo, Zhishan; Chang, Xiaoyong; Kuang, Xiaojun; Quan, Zewei; Chemical communications (Cambridge, England) 61 (2024) 85–88; doi:10.1039/d4cc05206d

data_7134023
_publ_section_title
;
 Efficient circularly polarized luminescence from zero-dimensional
 terbium- and europium-based hybrid metal halides.
;
_journal_issue                   1
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              85
_journal_page_last               88
_journal_paper_doi               10.1039/d4cc05206d
_journal_volume                  61
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(Cl6 Tb), 6(C5 H12 N O)'
_chemical_formula_sum            'C30 H72 Cl12 N6 O6 Tb2'
_chemical_formula_weight         1356.17
_chemical_properties_physical    Moisture-sensitive
_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   geom
_audit_creation_date             2024-09-18
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-20 deposited with the CCDC.	2024-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.179(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.2356(17)
_cell_length_b                   11.9576(15)
_cell_length_c                   16.874(2)
_cell_measurement_reflns_used    9468
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.31
_cell_volume                     2643.4(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Apex3 (Bruker 2018)'
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT 2014'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Bruker PHOTON III area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w and \f 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  0.0637
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32848
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         1.834
_diffrn_source                   'microfocus Metaljet'
_diffrn_source_type              'Incoatec Metaljet'
_exptl_absorpt_coefficient_mu    3.302
_exptl_absorpt_correction_T_max  0.0932
_exptl_absorpt_correction_T_min  0.0436
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1457 before and 0.0908 after correction.
The Ratio of minimum to maximum transmission is 0.4678.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.914
_refine_diff_density_min         -1.511
_refine_diff_density_rms         0.184
_refine_ls_abs_structure_details
;
 Flack x determined using 3253 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_coef       0.0018(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         9643
_refine_ls_number_restraints     226
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0735
_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^)+(0.0903P)^2^+50.8093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1879
_refine_ls_wR_factor_ref         0.2028
_reflns_Friedel_coverage         0.897
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                8002
_reflns_number_total             9643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc05206d2.cif
_cod_data_source_block           mo_923_1_0m_b
_cod_depositor_comments
'Adding full bibliography for 7134023--7134026.cif.'
_cod_database_code               7134023
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H6A,H6B,H6C} of C6, {H1C,H1D,H1E} of C1, {H16A,H16B,H16C}
  of C16, {H26A,H26B,H26C} of C26, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  {H11D,H11E,H11F} of C11A, {H11A,H11B,H11C} of C11, {H21A,H21B,H21C} of C21
2. Restrained distances
 O3-C14 \\sim O3A-C14A
 with sigma of 0.02
 O3-C13 \\sim O3A-C13A
 with sigma of 0.02
 N3-C15 \\sim N3A-C15A
 with sigma of 0.02
 N3-C12 \\sim N3A-C12A
 with sigma of 0.02
 C11-C12 \\sim C11A-C12A
 with sigma of 0.02
 C15-C14 \\sim C15A-C14A
 with sigma of 0.02
 C12-C13 \\sim C12A-C13A
 with sigma of 0.02
 O3-C15 \\sim O3A-C15A
 with sigma of 0.04
 O3-C12 \\sim O3A-C12A
 with sigma of 0.04
 N3-C11 \\sim N3A-C11A
 with sigma of 0.04
 N3-C14 \\sim N3A-C14A
 with sigma of 0.04
 N3-C13 \\sim N3A-C13A
 with sigma of 0.04
 C11-C13 \\sim C11A-C13A
 with sigma of 0.04
 C15-C12 \\sim C15A-C12A
 with sigma of 0.04
 C14-C13 \\sim C14A-C13A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O3 \\sim N3 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim O3A \\sim
N3A \\sim C11A \\sim C12A \\sim C13A \\sim C14A \\sim C15A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(Cl8) = Uanis(Cl8A)
Uanis(Cl11) = Uanis(Cl12)
Uanis(Cl9) = Uanis(Cl9A)
Uanis(Cl10) = Uanis(Cl)
4. Others
 Sof(Cl8A)=Sof(Cl12)=Sof(Cl9A)=Sof(Cl)=1-FVAR(1)
 Sof(Cl8)=Sof(Cl9)=Sof(Cl10)=Sof(Cl11)=FVAR(1)
 Sof(O3A)=Sof(N3A)=Sof(H3AA)=Sof(H3AB)=Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=
 Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C14A)=Sof(H14C)=
 Sof(H14D)=Sof(C15A)=Sof(H15C)=Sof(H15D)=1-FVAR(2)
 Sof(O3)=Sof(N3)=Sof(H3C)=Sof(H3D)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=
 Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C2(H2), C7(H7), C12(H12), C12A(H12A), C17(H17), C22(H22), C27(H27)
5.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), N2(H2A,H2B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), N3(H3C,H3D), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), N3A(H3AA,H3AB), C13A(H13C,H13D), C14A(H14C,H14D), C15A(H15C,
 H15D), N4(H4C,H4D), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), N5(H5C,
 H5D), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), N6(H6D,H6E), C28(H28A,
 H28B), C29(H29A,H29B), C30(H30A,H30B)
5.c Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E), C6(H6A,H6B,H6C), C11(H11A,H11B,H11C), C11A(H11D,H11E,H11F),
 C16(H16A,H16B,H16C), C21(H21A,H21B,H21C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              26159
_shelx_hkl_checksum              30763
_olex2_submission_special_instructions 'No special instructions were received'