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_7134024
_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 rm
_chemical_formula_moiety         '2(Cl6 Eu), 6(C5 H12 N O)'
_chemical_formula_sum            'C30 H72 Cl12 Eu2 N6 O6'
_chemical_formula_weight         1342.25
_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             2024-09-15
_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                 97.7990(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3330(5)
_cell_length_b                   11.9679(4)
_cell_length_c                   16.8004(6)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.30
_cell_volume                     2656.01(16)
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2014'
_diffrn_ambient_temperature      100.00
_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 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            74209
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         1.833
_exptl_absorpt_coefficient_mu    2.985
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6476
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0843 before and 0.0717 after correction.
The Ratio of minimum to maximum transmission is 0.8686.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.349
_refine_diff_density_min         -1.160
_refine_diff_density_rms         0.140
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_coef       0.00047(11)
_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   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         12185
_refine_ls_number_restraints     285
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0446
_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^)+17.9734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0885
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                10199
_reflns_number_total             12185
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc05206d2.cif
_cod_data_source_block           mo_reu_0m
_cod_depositor_comments
'Adding full bibliography for 7134023--7134026.cif.'
_cod_database_code               7134024
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.97(2)
 0.03(2)
2. 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
3. Restrained distances
 O4A-C19A
 1.42 with sigma of 0.02
 C19-C20 = C19A-C20A
 1.54 with sigma of 0.02
 O4-C19
 1.42 with sigma of 0.02
 C12-C11
 1.54 with sigma of 0.02
 O3-C14 = O3-C13
 1.42 with sigma of 0.02
 C13-C12 = C15-C14
 1.54 with sigma of 0.02
 C15-C12
 2.5 with sigma of 0.04
 O4-C19 \\sim O4A-C19A
 with sigma of 0.02
 O4-C18 \\sim O4A-C18A
 with sigma of 0.02
 C17-C18 \\sim C17A-C18A
 with sigma of 0.02
 C17-C16 \\sim C17A-C16A
 with sigma of 0.02
 C17-N4 \\sim C17A-N4A
 with sigma of 0.02
 C19-C20 \\sim C19A-C20A
 with sigma of 0.02
 N4-C20 \\sim N4A-C20A
 with sigma of 0.02
 O4-C17 \\sim O4A-C17A
 with sigma of 0.04
 O4-C20 \\sim O4A-C20A
 with sigma of 0.04
 C17-C20 \\sim C17A-C20A
 with sigma of 0.04
 C19-C18 \\sim C19A-C18A
 with sigma of 0.04
 C19-N4 \\sim C19A-N4A
 with sigma of 0.04
 C18-C16 \\sim C18A-C16A
 with sigma of 0.04
 C18-N4 \\sim C18A-N4A
 with sigma of 0.04
 C16-N4 \\sim C16A-N4A
 with sigma of 0.04
 N3-C15 \\sim N3-C12
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
N3 \\sim C11 \\sim C12 \\sim C13 \\sim C15 \\sim O3 \\sim C14: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C17 \\sim O4 \\sim C19 \\sim C18 \\sim C20 \\sim N4 \\sim C16 \\sim C17A \\sim
C16A \\sim C18A \\sim N4A \\sim O4A \\sim C20A \\sim C19A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(N1) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(Cl11) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(Eu11) = Uanis(Eu)
Uanis(Cl4) = Uanis(Cl4A)
Uanis(Cl11) = Uanis(Cl14)
Uanis(Cl5A) = Uanis(Cl5)
Uanis(Cl10) = Uanis(Cl15)
Uanis(Cl3) = Uanis(Cl3A)
Uanis(Cl12) = Uanis(Cl13)
Uanis(Cl2) = Uanis(Cl2A)
5. Others
 Sof(Cl3A)=Sof(Cl5)=Sof(Cl4A)=1-FVAR(1)
 Sof(Cl4)=Sof(Cl5A)=Sof(Cl3)=FVAR(1)
 Sof(Cl2A)=Sof(Cl13)=Sof(Cl14)=Sof(Cl15)=Sof(Eu)=1-FVAR(2)
 Sof(Eu11)=Sof(Cl10)=Sof(Cl11)=Sof(Cl2)=Sof(Cl12)=FVAR(2)
 Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(O4A)=Sof(C19A)=Sof(H19C)=
 Sof(H19D)=Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(C20A)=Sof(H20C)=Sof(H20D)=
 Sof(C17A)=Sof(H17A)=Sof(N4A)=Sof(H4AA)=Sof(H4AB)=1-FVAR(3)
 Sof(O4)=Sof(C17)=Sof(H17)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C18)=Sof(H18A)=
 Sof(H18B)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(N4)=Sof(H4C)=Sof(H4D)=
 Sof(C20)=Sof(H20A)=Sof(H20B)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C22(H22), C7(H7), C27(H27), C2(H2), C17(H17), C17A(H17A), C12(H12)
6.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C25(H25A,H25B), C23(H23A,H23B), N2(H2A,H2B), C29(H29A,H29B),
 N5(H5C,H5D), C9(H9A,H9B), C4(H4A,H4B), C8(H8A,H8B), C5(H5A,H5B), C10(H10A,
 H10B), C24(H24A,H24B), C28(H28A,H28B), N6(H6A,H6B), C30(H30A,H30B), C3(H3A,
 H3B), C19(H19A,H19B), C18(H18A,H18B), N4(H4C,H4D), C20(H20A,H20B), C19A(H19C,
 H19D), C18A(H18C,H18D), C20A(H20C,H20D), N4A(H4AA,H4AB), N3(H3C,H3D), C15(H15A,
 H15B), C13(H13A,H13B), C14(H14A,H14B)
6.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C6(H6C,H6D,H6E), C26(H26A,H26B,H26C), C1(H1C,H1D,H1E),
 C16(H16A,H16B,H16C), C16A(H16D,H16E,H16F), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              81705
_shelx_hkl_checksum              39008
_olex2_submission_special_instructions 'No special instructions were received'