Supramolecular assemblies of tetravalent terbium complex units: syntheses, structure, and materials properties
Xue, Tianjiao; Yang, Qing-Song; Li, Lei; Chang, Xiao-Yong; Ding, You-Song; Zheng, Zhiping; Chemical Science 16 (2025) 6805–6811; doi:10.1039/D4SC08731C

data_1574131
_publ_section_title
;
 Supramolecular assemblies of tetravalent terbium complex units:
 syntheses, structure, and materials properties
;
_journal_issue                   16
_journal_name_full               'Chemical Science'
_journal_page_first              6805
_journal_page_last               6811
_journal_paper_doi               10.1039/D4SC08731C
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C88 H72 N2 O4 Si4 Tb, 4(C4 H10 O2)'
_chemical_formula_sum            'C104 H112 N2 O12 Si4 Tb'
_chemical_formula_weight         1853.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-02-10
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-14 deposited with the CCDC.	2025-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.8750(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.7842(9)
_cell_length_b                   18.3307(7)
_cell_length_c                   23.9399(8)
_cell_measurement_reflns_used    9607
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.40
_cell_volume                     9278.6(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Apex3 (Bruker 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2014'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Bruker PHOTON II 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 0.998
_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  0.0401
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            49787
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.552
_diffrn_reflns_theta_min         2.404
_diffrn_source                   'microfocus Metaljet'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  0.2617
_exptl_absorpt_correction_T_min  0.2172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0840 before and 0.0598 after correction.
The Ratio of minimum to maximum transmission is 0.8300.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       block
_exptl_crystal_F_000             3868
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.129
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         10686
_refine_ls_number_restraints     163
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+58.5606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1164
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9433
_reflns_number_total             10686
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08731c2.cif
_cod_data_source_block           20221213_1207_5b_bpb_0m
_cod_depositor_comments
'Adding full bibliography for 1574130--1574134.cif.'
_cod_database_code               1574131
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.957
_olex2_refinement_description
;
1. Restrained distances
 O45-C47 = O45A-C47A = O45-C25 = O45A-C25A = O11-C3 = O11A-C3A = O11A-C23A =
 O11-C23
 1.42 with sigma of 0.02
 C25A-C23A = C25-C23
 1.52 with sigma of 0.02
 O46A-C58A = O46-C58 = O46-C57 = O46A-C57A = O47A-C56A = O47-C56 = O47-C55 =
 O47A-C55A
 1.42 with sigma of 0.02
 C57A-C56A = C57-C56
 1.52 with sigma of 0.02
 C58A-C57A = C57-C58 = C55A-C56A = C56-C55
 2.4 with sigma of 0.04
 O46A-C56A = O46-C56 = C57A-O47A = C57-O47
 2.46 with sigma of 0.04
 C13-C20 \\sim C5-C20
 with sigma of 0.02
 C21-C5 \\sim C53-C13
 with sigma of 0.02
 C21-C20 \\sim C53-C20
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
C5 \\sim C13 \\sim C21 \\sim C53: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 2A
O46A \\sim O47A \\sim C55A \\sim C56A \\sim C57A \\sim C58A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O11 \\sim O45 \\sim C3 \\sim C23 \\sim C25 \\sim C47: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C9) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(C21) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
Uanis(C3) = Uanis(C3A)
Uanis(O11) = Uanis(O11A)
Uanis(C23) = Uanis(C23A)
Uanis(C25) = Uanis(C25A)
Uanis(O45) = Uanis(O45A)
Uanis(C47) = Uanis(C47A)
Uanis(C55) = Uanis(C55A)
Uanis(O47) = Uanis(O47A)
Uanis(C56) = Uanis(C56A)
Uanis(C57) = Uanis(C57A)
Uanis(O46) = Uanis(O46A)
Uanis(C58) = Uanis(C58A)
3. Others
 Sof(C5)=Sof(H5)=Sof(C21)=Sof(H21)=Sof(O46A)=Sof(O47A)=Sof(C55A)=Sof(H55D)=
 Sof(H55E)=Sof(H55F)=Sof(C56A)=Sof(H56C)=Sof(H56D)=Sof(C57A)=Sof(H57C)=
 Sof(H57D)=Sof(C58A)=Sof(H58D)=Sof(H58E)=Sof(H58F)=1-FVAR(1)
 Sof(O46)=Sof(O47)=Sof(C13)=Sof(H13)=Sof(C53)=Sof(H53)=Sof(C55)=Sof(H55A)=
 Sof(H55B)=Sof(H55C)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(C57)=Sof(H57A)=Sof(H57B)=
 Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=FVAR(1)
 Fixed Sof: O11(0.5) O45(0.5) C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) C23(0.5)
 H23A(0.5) H23B(0.5) C25(0.5) H25A(0.5) H25B(0.5) C47(0.5) H47A(0.5) H47B(0.5)
 H47C(0.5) O11A(0.5) O45A(0.5) C3A(0.5) H3AA(0.5) H3AB(0.5) H3AC(0.5) C23A(0.5)
 H23C(0.5) H23D(0.5) C25A(0.5) H25C(0.5) H25D(0.5) C47A(0.5) H47D(0.5)
 H47E(0.5) H47F(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C57(H57A,H57B), C23(H23A,H23B), C25(H25A,H25B), C23A(H23C,
 H23D), C25A(H25C,H25D), C56A(H56C,H56D), C57A(H57C,H57D)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13),
 C15(H15), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C24(H24), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
 C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43),
  C44(H44), C46(H46), C48(H48), C50(H50), C52(H52), C53(H53), C54(H54)
4.c Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C58(H58A,H58B,H58C), C3(H3A,H3B,H3C), C47(H47A,H47B,
 H47C), C3A(H3AA,H3AB,H3AC), C47A(H47D,H47E,H47F), C55A(H55D,H55E,H55F),
 C58A(H58D,H58E,H58F)
;
_shelx_res_checksum              50075
_olex2_submission_special_instructions 'No special instructions were received'