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_1574132
_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         'C84 H68 N2 O4 Si4 Tb, 3(C7 H8)'
_chemical_formula_sum            'C105 H92 N2 O4 Si4 Tb'
_chemical_formula_weight         1717.08
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
;
2025-02-25 deposited with the CCDC.	2025-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                109.025(4)
_cell_angle_beta                 101.840(4)
_cell_angle_gamma                90.039(4)
_cell_formula_units_Z            4
_cell_length_a                   17.7840(16)
_cell_length_b                   21.250(2)
_cell_length_c                   25.315(3)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      54.23
_cell_measurement_theta_min      2.46
_cell_volume                     8828.2(16)
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0893
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_number            31807
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.402
_diffrn_reflns_theta_min         2.070
_diffrn_source_current           2.49
_diffrn_source_power             0.1739265
_diffrn_source_voltage           69.85
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.765
_exptl_absorpt_correction_T_max  0.1434
_exptl_absorpt_correction_T_min  0.0466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1015 before and 0.0635 after correction.
 
For component 2:
 wR2(int) was 0.1116 before and 0.0698 after correction.
 The Ratio of minimum to maximum transmission is 0.33.

Final HKLF 4 output contains 174678 reflections, Rint = 0.0930
 (74710 with I > 3sig(I), Rint = 0.0620)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       plate
_exptl_crystal_F_000             3556
_exptl_crystal_preparation       'Magnetic properties,Luminescent'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.767
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2095
_refine_ls_number_reflns         31807
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_gt           0.0800
_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^)+(0.0825P)^2^+70.2203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1940
_refine_ls_wR_factor_ref         0.2201
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22264
_reflns_number_total             31807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08731c2.cif
_cod_data_source_block           2351768
_cod_depositor_comments
'Adding full bibliography for 1574130--1574134.cif.'
_cod_original_cell_volume        8828.1(15)
_cod_database_code               1574132
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.647
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C197) \\sim Ueq, Uanis(C207) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C8(H8), C9(H9), C11(H11), C12(H12), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C24(H24), C26(H26), C27(H27), C31(H31),
  C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
 C40(H40), C41(H41), C42(H42), C46(H46), C48(H48), C50(H50), C52(H52), C53(H53),
  C55(H55), C56(H56), C59(H59), C61(H61), C62(H62), C63(H63), C64(H64),
 C65(H65), C66(H66), C67(H67), C68(H68), C69(H69), C71(H71), C72(H72), C73(H73),
  C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C79(H79), C84(H84),
 C85(H85), C86(H86), C87(H87), C88(H88), C89(H89), C93(H93), C94(H94), C96(H96),
  C98(H98), C102(H102), C104(H104), C105(H105), C106(H106), C107(H107),
 C108(H108), C111(H111), C112(H112), C113(H113), C115(H115), C116(H116),
 C117(H117), C118(H118), C120(H120), C121(H121), C123(H123), C124(H124),
 C125(H125), C127(H127), C128(H128), C130(H130), C131(H131), C132(H132),
 C133(H133), C134(H134), C135(H135), C136(H136), C137(H137), C140(H140),
 C141(H141), C142(H142), C143(H143), C144(H144), C145(H145), C147(H147),
 C149(H149), C150(H150), C152(H152), C153(H153), C155(H155), C156(H156),
 C157(H157), C158(H158), C160(H160), C162(H162), C163(H163), C164(H164),
 C165(H165), C166(H166), C167(H167), C168(H168), C169(H169), C170(H170),
 C172(H172), C173(H173), C174(H174), C176(H176), C178(H178), C181(H181),
 C182(H182), C186(H186), C187(H187), C188(H188), C190(H190), C192(H192),
 C194(H194), C196(H196), C198(H198), C200(H200), C202(H202), C204(H204),
 C206(H206), C208(H208), C210(H210), C5(H5), C21(H21), C179(H179), C183(H183),
 C195(H195), C13(H13), C47(H47), C51(H51), C103(H103), C205(H205), C57(H57),
 C151(H151), C171(H171), C177(H177), C185(H185), C25(H25), C99(H99), C189(H189),
  C193(H193), C203(H203), C43(H43), C83(H83), C91(H91), C95(H95), C161(H161),
 C197(H197), C199(H199), C201(H201), C207(H207), C209(H209)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C101(H10A,H10B,H10C), C81(H81A,H81B,H81C), C97(H97A,H97B,
 H97C), C191(H19A,H19B,H19C), C175(H17A,H17B,H17C)
;
_shelx_res_checksum              47459
_olex2_submission_special_instructions 'No special instructions were received'