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_1574130
_publ_section_title
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 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         'C82 H68 N2 O4 Si4 Tb, 2.5(C7 H8)'
_chemical_formula_sum            'C99.5 H88 N2 O4 Si4 Tb'
_chemical_formula_weight         1646.99
_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
_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                93.487(3)
_cell_angle_beta                 110.590(3)
_cell_angle_gamma                109.064(4)
_cell_formula_units_Z            4
_cell_length_a                   17.3266(11)
_cell_length_b                   23.1849(15)
_cell_length_c                   24.3639(14)
_cell_measurement_reflns_used    9162
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      58.55
_cell_measurement_theta_min      2.45
_cell_volume                     8487.2(10)
_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 2019/2 (Sheldrick, 2015)'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.1129
_diffrn_reflns_av_unetI/netI     0.1133
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            168101
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        52.981
_diffrn_reflns_theta_max         52.981
_diffrn_reflns_theta_min         1.719
_diffrn_source                   'microfocus Metaljet'
_diffrn_source_type              'Incoatec Metaljet'
_exptl_absorpt_coefficient_mu    4.941
_exptl_absorpt_correction_T_max  0.0998
_exptl_absorpt_correction_T_min  0.0178
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1336 before and 0.0936 after correction.
The Ratio of minimum to maximum transmission is 0.3030.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       needle
_exptl_crystal_F_000             3408
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.004
_refine_diff_density_min         -1.068
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.00025(4)
_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   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1660
_refine_ls_number_reflns         30012
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0635
_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^)+(0.0426P)^2^+8.0681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1621
_refine_ls_wR_factor_ref         0.1767
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21137
_reflns_number_total             30012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08731c2.cif
_cod_data_source_block           20221020_1013_2b_4bpy_0m
_cod_depositor_comments
'Adding full bibliography for 1574130--1574134.cif.'
_cod_original_cell_volume        8487.2(9)
_cod_original_formula_sum        'C99.50 H88 N2 O4 Si4 Tb'
_cod_database_code               1574130
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.866
_olex2_refinement_description
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1. Uiso/Uaniso restraints and constraints
C168 \\sim C169 \\sim C170 \\sim C171 \\sim C166 \\sim C167: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
C183 \\sim C184 \\sim C185 \\sim C180 \\sim C181 \\sim C182 \\sim C179: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
Uanis(C183) \\sim Ueq, Uanis(C184) \\sim Ueq, Uanis(C185) \\sim Ueq,
Uanis(C180) \\sim Ueq, Uanis(C179) \\sim Ueq, Uanis(C181) \\sim Ueq,
Uanis(C182) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C183) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C150) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C67)
\\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C199) \\sim Ueq, Uanis(C68) \\sim Ueq,
Uanis(C73) \\sim Ueq, Uanis(C190) \\sim Ueq, Uanis(C189) \\sim Ueq, Uanis(C183)
\\sim Ueq, Uanis(C165) \\sim Ueq, Uanis(C92) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
2.a Aromatic/amide H refined with riding coordinates:
 C124(H124), C125(H125), C126(H126), C127(H127), C128(H128), C110(H110),
 C109(H109), C108(H108), C107(H107), C106(H106), C134(H134), C133(H133),
 C132(H132), C131(H131), C130(H130), C11(H11), C136(H136), C137(H137),
 C138(H138), C139(H139), C140(H140), C18(H18), C4(H4), C14(H14), C118(H118),
 C119(H119), C120(H120), C121(H121), C122(H122), C17(H17), C13(H13), C9(H9),
 C100(H100), C101(H101), C102(H102), C103(H103), C104(H104), C46(H46), C47(H47),
  C48(H48), C49(H49), C50(H50), C8(H8), C82(H82), C83(H83), C84(H84), C85(H85),
 C86(H86), C20(H20), C2(H2), C116(H116), C115(H115), C114(H114), C113(H113),
 C112(H112), C154(H154), C155(H155), C156(H156), C157(H157), C158(H158),
 C19(H19), C146(H146), C145(H145), C144(H144), C143(H143), C142(H142), C10(H10),
  C164(H164), C163(H163), C162(H162), C161(H161), C160(H160), C7(H7), C40(H40),
 C41(H41), C42(H42), C43(H43), C44(H44), C12(H12), C38(H38), C34(H34), C35(H35),
  C36(H36), C37(H37), C148(H148), C149(H149), C150(H150), C151(H151),
 C152(H152), C62(H62), C61(H61), C60(H60), C59(H59), C58(H58), C88(H88),
 C89(H89), C90(H90), C91(H91), C92(H92), C80(H80), C79(H79), C78(H78), C77(H77),
  C76(H76), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C3(H3), C56(H56),
 C55(H55), C54(H54), C53(H53), C52(H52), C1(H1), C98(H98), C97(H97), C96(H96),
 C95(H95), C94(H94), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C23(H23),
  C24(H24), C25(H25), C26(H26), C22(H22), C74(H74), C73(H73), C72(H72),
 C71(H71), C70(H70), C174(H174), C175(H175), C199(H199), C191(H191), C188(H188),
  C189(H189), C190(H190), C177(H177), C178(H178), C181(H181), C182(H182),
 C183(H183), C184(H184), C185(H185), C176(H176), C171(H171), C170(H170),
 C169(H169), C168(H168), C167(H167), C197(H197), C193(H193), C194(H194),
 C195(H195), C196(H196)
2.b Fitted hexagon refined as free rotating group:
 C123(C124,C125,C126,C127,C128), C105(C110,C109,C108,C107,C106), C129(C134,
 C133,C132,C131,C130), C135(C136,C137,C138,C139,C140), C117(C118,C119,C120,C121,
 C122), C99(C100,C101,C102,C103,C104), C45(C46,C47,C48,C49,C50), C81(C82,C83,
 C84,C85,C86), C111(C116,C115,C114,C113,C112), C153(C154,C155,C156,C157,C158),
 C141(C146,C145,C144,C143,C142), C159(C164,C163,C162,C161,C160), C39(C40,C41,
 C42,C43,C44), C38(C33,C34,C35,C36,C37), C147(C148,C149,C150,C151,C152),
 C57(C62,C61,C60,C59,C58), C87(C88,C89,C90,C91,C92), C75(C80,C79,C78,C77,C76),
 C28(C29,C30,C31,C32,C27), C51(C56,C55,C54,C53,C52), C93(C98,C97,C96,C95,C94),
 C63(C64,C65,C66,C67,C68), C23(C24,C25,C26,C21,C22), C69(C74,C73,C72,C71,C70),
 C199(C191,C187,C188,C189,C190), C181(C182,C183,C184,C185,C180), C171(C170,C169,
 C168,C167,C166), C197(C192,C193,C194,C195,C196)
2.c Idealised Me refined as rotating group:
 C172(H17A,H17B,H17C), C198(H19A,H19B,H19C), C186(H18A,H18B,H18C), C165(H16A,
 H16B,H16C), C179(H17D,H17E,H17F)
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_shelx_res_checksum              44816
_olex2_submission_special_instructions 'No special instructions were received'