Controlling topological diversity and magnetic properties in three Tb(iii) metal–organic frameworks through amide ligand variation
Huang, Long; Zhang, Qian; Zhang, Yang-Lu; Cai, Meng-Tan; Shi, Le; Yang, Jiong; Shao, Dong; CrystEngComm 27 (2025) 7228–7236; doi:10.1039/D5CE00881F

data_7250931
_publ_section_title
;
 Controlling topological diversity and magnetic properties in three
 Tb(iii) metal--organic frameworks through amide ligand variation
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              7228
_journal_page_last               7236
_journal_paper_doi               10.1039/D5CE00881F
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C32 H34 N2 O22 Tb2, 3(C4 H9 N O)'
_chemical_formula_sum            'C44 H61 N5 O25 Tb2'
_chemical_formula_weight         1377.844
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-30
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-08-01 deposited with the CCDC.	2025-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                94.384(3)
_cell_angle_beta                 106.455(3)
_cell_angle_gamma                110.710(3)
_cell_formula_units_Z            2
_cell_length_a                   11.2214(10)
_cell_length_b                   14.5112(11)
_cell_length_c                   18.8206(18)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    289(2)
_cell_measurement_theta_max      24.986
_cell_measurement_theta_min      2.301
_cell_volume                     2695.4(4)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      289(2)
_diffrn_detector                 'Bruker PHOTON-II area detector'
_diffrn_detector_area_resol_mean 7.4
_diffrn_detector_type            'CMOS-PHOTONII area detector'
_diffrn_measured_fraction_theta_full 0.9951
_diffrn_measured_fraction_theta_max 0.9951
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON-II area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0799
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.9951
_diffrn_reflns_Laue_measured_fraction_max 0.9951
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9539
_diffrn_reflns_point_group_measured_fraction_full 0.9951
_diffrn_reflns_point_group_measured_fraction_max 0.9951
_diffrn_reflns_theta_full        24.9986
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.03
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.690
_exptl_absorpt_correction_T_max  0.026123
_exptl_absorpt_correction_T_min  0.007842
_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 0.1710 before and 0.0933 after correction.
 The Ratio of minimum to maximum transmission is 0.30.

Final HKLF 4 output contains 101874 reflections, Rint = 0.1416
 (27843 with I > 3sig(I), Rint = 0.0799)
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1381.174
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.2196
_refine_diff_density_min         -2.1171
_refine_diff_density_rms         0.2556
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             10.0533
_refine_ls_goodness_of_fit_ref   1.0650
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    155
_refine_ls_number_parameters     1067
_refine_ls_number_reflns         9459
_refine_ls_number_restraints     1221
_refine_ls_restrained_S_all      0.9951
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0711
_refine_ls_shift/su_max          0.0051
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0865P)^2^+39.9858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1969
_refine_ls_wR_factor_ref         0.2037
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                7834
_reflns_number_total             9459
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5ce00881f2.cif
_cod_data_source_block           051604Tb
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7250929--7250931.cif.
;
_cod_database_code               7250931
_exptl_crystal_mounting_method
;
 Crystals were removed from the crystallisation vial and immediately coated
 with PDMS (polydimethylsiloxane/Dimethicone, CAS: 9006-65-9 on a glass slide.
 A suitable single crystal was selected and mounted on a glass fiber using
 vacuum silicone grease as adhesive. The glass fiber with single crystal was
 mounted on copper pin with solid paraffin. Operator: DJ_Tokyo.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C26-C25
 1.51 with sigma of 0.01
 N1-C28 = N1-C27
 1.45 with sigma of 0.01
 C34-C33
 1.51 with sigma of 0.01
 O24-C33
 1.21 with sigma of 0.01
 O26-C41
 1.21 with sigma of 0.01
 C26A-C25A
 1.51 with sigma of 0.01
 N4-C40 = N4-C39
 1.45 with sigma of 0.01
 C37-N4
 1.4 with sigma of 0.01
 O25-C37
 1.21 with sigma of 0.01
 C38-C37
 1.51 with sigma of 0.01
 C26-O21
 2.36 with sigma of 0.02
 O24-C34
 2.36 with sigma of 0.02
 C26A-O21
 2.36 with sigma of 0.02
 O25-C38
 2.36 with sigma of 0.02
 O25-N4
 2.262 with sigma of 0.02
 Tb1-H22b \\sim Tb1-H22a
 with sigma of 0.02
3. Restrained planarity
 N1A, C28A, C27A, C25A
 with sigma of 0.01
 C33A, N3A, C36A, C35A
 with sigma of 0.01
 C33A, C34A, O24A, N3A
 with sigma of 0.01
 C33A, O24A, C34A, N3A
 with sigma of 0.01
 C37, C38, N4, O25
 with sigma of 0.01
 C37A, O25A, C38A, N4A
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
O3 \\sim C3: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 2A
O21 \\sim N1 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim N1A \\sim C25A \\sim
C26A \\sim C27A \\sim C28A: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
O24 \\sim C33 \\sim N3 \\sim C34 \\sim C35 \\sim C36 \\sim C33A \\sim O24A
\\sim N3A \\sim C34A \\sim C35A \\sim C36A: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 2A
O16 \\sim N2 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim N2A \\sim C29A \\sim
C30A \\sim C31A \\sim C32A: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
O26 \\sim C41 \\sim N5 \\sim C42 \\sim C43 \\sim C44 \\sim O26A \\sim C41A
\\sim N5A \\sim C42A \\sim C43A \\sim C44A: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 2A
O25 \\sim C37 \\sim N4 \\sim C38 \\sim C39 \\sim C40 \\sim O25A \\sim C37A
\\sim N4A \\sim C38A \\sim C39A \\sim C40A: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 2A
5. Rigid body (RIGU) restrains
 O21, N1, C25, C26, C27, C28, N1A, C25A, C26A, C27A, C28A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 O24, C33, N3, C34, C35, C36, C34A, O24A, C33A, N3A, C35A, C36A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 O16, N2, C29, C30, C31, C32, N2A, C29A, C30A, C31A, C32A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 O26, C41, N5, C42, C43, C44, O26A, C41A, N5A, C42A, C43A, C44A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 C37, O25, N4, C38, C39, C40, O25A, C37A, N4A, C38A, C39A, C40A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{O21, N1A, C25A, C26A, C27A, C28A} sigma for 1-2: 0.01, 1-3: 0.04
as in
{O21, N1, C25, C26, C27, C28}
{O24A, N3A, C33A, C34A, C35A, C36A} sigma for 1-2: 0.01, 1-3: 0.04
as in
{O24, N3, C33, C34, C35, C36}
{O16, N2A, C29A, C30A, C31A, C32A} sigma for 1-2: 0.01, 1-3: 0.04
as in
{O16, N2, C29, C30, C31, C32}
{O26A, N5A, C41A, C42A, C43A, C44A} sigma for 1-2: 0.01, 1-3: 0.04
as in
{O26, N5, C41, C42, C43, C44}
{O25A, N4A, C37A, C38A, C39A, C40A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{O25, N4, C37, C38, C39, C40}
7. Others
 Sof(N1A)=Sof(C25A)=Sof(C26A)=Sof(H26d)=Sof(H26e)=Sof(H26f)=Sof(C27A)=
 Sof(H27d)=Sof(H27e)=Sof(H27f)=Sof(C28A)=Sof(H28d)=Sof(H28e)=Sof(H28f)=
 Sof(H26d)=Sof(H26e)=Sof(H26f)=1-FVAR(1)
 Sof(N1)=Sof(C25)=Sof(C26)=Sof(H26a)=Sof(H26b)=Sof(H26c)=Sof(C27)=Sof(H27a)=
 Sof(H27b)=Sof(H27c)=Sof(C28)=Sof(H28a)=Sof(H28b)=Sof(H28c)=FVAR(1)
 Sof(O24A)=Sof(N3A)=Sof(C33A)=Sof(C34A)=Sof(H34d)=Sof(H34e)=Sof(H34f)=
 Sof(C35A)=Sof(H35d)=Sof(H35e)=Sof(H35f)=Sof(C36A)=Sof(H36d)=Sof(H36e)=
 Sof(H36f)=1-FVAR(2)
 Sof(O24)=Sof(N3)=Sof(C33)=Sof(C34)=Sof(H34a)=Sof(H34b)=Sof(H34c)=Sof(C35)=
 Sof(H35a)=Sof(H35b)=Sof(H35c)=Sof(C36)=Sof(H36a)=Sof(H36b)=Sof(H36c)=FVAR(2)
 Sof(N2A)=Sof(C29A)=Sof(C30A)=Sof(H30d)=Sof(H30e)=Sof(H30f)=Sof(C31A)=
 Sof(H31d)=Sof(H31e)=Sof(H31f)=Sof(C32A)=Sof(H32d)=Sof(H32e)=Sof(H32f)=1-FVAR(3)
 Sof(N2)=Sof(C29)=Sof(C30)=Sof(H30a)=Sof(H30b)=Sof(H30c)=Sof(C31)=Sof(H31a)=
 Sof(H31b)=Sof(H31c)=Sof(C32)=Sof(H32a)=Sof(H32b)=Sof(H32c)=FVAR(3)
 Sof(O25A)=Sof(N4A)=Sof(C37A)=Sof(C38A)=Sof(H38d)=Sof(H38e)=Sof(H38f)=
 Sof(C39A)=Sof(H39d)=Sof(H39e)=Sof(H39f)=Sof(C40A)=Sof(H40d)=Sof(H40e)=
 Sof(H40f)=1-FVAR(4)
 Sof(O25)=Sof(N4)=Sof(C37)=Sof(C38)=Sof(H38a)=Sof(H38b)=Sof(H38c)=Sof(C39)=
 Sof(H39a)=Sof(H39b)=Sof(H39c)=Sof(C40)=Sof(H40a)=Sof(H40b)=Sof(H40c)=FVAR(4)
 Sof(O26A)=Sof(N5A)=Sof(C41A)=Sof(C42A)=Sof(H42d)=Sof(H42e)=Sof(H42f)=
 Sof(C43A)=Sof(H43d)=Sof(H43e)=Sof(H43f)=Sof(C44A)=Sof(H44d)=Sof(H44e)=
 Sof(H44f)=1-FVAR(5)
 Sof(O26)=Sof(N5)=Sof(C41)=Sof(C42)=Sof(H42a)=Sof(H42b)=Sof(H42c)=Sof(C43)=
 Sof(H43a)=Sof(H43b)=Sof(H43c)=Sof(C44)=Sof(H44a)=Sof(H44b)=Sof(H44c)=FVAR(5)
8.a Riding coordinates:
 O9(H9), O22(H22a,H22b), O23(H23a,H23b), O3(H3), O20(H20), O10(H10), C26(H26a,
 H26b,H26c), C27(H27a,H27b,H27c), C28(H28a,H28b,H28c), C27A(H27d,H27e,H27f),
 C28A(H28d,H28e,H28f), C34(H34a,H34b,H34c), C35(H35a,H35b,H35c), C36(H36a,H36b,
 H36c), C34A(H34d,H34e,H34f), C35A(H35d,H35e,H35f), C36A(H36d,H36e,H36f),
 O6(H6), O15(H15), C30(H30a,H30b,H30c), C31(H31a,H31b,H31c), C32(H32a,H32b,
 H32c), C30A(H30d,H30e,H30f), C31A(H31d,H31e,H31f), C32A(H32d,H32e,H32f),
 C42(H42a,H42b,H42c), C43(H43a,H43b,H43c), C44(H44a,H44b,H44c), C42A(H42d,H42e,
 H42f), C43A(H43d,H43e,H43f), C44A(H44d,H44e,H44f), C26A(H26f,H26e,H26d),
 C38(H38a,H38b,H38c), C39(H39a,H39b,H39c), C40(H40a,H40b,H40c), C38A(H38d,H38e,
 H38f), C39A(H39d,H39e,H39f), C40A(H40d,H40e,H40f)
8.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C8(H8), C12(H12), C15(H15a), C20(H20a), C23(H23)
;
_olex2_submission_special_instructions 'No special instructions were received'