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_7250930
_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         'C22 H28 N2 O11 Tb, 1.7[H2O]'
_chemical_formula_sum            'C22 H31.4 N2 O12.7 Tb'
_chemical_formula_weight         686.01
_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   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-07-31
_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                90
_cell_angle_beta                 99.577(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.737(8)
_cell_length_b                   10.588(3)
_cell_length_c                   22.263(6)
_cell_measurement_reflns_used    9579
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.33
_cell_measurement_theta_min      2.57
_cell_volume                     6447(3)
_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  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298(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 0.998
_diffrn_measured_fraction_theta_max 0.993
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1116
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            60341
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.587
_diffrn_reflns_theta_min         2.210
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.249
_exptl_absorpt_correction_type   none
_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    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.639
_refine_diff_density_min         -1.394
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         7424
_refine_ls_number_restraints     372
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0652
_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^)+(0.0558P)^2^+62.0918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1589
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6221
_reflns_number_total             7424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00881f2.cif
_cod_data_source_block           a_a_CCDC1
_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_original_formula_sum        'C22 H31.40 N2 O12.70 Tb'
_cod_database_code               7250930
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.806
_shelx_estimated_absorpt_t_min   0.759
_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, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O11-C18 = O10-C13
 1.2164 with sigma of 0.01
 N2-C18 = N1-C13
 1.3625 with sigma of 0.01
 N1-C14 = N2-C19
 1.4503 with sigma of 0.01
 C21-C22 = C19-C20 = C16-C17 = C14-C15
 1.54 with sigma of 0.01
 N1-C16 = N2-C19
 1.4533 with sigma of 0.01
 C13-C16 = C18-C21
 2.4456 with sigma of 0.02
 C16-C14 = C19-C21
 2.4848 with sigma of 0.02
 C13-C14 = C18-C19
 2.4578 with sigma of 0.02
 C16-O10 = C21-O11
 2.828 with sigma of 0.02
 N1-C15 = N2-C20
 2.442 with sigma of 0.02
 N1-C17 = N2-C22
 2.442 with sigma of 0.02
 N1-O10 = O11-N2
 2.2984 with sigma of 0.02
3. Restrained planarity
 N1, C13, C14, C16
 with sigma of 0.01
 N2, C18, C19, C21
 with sigma of 0.01
 C18A, N2A, C21A, C19A
 with sigma of 0.01
 C13A, N1A, C14A, C16A
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
O11 \\sim N2 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim N2A \\sim
C18A \\sim C19A \\sim C20A \\sim C21A \\sim C22A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
O10 \\sim N1 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim N1A \\sim
C13A \\sim C14A \\sim C15A \\sim C16A \\sim C17A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
5. Same fragment restrains
{O10, N1A, C13A, C14A, C15A, C16A, C17A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{O10, N1, C13, C14, C15, C16, C17}
{O11, N2A, C18A, C19A, C20A, C21A, C22A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{O11, N2, C18, C19, C20, C21, C22}
6. Others
 Sof(N1A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14C)=Sof(H14D)=Sof(C15A)=
 Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16A)=Sof(H16C)=Sof(H16D)=Sof(C17A)=
 Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(N1)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C15)=Sof(H15A)=
 Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(C17)=Sof(H17A)=Sof(H17B)=
 Sof(H17C)=FVAR(1)
 Sof(N2A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19C)=Sof(H19D)=Sof(C20A)=
 Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(C22A)=
 Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(2)
 Sof(N2)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=
 Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=
 Sof(H22C)=FVAR(2)
7.a Riding coordinates:
 O3(H3), O6(H6), O9(H9), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C15A(H15D,
 H15E,H15F)
7.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C16(H16A,H16B), C19(H19A,H19B), C21(H21A,H21B), C14A(H14C,
 H14D), C16A(H16C,H16D), C19A(H19C,H19D), C21A(H21C,H21D)
7.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C18(H18), C4(H4), C7(H7), C12(H12), C13A(H13A), C18A(H18A)
7.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C17A(H17D,H17E,H17F), C20A(H20D,
 H20E,H20F), C22A(H22D,H22E,H22F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 136 electrons were 
found in a volume of 1140\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.7[H2O] per Asymmetric Unit 
which account for 136 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              39094
_shelx_fab_checksum              701
_olex2_submission_special_instructions 'No special instructions were received'