Highly proton-conducting lanthanide metal–organic frameworks featuring highly oxygenated ligands with slow magnetic relaxation or magnetocaloric effect
Yang, Shun-Yi; Zhang, Qian; Zhang, Yang-Lu; Tan, Tie-Shen; Zhu, Junlun; Yang, Xiaodong; Shi, Le; Yang, Jiong; Shao, Dong; CrystEngComm 26 (2024) 4181–4189; doi:10.1039/D4CE00501E

data_7248921
_publ_section_title
;
 Highly proton-conducting lanthanide metal--organic frameworks featuring
 highly oxygenated ligands with slow magnetic relaxation or magnetocaloric
 effect
;
_journal_issue                   31
_journal_name_full               CrystEngComm
_journal_page_first              4181
_journal_page_last               4189
_journal_paper_doi               10.1039/D4CE00501E
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C12 H12 O12 Tb'
_chemical_formula_sum            'C12 H12 O12 Tb'
_chemical_formula_weight         507.14
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-01-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-17 deposited with the CCDC.	2024-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                85.893(5)
_cell_angle_beta                 76.937(5)
_cell_angle_gamma                63.663(5)
_cell_formula_units_Z            2
_cell_length_a                   10.3636(17)
_cell_length_b                   11.0274(16)
_cell_length_c                   11.1750(17)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    304.00
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.67
_cell_volume                     1114.3(3)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      304.00
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32186
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.537
_diffrn_reflns_theta_min         2.062
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.219
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_correction_T_min  0.240
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       block
_exptl_crystal_F_000             490
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         5091
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0184
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0179P)^2^+0.5155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0443
_refine_ls_wR_factor_ref         0.0448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4776
_reflns_number_total             5091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00501e2.cif
_cod_data_source_block           Tb
_cod_depositor_comments
'Adding full bibliography for 7248921--7248922.cif.'
_cod_database_code               7248921
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.661
_shelx_estimated_absorpt_t_min   0.390
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 Tb1-H7A \\sim Tb1-H7B
 with sigma of 0.02
 Tb1-H9A \\sim Tb1-H9B
 with sigma of 0.02
 Tb1-H12A \\sim Tb1-H12B
 with sigma of 0.02
3.a Free rotating group:
 O7(H7A,H7B), O9(H9A,H9B), O12(H12A,H12B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C5(H5A)
3.c Idealised tetrahedral OH refined as rotating group:
 O2(H2), O5(H5), O18(H18)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              85482
_shelx_fab_checksum              50286
_olex2_submission_special_instructions 'No special instructions were received'