Reversible single-crystal-to-single-crystal transition in Gd(III) metal-organic frameworks induced by heat and solvents with a significant magnetocaloric effect.
Wang, Jin-Jin; Li, Yu; Zheng, Teng-Fei; Peng, Yan; Chen, Jing-Lin; Liu, Sui-Jun; Wen, He-Rui; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5601–5607; doi:10.1039/d3dt03867j

data_7715173
_publ_section_title
;
 Reversible single-crystal-to-single-crystal transition in Gd(III)
 metal-organic frameworks induced by heat and solvents with a significant
 magnetocaloric effect.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5601
_journal_page_last               5607
_journal_paper_doi               10.1039/d3dt03867j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C66 H30 Dy4 N6 O28 S3, 6[H2O]'
_chemical_formula_sum            'C66 H42 Dy4 N6 O34 S3'
_chemical_formula_weight         2209.27
_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
_audit_creation_date             2024-01-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-16 deposited with the CCDC.	2024-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                104.902(4)
_cell_angle_beta                 109.430(3)
_cell_angle_gamma                90.228(4)
_cell_formula_units_Z            1
_cell_length_a                   10.9980(12)
_cell_length_b                   11.1805(13)
_cell_length_c                   15.8136(17)
_cell_measurement_reflns_used    9324
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      55.023
_cell_measurement_theta_min      5.714
_cell_volume                     1763.5(3)
_computing_cell_refinement       'SAINT V8.38A (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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0615
_diffrn_reflns_av_unetI/netI     0.0757
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18642
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.006
_diffrn_reflns_theta_max         25.006
_diffrn_reflns_theta_min         2.845
_exptl_absorpt_coefficient_mu    4.378
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1313 before and 0.0659 after correction.
The Ratio of minimum to maximum transmission is 0.5951.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.080
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.787
_refine_diff_density_min         -1.462
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         6110
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_gt           0.0629
_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^)+(0.0300P)^2^+48.3742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1511
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4166
_reflns_number_total             6110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03867j2.cif
_cod_data_source_block           JXUST-41a
_cod_depositor_comments
'Adding full bibliography for 7715168--7715173.cif.'
_cod_database_code               7715173
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O1W-O2W
 4.2 with sigma of 0.01
 O1W-Dy2
 2.2 with sigma of 0.01
 O1-H1WB
 2.12 with sigma of 0.01
 H2WB-O5_$1
 2.034 with sigma of 0.01
 H1WB-O1
 2.101 with sigma of 0.01
 H1WA-O4_$2
 2.15 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(C8) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: S2(0.5) N4(0.5) N3(0.5)
5.a Riding coordinates:
 O1W(H1WA,H1WB)
5.b Rotating group:
 O2W(H2WA,H2WB)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C8(H8), C13(H13), C14(H14), C16(H16), C18(H18), C20(H20),
 C26(H26), C28(H28), C30(H30)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 66 electrons were 
found in a volume of 288\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
6[H2O] per Unit Cell 
which account for 60 electrons 
per unit cell.
;
_shelx_res_checksum              73590
_shelx_fab_checksum              66323
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'