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_7715172
_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 Gd4 N6 O28 S3, 6[H2O]'
_chemical_formula_sum            'C66 H42 Gd4 N6 O34 S3'
_chemical_formula_weight         2188.23
_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             2024-01-05
_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                104.973(3)
_cell_angle_beta                 109.460(3)
_cell_angle_gamma                90.221(3)
_cell_formula_units_Z            1
_cell_length_a                   11.0108(10)
_cell_length_b                   11.1168(10)
_cell_length_c                   15.8231(14)
_cell_measurement_reflns_used    6467
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      54.975
_cell_measurement_theta_min      5.706
_cell_volume                     1755.6(3)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0685
_diffrn_reflns_av_unetI/netI     0.0969
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_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            19408
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.890
_exptl_absorpt_coefficient_mu    3.919
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5291
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.070
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.857
_refine_diff_density_min         -1.237
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         6112
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0616
_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^)+(0.0801P)^2^+0.6009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1572
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3921
_reflns_number_total             6112
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03867j2.cif
_cod_data_source_block           JXUST-40a
_cod_depositor_comments
'Adding full bibliography for 7715168--7715173.cif.'
_cod_database_code               7715172
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 Gd1-O1W
 2.26 with sigma of 0.01
 H1WA-H1WB
 1.5 with sigma of 0.01
 H1WB-O9
 2.145 with sigma of 0.01
 Gd2-O2W
 2.25 with sigma of 0.01
 H2WA-O8_$1
 2.1 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: S1(0.5) N3(0.5) N4(0.5)
4.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C4(H4), C11(H11), C12(H12), C20(H20), C16(H16), C18(H18),
 C26(H26), C28(H28), C30(H30)
4.c Fitted hexagon refined as free rotating group:
 C5(C6,C7,C8,C3,C4), C20(C15,C16,C17,C18,C19)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 54 electrons were 
found in a volume of 283\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
6[H2O] per Asymmetric Unit 
which account for 60 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              44739
_shelx_fab_checksum              58426
_olex2_submission_special_instructions 'No special instructions were received'