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_7715168
_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         'C78 H52 Gd4 N10 O28 S3'
_chemical_formula_sum            'C78 H52 Gd4 N10 O28 S3'
_chemical_formula_weight         2302.47
_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   geom
_audit_creation_date             2024-02-04
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-07 deposited with the CCDC.	2024-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                73.776(2)
_cell_angle_beta                 70.816(2)
_cell_angle_gamma                86.974(2)
_cell_formula_units_Z            1
_cell_length_a                   10.9770(6)
_cell_length_b                   11.9536(7)
_cell_length_c                   15.8824(10)
_cell_measurement_reflns_used    6921
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      54.958
_cell_measurement_theta_min      5.658
_cell_volume                     1888.14(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      273.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0538
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_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       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23531
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         2.981
_exptl_absorpt_coefficient_mu    3.645
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0769 before and 0.0536 after correction.
The Ratio of minimum to maximum transmission is 0.8625.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.025
_exptl_crystal_description       block
_exptl_crystal_F_000             1118
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.148
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         6575
_refine_ls_number_restraints     640
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+3.2626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0735
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4871
_reflns_number_total             6575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03867j2.cif
_cod_data_source_block           JXUST-40
_cod_depositor_comments
'Adding full bibliography for 7715168--7715173.cif.'
_cod_database_code               7715168
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details   SADABS
_olex2_refinement_description
;
1. Restrained distances
 N7-C33 = N3-C1I
 1.345 with sigma of 0.01
 S2-N7 = S2-N3
 1.6 with sigma of 0.01
 O6-C21 \\sim O6A-C21 \\sim O5A-C21 \\sim O5-C21
 with sigma of 0.02
 C1F-C1J \\sim C1J-C1H
 with sigma of 0.02
 O14-C37 \\sim O14-C37A
 with sigma of 0.02
 N4-C37 \\sim N4A-C37A
 with sigma of 0.02
 C37-C38 \\sim C37A-C38A
 with sigma of 0.04
 O5-O6 \\sim O5A-O6A
 with sigma of 0.02
 O16-C1A \\sim O15-C1A
 with sigma of 0.02
 C37-C39 \\sim C37A-C39A
 with sigma of 0.04
 N4-C38 \\sim N4A-C38A
 with sigma of 0.02
 N4-C39 \\sim N4A-C39A
 with sigma of 0.02
 O14-N4 \\sim O14-N4A
 with sigma of 0.04
 Gd1-O11 \\sim Gd1A-O11
 with sigma of 0.02
 C38-C39 \\sim C38A-C39A
 with sigma of 0.04
 C28-C32 \\sim C32-C30
 with sigma of 0.02
 C33-S2 \\sim S2-C1I
 with sigma of 0.02
 Gd1-O1 \\sim Gd1A-O1
 with sigma of 0.02
 Gd1-O12 \\sim Gd1A-O12
 with sigma of 0.02
 Gd1-O14 \\sim Gd1A-O14
 with sigma of 0.02
 O12_$3-C1B \\sim O17-C1B
 with sigma of 0.02
 C35-C36 \\sim C35A-C36A
 with sigma of 0.02
 N5-C35 \\sim N5-C35A \\sim N5-C36A \\sim N5-C36
 with sigma of 0.02
2. Restrained planarity
 O14, C37A, N4A, C38A, C39A
 with sigma of 0.1
 C37, O14, N4, C38, C39
 with sigma of 0.1
 C33, N7, S2, N3, C1I
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C1G \\sim C1J \\sim C1I \\sim C33 \\sim C32 \\sim C31 \\sim C1K \\sim C29 \\sim
C30 \\sim C25 \\sim C24 \\sim C26 \\sim C27 \\sim C28 \\sim C23 \\sim O10 \\sim
O9 \\sim O11 \\sim C1A \\sim O15 \\sim O16 \\sim C1F \\sim C1E \\sim C7 \\sim
C1D \\sim C1C \\sim C1H \\sim C1B: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
O15 \\sim C1A: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
N4 \\sim C37 \\sim C38 \\sim C39 \\sim N4A \\sim C37A \\sim C38A \\sim C39A:
within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004 within 2A
C30 \\sim C28 \\sim C27 \\sim C25 \\sim C29 \\sim C26: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002 within 2A
O11 \\sim C24: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
C1J \\sim C31 \\sim C1I \\sim C1K \\sim C33: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
Gd1 \\sim Gd1A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C34 \\sim N5 \\sim C35 \\sim C35A \\sim C36A \\sim C36: within 3A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 3A
C21 \\sim O6A \\sim O6 \\sim O5A \\sim O5: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Uanis(O15) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(C1E)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1E) \\sim Ueq, Uanis(C1D) \\sim Ueq, Uanis(C1C) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C1E) \\sim Ueq, Uanis(C1C) \\sim Ueq, Uanis(C1H) \\sim Ueq, Uanis(C1F)
\\sim Ueq, Uanis(C1D) \\sim Ueq, Uanis(C1G) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(N4) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(N4A) \\sim Ueq, Uanis(C37A) \\sim Ueq, Uanis(C38A) \\sim Ueq,
Uanis(C39A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C1I) \\sim Ueq, Uanis(C1J)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C32) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C22) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C4) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C35) \\sim Ueq, Uanis(C35A) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C36A)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C32) = Uanis(C29)
Uanis(C36) = Uanis(C36A)
Uanis(C35) = Uanis(C35A)
Uanis(C1B) = Uanis(C24)
Uanis(Gd1) = Uanis(Gd1A)
Uanis(O17) = Uanis(O11)
Uanis(C1E) = Uanis(C1B)
4. Others
 Sof(Gd1A)=1-FVAR(1)
 Sof(Gd1)=FVAR(1)
 Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C36A)=Sof(H36D)=Sof(H36E)=
 Sof(H36F)=1-FVAR(2)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=
 FVAR(2)
 Sof(O6A)=Sof(O5A)=1-FVAR(3)
 Sof(O5)=Sof(O6)=FVAR(3)
 Sof(N4A)=Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=
 Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=1-FVAR(4)
 Sof(N4)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=
 Sof(H39A)=Sof(H39B)=Sof(H39C)=FVAR(4)
 Fixed Sof: O9(0.5) O10(0.5) O11(0.5) C23(0.5) C24(0.5) C26(0.5) H26(0.5)
 C27(0.5) C28(0.5) H28(0.5) C29(0.5) C30(0.5) H30(0.5) C25(0.5) C32(0.5)
 C31(0.5) H31(0.5) C1K(0.5) H1K(0.5) C1J(0.5) C1I(0.5) C33(0.5) S2(0.5)
 O15(0.5) O16(0.5) O17(0.5) N3(0.5) N7(0.5) C1A(0.5) C1B(0.5) C1G(0.5) C1H(0.5)
 H1H(0.5) C1C(0.5) C1D(0.5) H1D(0.5) C1E(0.5) C1F(0.5) H1F(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C8(H8), C10(H10), C11(H11), C16(H16), C18(H18), C20(H20),
 C26(H26), C28(H28), C30(H30), C31(H31), C1K(H1K), C34(H34), C1H(H1H), C1D(H1D),
  C1F(H1F), C37(H37), C37A(H37A)
5.b Fitted hexagon refined as free rotating group:
 C26(C27,C28,C29,C30,C25), C32(C31,C1K,C1J,C1I,C33), C1G(C1H,C1C,C1D,C1E,C1F)
5.c Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C35A(H35D,H35E,H35F), C36A(H36D,
 H36E,H36F), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C38A(H38D,H38E,H38F),
 C39A(H39D,H39E,H39F)
;
_shelx_res_checksum              53897
_olex2_submission_special_instructions 'No special instructions were received'