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_7715170
_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             2024-02-05
_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                73.676(2)
_cell_angle_beta                 71.786(2)
_cell_angle_gamma                86.984(2)
_cell_formula_units_Z            1
_cell_length_a                   10.9670(6)
_cell_length_b                   11.1536(7)
_cell_length_c                   15.9824(10)
_cell_measurement_reflns_used    6921
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.83
_cell_volume                     1780.84(19)
_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 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0514
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_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       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22729
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.984
_exptl_absorpt_coefficient_mu    3.865
_exptl_absorpt_correction_T_max  0.7312
_exptl_absorpt_correction_T_min  0.6131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0769 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    2.147
_exptl_crystal_description       block
_exptl_crystal_F_000             1118
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.903
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         6234
_refine_ls_number_restraints     438
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0197P)^2^+4.5315P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0691
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4738
_reflns_number_total             6234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03867j2.cif
_cod_data_source_block           JXUST-40b
_cod_depositor_comments
'Adding full bibliography for 7715168--7715173.cif.'
_cod_original_cell_volume        1780.85(19)
_cod_database_code               7715170
_shelx_shelxl_version_number     2019/2
_olex2_refinement_description
;
1. Restrained distances
 O2-C23
 1.2 with sigma of 0.01
 C31-C2
 1.39 with sigma of 0.01
 S1-N4 = N4-C28 = C28-C26 = C26-N1 = N1-S1
 1.39 with sigma of 0.01
 C35-C29 \\sim C52-C31
 with sigma of 0.02
 C17-C3 \\sim C13-C2
 with sigma of 0.02
 O13-C5 \\sim O13-C43
 with sigma of 0.02
 C39-N7 \\sim C21-N2
 with sigma of 0.02
 O13-N7 \\sim O13-N2
 with sigma of 0.04
 C39-C5 \\sim C21-C43
 with sigma of 0.04
 C39-C41 \\sim C21-C11
 with sigma of 0.04
 C5-C41 \\sim C43-C11
 with sigma of 0.04
 O13-C43 \\sim O13-C5
 with sigma of 0.02
 N7-C5 \\sim N2-C43
 with sigma of 0.02
 N7-C39 \\sim N2-C21
 with sigma of 0.02
 N7-C41 \\sim N2-C11
 with sigma of 0.02
 Gd2-O6 \\sim Gd2-O4
 with sigma of 0.02
 O14B-C44 \\sim O14A-C44
 with sigma of 0.02
2. Restrained planarity
 S1, N4, C28, C26, N1
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
O16 \\sim C46: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
C2 \\sim C15 \\sim C31: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Gd1 \\sim Gd1A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
O13 \\sim C39 \\sim N7 \\sim C5 \\sim C41 \\sim C21 \\sim N2 \\sim C43 \\sim
C11: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C50 \\sim C49 \\sim C51 \\sim C17 \\sim C31 \\sim C15 \\sim C47 \\sim C53 \\sim
C52 \\sim C2 \\sim C7 \\sim C27 \\sim C13 \\sim C35 \\sim C3 \\sim C29 \\sim
C25 \\sim C33: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
C45: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004 within
2A
C44 \\sim O14B \\sim O14A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(C48) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O16)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O7) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O16) \\sim Ueq, Uanis(C46) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C5) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(C41) \\sim Ueq: with sigma of 0.05 and sigma for terminal
atoms of 0.01
Uanis(C5) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C41)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C43) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C21)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C13) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C51)
\\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C25) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C45) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C7) = Uanis(C48)
Uanis(C45) = Uanis(C49)
Uanis(C46) = Uanis(C53)
4. Rigid body (RIGU) restrains
 C2, C15, C31
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(Gd1A)=1-FVAR(1)
 Sof(Gd1)=FVAR(1)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(N2)=Sof(C43)=Sof(H43)=Sof(C11)=
 Sof(H11A)=Sof(H11B)=Sof(H11C)=1-FVAR(2)
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(N7)=Sof(C5)=Sof(H5)=Sof(C41)=
 Sof(H41A)=Sof(H41B)=Sof(H41C)=FVAR(2)
 Sof(O14B)=1-FVAR(3)
 Sof(O14A)=FVAR(3)
 Fixed Sof: O16(0.5) O17(0.5) O9(0.5) C46(0.5) C48(0.5) C50(0.5) C52(0.5)
 H52(0.5) C53(0.5) C27(0.5) H27(0.5) C7(0.5) C29(0.5) H29(0.5) C15(0.5)
 C31(0.5) H31(0.5) C2(0.5) H2(0.5) C33(0.5) C17(0.5) C35(0.5) S2(0.5) O7(0.5)
 O15(0.5) O2(0.5) N5(0.5) N3(0.5) C45(0.5) C23(0.5) C47(0.5) C3(0.5) H3(0.5)
 C49(0.5) C25(0.5) H25(0.5) C51(0.5) C13(0.5) H13(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C12(H12), C16(H16), C20(H20), C22(H22), C32(H32), C36(H36), C40(H40),
 C52(H52), C27(H27), C29(H29), C31(H31), C2(H2), C9(H9), C5(H5), C43(H43),
 C3(H3), C25(H25), C13(H13)
6.b Fitted hexagon refined as free rotating group:
 C50(C52,C53,C27,C7,C29), C15(C31,C2,C33,C17,C35), C47(C3,C49,C25,C51,C13)
6.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C19(H19A,H19B,H19C), C39(H39A,H39B,H39C), C41(H41A,H41B,
 H41C), C21(H21A,H21B,H21C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              8861
_olex2_submission_special_instructions 'No special instructions were received'