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_7715169
_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 Dy4 N10 O28 S3'
_chemical_formula_sum            'C78 H52 Dy4 N10 O28 S3'
_chemical_formula_weight         2323.47
_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
_atom_sites_solution_primary     iterative
_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                73.3540(10)
_cell_angle_beta                 70.6160(10)
_cell_angle_gamma                86.5110(10)
_cell_formula_units_Z            1
_cell_length_a                   10.9883(5)
_cell_length_b                   12.5025(6)
_cell_length_c                   15.4371(6)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.66
_cell_measurement_theta_min      2.79
_cell_volume                     1915.34(15)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0269
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_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            23480
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         2.649
_exptl_absorpt_coefficient_mu    4.032
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0874 before and 0.0452 after correction.
The Ratio of minimum to maximum transmission is 0.7590.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_description       block
_exptl_crystal_F_000             1126
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.036
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         6703
_refine_ls_number_restraints     386
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0245P)^2^+8.5372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0711
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5821
_reflns_number_total             6703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03867j2.cif
_cod_data_source_block           JXUST-41b
_cod_depositor_comments
'Adding full bibliography for 7715168--7715173.cif.'
_cod_database_code               7715169
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details   SADABS
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N6-C3 = N2-C49
 1.37 with sigma of 0.02
 S2-N2 = S2-N6
 1.62 with sigma of 0.02
 N5-C31 \\sim N5A-C31
 with sigma of 0.02
 N5-C35 \\sim N5A-C35A
 with sigma of 0.02
 C31-C17 \\sim C31-C17A
 with sigma of 0.04
 Dy2-O10 \\sim Dy2A-O10
 with sigma of 0.02
 C31-C35 \\sim C31-C35A
 with sigma of 0.04
 C17-C35 \\sim C17A-C35A
 with sigma of 0.04
 Dy2-O3 \\sim Dy2A-O3
 with sigma of 0.02
 N5A-C31 \\sim N5-C31
 with sigma of 0.02
 N5A-C35A \\sim N5-C35
 with sigma of 0.02
 N5-C17 \\sim N5A-C17A
 with sigma of 0.02
3. Restrained planarity
 N5, C17, C35, C31
 with sigma of 0.1
 C17A, N5A, C35A, C31
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C31 \\sim N5 \\sim C35 \\sim C17: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
C25 \\sim C29 \\sim C7 \\sim C13 \\sim C50 \\sim C27: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.004 within 2A
N5 \\sim C31 \\sim C17 \\sim C35 \\sim N5A \\sim C17A \\sim C35A: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C49 \\sim C11 \\sim C3 \\sim C47 \\sim C23 \\sim C45: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.004 within 2A
C21 \\sim C5 \\sim C39 \\sim C43 \\sim C41 \\sim C19 \\sim C37 \\sim O7: within
2A with sigma of 0.002 and sigma for terminal atoms of 0.004 within 2A
C2 \\sim C33: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Uanis(O5) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O2) \\sim
Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.1
Uanis(C46) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N5) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(N5A) \\sim Ueq, Uanis(C17A) \\sim Ueq, Uanis(C35A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C50) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C37) \\sim Ueq,
Uanis(O7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.001
Uanis(C11) \\sim Ueq, Uanis(C45) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C23) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C49)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C45) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C2) \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C9) = Uanis(C5) = Uanis(C46)
5. Others
 Sof(Dy2A)=1-FVAR(1)
 Sof(Dy2)=FVAR(1)
 Sof(H31A)=Sof(N5A)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C35A)=
 Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(2)
 Sof(N5)=Sof(H31)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C35)=Sof(H35A)=
 Sof(H35B)=Sof(H35C)=FVAR(2)
 Fixed Sof: S2(0.5) O17(0.5) O9(0.5) O5(0.5) N6(0.5) N2(0.5) C46(0.5) C48(0.5)
 C50(0.5) C25(0.5) H25(0.5) C13(0.5) C27(0.5) H27(0.5) C7(0.5) C29(0.5)
 H29(0.5) O7(0.5) O15(0.5) O2(0.5) C9(0.5) C37(0.5) C19(0.5) C39(0.5) H39(0.5)
 C5(0.5) C41(0.5) H41(0.5) C21(0.5) C43(0.5) H43(0.5) C11(0.5) C45(0.5)
 H45(0.5) C23(0.5) H23(0.5) C47(0.5) C3(0.5) C49(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C12(H12), C16(H16), C26(H26), C28(H28), C32(H32), C36(H36), C40(H40),
 C25(H25), C27(H27), C29(H29), C15(H15), C31(H31), C31(H31A), C39(H39),
 C41(H41), C43(H43), C45(H45), C23(H23)
6.b Fitted hexagon refined as free rotating group:
 C50(C25,C13,C27,C7,C29), C19(C39,C5,C41,C21,C43), C11(C45,C23,C47,C3,C49)
6.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C33(H33A,H33B,H33C), C17(H17A,H17B,H17C), C35(H35A,H35B,
 H35C), C17A(H17D,H17E,H17F), C35A(H35D,H35E,H35F)
;
_shelx_res_checksum              6455
_olex2_submission_special_instructions 'No special instructions were received'