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_7715171
_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
_audit_creation_date             2024-02-03
_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                73.4540(10)
_cell_angle_beta                 70.8160(10)
_cell_angle_gamma                86.9110(10)
_cell_formula_units_Z            1
_cell_length_a                   10.9183(5)
_cell_length_b                   12.0025(6)
_cell_length_c                   15.8371(6)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      55.016
_cell_measurement_theta_min      6.027
_cell_volume                     1877.18(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    '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  0.0265
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_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            23053
_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         2.712
_exptl_absorpt_coefficient_mu    4.114
_exptl_absorpt_correction_T_max  0.7236
_exptl_absorpt_correction_T_min  0.5816
_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    2.055
_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          0.13
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         6546
_refine_ls_number_restraints     539
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0140P)^2^+4.4126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0491
_refine_ls_wR_factor_ref         0.0511
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5713
_reflns_number_total             6546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03867j2.cif
_cod_data_source_block           JXUST-41
_cod_depositor_comments
'Adding full bibliography for 7715168--7715173.cif.'
_cod_database_code               7715171
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details   SADABS
_olex2_refinement_description
;
1. Restrained distances
 N6A-C38A \\sim N6B-C38B \\sim N6B-C39A \\sim N6A-C39
 with sigma of 0.02
 N6A-C35 \\sim N6B-C35
 with sigma of 0.02
2. Restrained planarity
 O14, C35, C39, N6A, C38A
 with sigma of 0.1
 O14, N6B, C35, C38B, C39A
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
N6B \\sim C35 \\sim C38B \\sim C39 \\sim C39A \\sim N6A \\sim C38A: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C30
\\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C32B \\sim C31B \\sim
C1J \\sim C1I \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38B
\\sim C39 \\sim C39A \\sim C1A \\sim C1B \\sim C1G \\sim C1H \\sim C1C \\sim
C1D \\sim C1E \\sim C1F \\sim C40 \\sim C38A: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004 within 2A
Uanis(C30) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C32B) \\sim Ueq, Uanis(C31B)
\\sim Ueq, Uanis(C1J) \\sim Ueq, Uanis(C1I) \\sim Ueq, Uanis(C33) \\sim Ueq,
Uanis(C1F) \\sim Ueq, Uanis(C1E) \\sim Ueq, Uanis(C1D) \\sim Ueq, Uanis(C1C)
\\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(C1A) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C1J) \\sim Ueq, Uanis(C1F) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(O18)
\\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O15) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C1F) \\sim Ueq, Uanis(C1J) \\sim Ueq, Uanis(C1I) \\sim Ueq, Uanis(C33)
\\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C31B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C1A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(N3BB) \\sim Ueq, Uanis(S2BB) \\sim Ueq, Uanis(N5BB) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O12) \\sim Ueq, Uanis(O18) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
4. Others
 Sof(Dy2A)=1-FVAR(1)
 Sof(Dy2)=FVAR(1)
 Fixed Sof: S2BB(0.5) O9(0.5) O10(0.5) O11(0.5) N3BB(0.5) N5BB(0.5) N6B(0.5)
 O12(0.5) C23(0.5) C24(0.5) C30(0.5) C25(0.5) H25(0.5) C26(0.5) C27(0.5)
 H27(0.5) C28(0.5) C29(0.5) H29(0.5) C32B(0.5) C31B(0.5) C1J(0.5) C1I(0.5)
 H1I(0.5) C33(0.5) H33(0.5) H35A(0.5) H35(0.5) C38B(0.5) H38A(0.5) H38B(0.5)
 H38C(0.5) C39(0.5) H39A(0.5) H39B(0.5) H39C(0.5) C39A(0.5) H39D(0.5) H39E(0.5)
 H39F(0.5) O15(0.5) O16(0.5) O17(0.5) C1A(0.5) C1B(0.5) C1G(0.5) H1G(0.5)
 C1H(0.5) C1C(0.5) H1C(0.5) C1D(0.5) C1E(0.5) H1E(0.5) C1F(0.5) O18(0.5)
 C40(0.5) N6A(0.5) C38A(0.5) H38D(0.5) H38E(0.5) H38F(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C8(H8), C13(H13), C14(H14), C16(H16), C18(H18), C20(H20),
 C25(H25), C27(H27), C29(H29), C1I(H1I), C33(H33), C34(H34), C35(H35A),
 C35(H35), C1G(H1G), C1C(H1C), C1E(H1E)
5.b Fitted hexagon refined as free rotating group:
 C30(C25,C26,C27,C28,C29), C1G(C1H,C1C,C1D,C1E,C1F)
5.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38B(H38A,H38B,H38C), C39(H39A,H39B,
 H39C), C39A(H39D,H39E,H39F), C38A(H38D,H38E,H38F)
;
_shelx_res_checksum              32073
_olex2_submission_special_instructions 'No special instructions were received'