Magnetic modulation and magnetocaloric effect of lanthanide porous organic frameworks with croconic acid.
Shao, Xueying; Yang, Yue; Dong, Xiaofang; Wang, Shen; Liang, Yulu; Liu, Zhongyi; Min, Hui; Wang, Yu-Xia; Cheng, Peng; Chemical communications (Cambridge, England) 61 (2025) 16862–16865; doi:10.1039/d5cc04708k

data_7135026
_publ_section_title
;
 Magnetic modulation and magnetocaloric effect of lanthanide porous
 organic frameworks with croconic acid.
;
_journal_issue                   86
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              16862
_journal_page_last               16865
_journal_paper_doi               10.1039/d5cc04708k
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C60 H48 Gd8 O84, 0.5(Cl3 Gd), 2(H2 O)'
_chemical_formula_sum            'C60 H52 Cl1.5 Gd8.5 O86'
_chemical_formula_weight         3538.81
_space_group_crystal_system      tetragonal
_space_group_IT_number           83
_space_group_name_Hall           '-P 4'
_space_group_name_H-M_alt        'P 4/m'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2025-08-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-08-14 deposited with the CCDC.	2025-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   21.8854(2)
_cell_length_b                   21.8854(2)
_cell_length_c                   7.77440(10)
_cell_measurement_reflns_used    6678
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      75.4150
_cell_measurement_theta_min      2.0020
_cell_volume                     3723.71(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.99a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.99a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.99a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.02(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     73.00 109.00   0.50    0.15    --  105.43-124.00 140.00   72
  2  \w     36.00  61.00   0.50    0.15    --  105.43 -61.00 -90.00   50
  3  \w     79.00 104.00   0.50    0.15    --  105.43 -95.00-180.00   50
  4  \w     36.00  71.00   0.50    0.15    --  105.43 -95.00-180.00   70
  5  \w    -22.00  27.00   0.50    0.05    --  -47.26  19.00 -60.00   98
  6  \w    -21.00  27.00   0.50    0.05    --  -47.26  31.00 158.00   96
  7  \w    -57.00 -32.00   0.50    0.15    -- -104.50  61.00  60.00   50
  8  \w    -65.00 -39.00   0.50    0.15    -- -104.50  61.00  30.00   52
  9  \w    -17.00  28.00   0.50    0.05    --  -47.26  19.00-150.00   90
 10  \w    -68.00 -43.00   0.50    0.15    -- -104.50  61.00-180.00   50
 11  \w   -104.00 -33.00   0.50    0.15    -- -104.50  92.00 -32.00  142
 12  \w   -174.00 -98.00   0.50    0.15    -- -104.50 -31.00  -1.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0701598000
_diffrn_orient_matrix_UB_12      0.0014769000
_diffrn_orient_matrix_UB_13      -0.0156941000
_diffrn_orient_matrix_UB_21      0.0008507000
_diffrn_orient_matrix_UB_22      -0.0647030000
_diffrn_orient_matrix_UB_23      -0.0778162000
_diffrn_orient_matrix_UB_31      -0.0057974000
_diffrn_orient_matrix_UB_32      -0.0275932000
_diffrn_orient_matrix_UB_33      0.1816359000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0875
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            12135
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.489
_diffrn_reflns_theta_min         2.019
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    25.067
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.99a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       block
_exptl_crystal_F_000             1670
_refine_diff_density_max         1.296
_refine_diff_density_min         -1.698
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         4065
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0671
_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^)+(0.1365P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1861
_refine_ls_wR_factor_ref         0.1909
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3494
_reflns_number_total             4065
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04708k2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7135024--7135026.cif.'
_cod_original_cell_volume        3723.71(8)
_cod_original_formula_sum        'C60 H52 Cl1.50 Gd8.50 O86'
_cod_database_code               7135026
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Gd2-Cl2 = Gd2-Cl8 = Gd2-Cl1
 2 with sigma of 0.02
 Cl1-Cl8 \\sim Cl8-Cl2
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(Cl2) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O0) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C00F) \\sim Ueq, Uanis(O5)
\\sim Ueq, Uanis(C0) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(O3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Cl1) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C00X) \\sim Ueq, Uanis(O11B) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C00U)
\\sim Ueq, Uanis(O33) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(O4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C00W) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C00V) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O5) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(Cl8) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O33) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(Gd2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Gd2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Fixed Sof: O11B(0.5) O0(0.5) C0(0.25) C00F(0.25) O12(0.5) O00L(0.5) H00A(0.5)
 H00B(0.5) O00M(0.5) H00C(0.5) H00D(0.5) O00Q(0.5) H00E(0.5) H00F(0.5)
 O00S(0.5) C00U(0.5) C00V(0.5) C00W(0.5) C00X(0.5) O1(0.5) C010(0.5) C011(0.5)
 O2(0.5) H2A(0.5) H2B(0.5) Gd2(0.0625) O10(0.5) C14(0.5) O18(0.5) H18A(0.5)
 H18B(0.5) C2(0.5) O4(0.5) C1A(0.25) O7(0.25) O6(0.25) O5(0.25) Cl2(0.0625)
 O33(0.25) C35(0.25) O11(0.5) O13(0.5) H13A(0.5) H13B(0.5) O3(0.25) H3A(0.25)
 H3B(0.25) Cl8(0.0625) Cl1(0.0625)
6.a Riding coordinates:
 O00L(H00A,H00B), O00M(H00C,H00D), O00Q(H00E,H00F), O18(H18A,H18B), O13(H13A,
 H13B), O3(H3A,H3B)
6.b Rotating group:
 O2(H2A,H2B)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 395 electrons were 
found in a volume of 1221\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
22[H2O], 16[H2O] per Unit Cell 
which account for 380 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.451
_oxdiff_exptl_absorpt_empirical_full_min 0.491