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_7135024
_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         'C19 H16 Dy2 O19, C H4 O'
_chemical_formula_sum            'C20 H20 Dy2 O20'
_chemical_formula_weight         905.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-08-14
_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                 97.457(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6415(3)
_cell_length_b                   15.8785(5)
_cell_length_c                   21.8456(6)
_cell_measurement_reflns_used    5039
_cell_measurement_temperature    100(15)
_cell_measurement_theta_max      73.9450
_cell_measurement_theta_min      4.0440
_cell_volume                     2628.23(15)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(15)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     35.00  64.00   0.50    1.50    --  105.43 -61.00  30.00   58
  2  \w     35.00  67.00   0.50    1.50    --  105.43 -95.00   0.00   64
  3  \w     20.00  93.00   0.50    0.75    --   47.01-125.00   0.00  146
  4  \w     -5.00  20.00   0.50    0.75    --   47.01 -56.00-153.00   50
  5  \w     33.00  58.00   0.50    1.50    --  105.43 -56.00-153.00   50
  6  \w     97.00 125.00   0.50    1.50    --  105.43  56.00 -11.00   56
  7  \w     52.00  77.00   0.50    0.75    --   47.01  56.00 -11.00   50
  8  \w    -26.00  26.00   0.50    0.75    --  -47.01  56.00 -11.00  104
  9  \w     -6.00  29.00   0.50    0.75    --  -47.01  19.00 150.00   70
 10  \w    -38.00  -7.00   0.50    0.75    --  -47.01  38.00 150.00   62
 11  \w    -67.00 -40.00   0.50    1.50    -- -104.50  61.00 120.00   54
 12  \w   -101.00 -32.00   0.50    1.50    -- -104.50  77.00   0.00  138
 13  \w    -99.00 -72.00   0.50    1.50    -- -104.50  77.00-120.00   54
 14  \w    -60.00 -32.00   0.50    1.50    -- -104.50  61.00-180.00   56
 15  \w    -61.00 -36.00   0.50    1.50    -- -104.50  77.00-120.00   50
 16  \w    -68.00 -34.00   0.50    1.50    -- -104.50  61.00 -90.00   68
 17  \w    -61.00 -36.00   0.50    1.50    -- -104.50  56.00 -11.00   50
 18  \w   -111.00 -46.00   0.50    1.50    -- -104.50 125.00  90.00  130
 19  \w   -129.00-103.00   0.50    1.50    -- -104.50 -61.00 -60.00   52
 20  \w   -167.00-138.00   0.50    1.50    -- -104.50 -61.00 -60.00   58
 21  \w   -172.00-100.00   0.50    1.50    -- -104.50 -45.00 -90.00  144
 22  \w   -158.00 -90.00   0.50    1.50    -- -104.50 -56.00-153.00  136
 23  \w   -118.00 -41.00   0.50    0.75    --  -47.01 -56.00-153.00  154
 24  \w   -125.00 -92.00   0.50    1.50    -- -104.50 -30.00 150.00   66
 25  \w   -169.00-129.00   0.50    1.50    -- -104.50 -30.00 150.00   80
 26  \w   -174.00 -84.00   0.50    1.50    -- -104.50 -95.00 150.00  180
;
_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      0.1879429000
_diffrn_orient_matrix_UB_12      0.0089067000
_diffrn_orient_matrix_UB_13      -0.0176045000
_diffrn_orient_matrix_UB_21      0.0677195000
_diffrn_orient_matrix_UB_22      -0.0649269000
_diffrn_orient_matrix_UB_23      0.0499371000
_diffrn_orient_matrix_UB_31      -0.0379290000
_diffrn_orient_matrix_UB_32      -0.0715165000
_diffrn_orient_matrix_UB_33      -0.0474950000
_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  0.0884
_diffrn_reflns_av_unetI/netI     0.0762
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17819
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.599
_diffrn_reflns_theta_max         66.599
_diffrn_reflns_theta_min         2.040
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    30.940
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26041
_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 light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.288
_exptl_crystal_description       needle
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         4.752
_refine_diff_density_min         -1.894
_refine_diff_density_rms         0.490
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         4653
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0928
_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^)+(0.1138P)^2^+104.3036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2255
_refine_ls_wR_factor_ref         0.2412
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3708
_reflns_number_total             4653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04708k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7135024--7135026.cif.'
_cod_database_code               7135024
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9663(14)
 0.0337(14)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Restrained distances
 O00K-H00K
 0.87 with sigma of 0.01
 O00L-H00L
 0.87 with sigma of 0.01
 O00D-H00D
 0.87 with sigma of 0.01
 O00P-H00P
 0.87 with sigma of 0.01
 Dy02-H00L
 2.913783 with sigma of 0.02
 Dy02-H00P
 2.868355 with sigma of 0.02
 C016-H00L
 1.946572 with sigma of 0.02
 C014-H00P
 1.955127 with sigma of 0.02
 Dy02-H00D
 2.872844 with sigma of 0.02
 C015-H00D
 1.918113 with sigma of 0.02
 C013-H00K
 1.893078 with sigma of 0.02
 Dy01-H00K
 2.914214 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C00G) \\sim Ueq, Uanis(C00T) \\sim Ueq, Uanis(O00C) \\sim Ueq,
Uanis(C00R) \\sim Ueq, Uanis(C00N) \\sim Ueq, Uanis(O007) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(C00G) \\sim Ueq, Uanis(C00T) \\sim Ueq, Uanis(O00C) \\sim Ueq: with sigma
of 0.002 and sigma for terminal atoms of 0.004
Uanis(O00I) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
5.a Riding coordinates:
 O00O(H00O)
5.b Fitted pentagon refined as free rotating group:
 C00Y(C00M,C00R,C00N,C00V), C00Z(C00X,C00G,C00T,C00Q), C011(C00S,C010,C00W,C012)
5.c Idealised Me refined as rotating group:
 C00U(H00A,H00B,H00C), C013(H01A,H01B,H01C), C014(H01D,H01E,H01F), C015(H01G,
 H01H,H01I), C016(H01J,H01K,H01L)
;
_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 2.974
_oxdiff_exptl_absorpt_empirical_full_min 0.557