Implementing magnetic properties on demand with a dynamic lanthanoid-organic framework.
Gómez-Muñoz, Iván; Hu, Ziqi; Vitórica-Yrezábal, Iñigo J; Coronado, Eugenio; Mínguez Espallargas, Guillermo; Chemical science 16 (2025) 2879–2885; doi:10.1039/d4sc07042a

data_1574050
_publ_section_title
;
 Implementing magnetic properties on demand with a dynamic
 lanthanoid-organic framework.
;
_journal_issue                   6
_journal_name_full               'Chemical science'
_journal_page_first              2879
_journal_page_last               2885
_journal_paper_doi               10.1039/d4sc07042a
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C30 H22 Ce N O7, 0.5(C3 H7 N O), 0.35[C3H7NO]'
_chemical_formula_sum            'C32.55 H27.95 Ce N1.85 O7.85'
_chemical_formula_weight         710.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-28
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-16 deposited with the CCDC.	2025-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.249(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.0927(3)
_cell_length_b                   27.9263(5)
_cell_length_c                   16.1650(3)
_cell_measurement_reflns_used    9156
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      20.3050
_cell_measurement_theta_min      3.1830
_cell_volume                     6758.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.92a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 40.84a (release 31-07-2020))'
_computing_data_reduction        'CrysAlisPro 1.171.43.92a (Rigaku OD, 2023)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -84.00 -15.00   1.00   20.00    --  -14.81 144.00  25.52   69
  2  \w    -88.00  58.00   1.00   20.00    --  -14.81   0.00 -90.00  146
  3  \w    -14.00  42.00   1.00   20.00    --   15.75  77.00 -30.00   56
  4  \w    -42.00  46.00   1.00   20.00    --   15.75 -77.00  90.00   88
  5  \w    -14.00  42.00   1.00   20.00    --   15.75  77.00  30.00   56
  6  \w      9.00  78.00   1.00   20.00    --   15.75-132.00 -75.18   69
  7  \w    -53.00  37.00   1.00   20.00    --   15.75 -57.00 -30.00   90
  8  \w     -6.00  85.00   1.00   20.00    --   15.75  57.00 120.00   91
  9  \w     -6.00  85.00   1.00   20.00    --   15.75  57.00-120.00   91
 10  \w    -79.00 -12.00   1.00   20.00    --  -14.81 136.00 -84.91   67
 11  \w    -91.00 -39.00   1.00   20.00    --  -14.81-178.00 150.00   52
 12  \w    -35.00  54.00   1.00   20.00    --  -14.81  57.00 150.00   89
 13  \w    -83.00 -51.00   1.00   20.00    --  -14.81 142.00 -24.43   32
 14  \w    -14.00  42.00   1.00   20.00    --   15.75  77.00-180.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0049681000
_diffrn_orient_matrix_UB_12      -0.0200792000
_diffrn_orient_matrix_UB_13      -0.0258742000
_diffrn_orient_matrix_UB_21      0.0260894000
_diffrn_orient_matrix_UB_22      0.0140017000
_diffrn_orient_matrix_UB_23      -0.0244486000
_diffrn_orient_matrix_UB_31      0.0392315000
_diffrn_orient_matrix_UB_32      -0.0067601000
_diffrn_orient_matrix_UB_33      0.0262616000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1565
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            114197
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        23.256
_diffrn_reflns_theta_max         23.256
_diffrn_reflns_theta_min         2.796
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.395
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.92a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       needle
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.618
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         9681
_refine_ls_number_restraints     678
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0525P)^2^+8.3215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7050
_reflns_number_total             9681
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc07042a2.cif
_cod_data_source_block           sx876
_cod_database_code               1574050
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.897
_olex2_refinement_description
;
1. Restrained distances
 C31-C38 \\sim C31-C32
 with sigma of 0.02
 C44-C35 \\sim C44-C41
 with sigma of 0.02
 C38-C43 \\sim C32-C33
 with sigma of 0.02
 C38-C37 \\sim C32-C39
 with sigma of 0.02
 C35-C42 \\sim C41-C34
 with sigma of 0.02
 C35-C36 \\sim C41-C40
 with sigma of 0.02
 C43-C42 \\sim C33-C34
 with sigma of 0.02
 C37-C36 \\sim C39-C40
 with sigma of 0.02
 C31-C43 \\sim C31-C33
 with sigma of 0.04
 C31-C37 \\sim C31-C39
 with sigma of 0.04
 C44-C42 \\sim C44-C34
 with sigma of 0.04
 C44-C36 \\sim C44-C40
 with sigma of 0.04
 C38-C42 \\sim C32-C34
 with sigma of 0.04
 C38-C36 \\sim C32-C40
 with sigma of 0.04
 C35-C43 \\sim C41-C33
 with sigma of 0.04
 C35-C37 \\sim C41-C39
 with sigma of 0.04
 C43-C37 \\sim C33-C39
 with sigma of 0.04
 C42-C36 \\sim C34-C40
 with sigma of 0.04
 N4-C72 \\sim N4-C8
 with sigma of 0.02
 N3-C70 \\sim N3-C23
 with sigma of 0.02
 C56-C53 \\sim C56-C53A
 with sigma of 0.02
 C53-C54 \\sim C53A-C54A
 with sigma of 0.02
 C53-C52 \\sim C53A-C52A
 with sigma of 0.02
 C46-C50 \\sim C46-C50A
 with sigma of 0.02
 C54-C55 \\sim C54A-C55A
 with sigma of 0.02
 C55-C50 \\sim C55A-C50A
 with sigma of 0.02
 C50-C51 \\sim C50A-C51A
 with sigma of 0.02
 C51-C52 \\sim C51A-C52A
 with sigma of 0.02
 C56-C54 \\sim C56-C54A
 with sigma of 0.04
 C56-C52 \\sim C56-C52A
 with sigma of 0.04
 C53-C55 \\sim C53A-C55A
 with sigma of 0.04
 C53-C51 \\sim C53A-C51A
 with sigma of 0.04
 C46-C55 \\sim C46-C55A
 with sigma of 0.04
 C46-C51 \\sim C46-C51A
 with sigma of 0.04
 C54-C50 \\sim C54A-C50A
 with sigma of 0.04
 C54-C52 \\sim C54A-C52A
 with sigma of 0.04
 C55-C51 \\sim C55A-C51A
 with sigma of 0.04
 C50-C52 \\sim C50A-C52A
 with sigma of 0.04
2. Restrained planarity
 C71, O15, N4, C72, C8
 with sigma of 0.1
 C19, O16, N3, C70, C23
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C38 \\sim C35 \\sim C43 \\sim C42 \\sim C37 \\sim C36 \\sim C32 \\sim C41 \\sim
C33 \\sim C34 \\sim C39 \\sim C40: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 2A
C71 \\sim O15 \\sim N4 \\sim C72 \\sim C8: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C19 \\sim O16 \\sim N3 \\sim C70 \\sim C23: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C71 \\sim O15 \\sim N4 \\sim C72 \\sim C8 \\sim C19 \\sim O16 \\sim N3 \\sim
C70 \\sim C23: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
C53 \\sim C54 \\sim C55 \\sim C50 \\sim C51 \\sim C52 \\sim C53A \\sim C54A
\\sim C55A \\sim C50A \\sim C51A \\sim C52A: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 2A
C52A \\sim C52 \\sim C51 \\sim C51A \\sim C50 \\sim C50A \\sim C54 \\sim C54A
\\sim C53A \\sim C53 \\sim C55 \\sim C55A: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004 within 2A
4. Rigid body (RIGU) restrains
 C38, C35, C43, C42, C37, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, C41, C33, C34, C39, C40
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C71, O15, N4, C72, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19, O16, N3, C70, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C53, C54, C55, C50, C51, C52
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C53A, C54A, C55A, C50A, C51A, C52A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C32)=Sof(C41)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34)=Sof(C39)=Sof(H39)=
 Sof(C40)=Sof(H40)=Sof(C19)=Sof(H19)=Sof(O16)=Sof(N3)=Sof(C70)=Sof(H70A)=
 Sof(H70B)=Sof(H70C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=1-FVAR(1)
 Sof(C38)=Sof(C35)=Sof(C43)=Sof(H43)=Sof(C42)=Sof(H42)=Sof(C37)=Sof(H37)=
 Sof(C36)=Sof(H36)=Sof(C71)=Sof(H71)=Sof(O15)=Sof(N4)=Sof(C72)=Sof(H72A)=
 Sof(H72B)=Sof(H72C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(1)
 Sof(C53A)=Sof(C54A)=Sof(H54A)=Sof(C55A)=Sof(H55A)=Sof(C50A)=Sof(C51A)=
 Sof(H51A)=Sof(C52A)=Sof(H52A)=1-FVAR(2)
 Sof(C53)=Sof(C54)=Sof(H54)=Sof(C55)=Sof(H55)=Sof(C50)=Sof(C51)=Sof(H51)=
 Sof(C52)=Sof(H52)=FVAR(2)
6.a Free rotating group:
 C71(O15,N4,C72,C8), C19(O16,N3,C70,C23)
6.b Me refined with riding coordinates:
 C69(H69A,H69B,H69C), C68(H68A,H68B,H68C), C65(H65A,H65B,H65C), C66(H66A,H66B,
 H66C), C72(H72A,H72B,H72C), C8(H8A,H8B,H8C), C70(H70A,H70B,H70C), C23(H23A,
 H23B,H23C)
6.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C20(H20), C49(H49), C28(H28), C12(H12), C47(H47), C10(H10),
 C54(H54), C7(H7), C14(H14), C17(H17), C55(H55), C59(H59), C25(H25), C3(H3),
 C62(H62), C58(H58), C6(H6), C16(H16), C26(H26), C4(H4), C45(H45), C29(H29),
 C61(H61), C43(H43), C67(H67), C64(H64), C51(H51), C42(H42), C52(H52), C37(H37),
  C36(H36), C33(H33), C34(H34), C39(H39), C40(H40), C71(H71), C19(H19),
 C54A(H54A), C55A(H55A), C51A(H51A), C52A(H52A)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 114 electrons were 
found in a volume of 1506\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
0.35[C3H7NO] per formula unit 
which account for 112 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              36316
_shelx_hkl_checksum              55840
_shelx_fab_checksum              49339
_olex2_date_sample_data_collection 2024-04-19
_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 1.045
_oxdiff_exptl_absorpt_empirical_full_min 0.956