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_1574049
_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 N O7 Pr, 0.5(C3 H7 N O), 1[H2O]'
_chemical_formula_sum            'C31.5 H27.5 N1.5 O8.5 Pr'
_chemical_formula_weight         703.96
_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                 97.259(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.0438(3)
_cell_length_b                   28.0476(6)
_cell_length_c                   16.0831(4)
_cell_measurement_reflns_used    7832
_cell_measurement_temperature    119.9(8)
_cell_measurement_theta_max      27.6360
_cell_measurement_theta_min      3.0890
_cell_volume                     6731.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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      119.9(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.837
_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     12.00  38.00   1.00   10.00    --  -14.81  77.00-180.00   26
  2  \w    -89.00 -50.00   1.00   10.00    --  -14.81-178.00-150.00   39
  3  \w     52.00  92.00   1.00   10.00    --   15.75 178.00 -30.00   40
  4  \w    -57.00  59.00   1.00   10.00    --   15.75 -19.00  60.00  116
;
_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      0.0004841000
_diffrn_orient_matrix_UB_12      -0.0002024000
_diffrn_orient_matrix_UB_13      -0.0440278000
_diffrn_orient_matrix_UB_21      0.0246772000
_diffrn_orient_matrix_UB_22      -0.0216227000
_diffrn_orient_matrix_UB_23      0.0034199000
_diffrn_orient_matrix_UB_31      -0.0406082000
_diffrn_orient_matrix_UB_32      -0.0131379000
_diffrn_orient_matrix_UB_33      -0.0050124000
_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  0.0513
_diffrn_reflns_av_unetI/netI     0.0968
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28894
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.935
_diffrn_reflns_theta_min         2.825
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.496
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.389
_exptl_crystal_description       plank
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.864
_refine_diff_density_min         -1.158
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     824
_refine_ls_number_reflns         13509
_refine_ls_number_restraints     562
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0346P)^2^+9.1779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1209
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9920
_reflns_number_total             13509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc07042a2.cif
_cod_data_source_block           sx870
_cod_original_formula_sum        'C31.50 H27.50 N1.50 O8.50 Pr'
_cod_database_code               1574049
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.841
_olex2_refinement_description
;
1. Restrained distances
 C28-C29 \\sim C28-C35
 with sigma of 0.02
 C29-C36 \\sim C35-C34
 with sigma of 0.02
 C29-C30 \\sim C35-C40
 with sigma of 0.02
 C41-C32 \\sim C41-C38
 with sigma of 0.02
 C32-C37 \\sim C38-C33
 with sigma of 0.02
 C32-C31 \\sim C38-C39
 with sigma of 0.02
 C36-C37 \\sim C34-C33
 with sigma of 0.02
 C30-C31 \\sim C40-C39
 with sigma of 0.02
 C28-C36 \\sim C28-C34
 with sigma of 0.04
 C28-C30 \\sim C28-C40
 with sigma of 0.04
 C29-C37 \\sim C35-C33
 with sigma of 0.04
 C29-C31 \\sim C35-C39
 with sigma of 0.04
 C41-C37 \\sim C41-C33
 with sigma of 0.04
 C41-C31 \\sim C41-C39
 with sigma of 0.04
 C32-C36 \\sim C38-C34
 with sigma of 0.04
 C32-C30 \\sim C38-C40
 with sigma of 0.04
 C36-C30 \\sim C34-C40
 with sigma of 0.04
 C37-C31 \\sim C33-C39
 with sigma of 0.04
 C50-C49 \\sim C50-C49A
 with sigma of 0.02
 C50-C51 \\sim C50-C51A
 with sigma of 0.02
 C49-C48 \\sim C49A-C48A
 with sigma of 0.02
 C47-C48 \\sim C47-C48A
 with sigma of 0.02
 C47-C52 \\sim C47-C52A
 with sigma of 0.02
 C52-C51 \\sim C52A-C51A
 with sigma of 0.02
 C50-C48 \\sim C50-C48A
 with sigma of 0.04
 C50-C52 \\sim C50-C52A
 with sigma of 0.04
 C49-C47 \\sim C49A-C47
 with sigma of 0.04
 C47-C51 \\sim C47-C51A
 with sigma of 0.04
 N1-C1E \\sim N1-C1F
 with sigma of 0.02
 N4-C1B \\sim N4-C1C
 with sigma of 0.02
2. Restrained planarity
 C1D, O15, N1, C1E, C1F
 with sigma of 0.1
 C1A, O16, N4, C1B, C1C
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C29 \\sim C32 \\sim C36 \\sim C37 \\sim C30 \\sim C31 \\sim C35 \\sim C38 \\sim
C34 \\sim C33 \\sim C40 \\sim C39: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 2A
C50 \\sim C49 \\sim C47 \\sim C48 \\sim C52 \\sim C51 \\sim C52A \\sim C51A
\\sim C49A \\sim C48A: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
C1D \\sim O15 \\sim N1 \\sim C1E \\sim C1F: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C1A \\sim O16 \\sim N4 \\sim C1B \\sim C1C: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C1B \\sim N4 \\sim C1C \\sim C1A \\sim O16 \\sim C1E \\sim N1 \\sim C1F \\sim
C1D \\sim O15: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C35) = Uanis(C29) = Uanis(C34) = Uanis(C36)
Uanis(C51) = Uanis(C51A) = Uanis(C52A) = Uanis(C52)
4. Rigid body (RIGU) restrains
 C29, C32, C36, C37, C30, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C35, C38, C34, C33, C40, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C49, C48, C52, C51
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C49A, C48A, C52A, C51A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1D, O15, N1, C1E, C1F
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1A, O16, N4, C1B, C1C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C1A)=Sof(H1A)=Sof(O16)=Sof(N4)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=
 Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=1-FVAR(1)
 Sof(C1D)=Sof(H1D)=Sof(O15)=Sof(N1)=Sof(C1E)=Sof(H1EA)=Sof(H1EB)=Sof(H1EC)=
 Sof(C1F)=Sof(H1FA)=Sof(H1FB)=Sof(H1FC)=FVAR(1)
 Sof(C35)=Sof(C38)=Sof(C34)=Sof(H34)=Sof(C33)=Sof(H33)=Sof(C40)=Sof(H40)=
 Sof(C39)=Sof(H39)=1-FVAR(2)
 Sof(C29)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(C37)=Sof(H37)=
 Sof(C36)=Sof(H36)=FVAR(2)
 Sof(C52A)=Sof(H52A)=Sof(C51A)=Sof(H51A)=Sof(C49A)=Sof(H49A)=Sof(C48A)=
 Sof(H48A)=1-FVAR(3)
 Sof(C49)=Sof(H49)=Sof(C48)=Sof(H48)=Sof(C52)=Sof(H52)=Sof(C51)=Sof(H51)=FVAR(3)
6.a Free rotating group:
 C1D(O15,N1,C1E,C1F), C1A(O16,N4,C1B,C1C)
6.b Me refined with riding coordinates:
 C1E(H1EA,H1EB,H1EC), C1F(H1FA,H1FB,H1FC), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,
 H1CC)
6.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C16(H16), C9(H9), C22(H22), C42(H42), C44(H44), C13(H13), C30(H30),
 C31(H31), C37(H37), C36(H36), C58(H58), C49(H49), C3(H3), C11(H11), C59(H59),
 C25(H25), C55(H55), C18(H18), C7(H7), C56(H56), C19(H19), C15(H15), C48(H48),
 C6(H6), C26(H26), C46(H46), C4(H4), C69(H69), C66(H66), C52(H52), C51(H51),
 C34(H34), C33(H33), C40(H40), C39(H39), C52A(H52A), C51A(H51A), C49A(H49A),
 C48A(H48A), C1D(H1D), C1A(H1A)
6.d Fitted hexagon refined as free rotating group:
 C29(C30,C31,C32,C37,C36)
6.e Idealised Me refined as rotating group:
 C68(H68A,H68B,H68C), C70(H70A,H70B,H70C), C67(H67A,H67B,H67C), C71(H71A,H71B,
 H71C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 88 electrons were 
found in a volume of 1494\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[H2O] per formula unit 
which account for 80 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              68105
_shelx_hkl_checksum              64925
_shelx_fab_checksum              63740
_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 1.149
_oxdiff_exptl_absorpt_empirical_full_min 0.924