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_1574047
_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 La N O7, 0.752(C3 H7 N O), 1[C3H7NO]'
_chemical_formula_sum            'C35.26 H34.26 La N2.75 O8.75'
_chemical_formula_weight         775.44
_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                 95.014(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7495(3)
_cell_length_b                   26.5927(6)
_cell_length_c                   8.4965(2)
_cell_measurement_reflns_used    10159
_cell_measurement_temperature    119.8(3)
_cell_measurement_theta_max      20.6560
_cell_measurement_theta_min      3.0570
_cell_volume                     3769.98(14)
_computing_cell_refinement       'CrysAlisPro 1.171.43.92a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 41.109a (release 07-05-2021))'
_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      119.8(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_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    -59.00  58.00   0.75   17.50    --  -14.97  19.00 -90.00  156
  2  \w    -40.00  56.00   0.75   17.50    --  -14.97  38.00  90.00  128
  3  \w    -42.00  15.00   0.75   17.50    --  -14.97 -77.00-150.00   76
  4  \w    -42.00  15.00   0.75   17.50    --  -14.97 -77.00 -90.00   76
  5  \w    -45.00  42.00   0.75   17.50    --  -14.97  77.00 120.00  116
  6  \w    -14.00  41.50   0.75   17.50    --   15.98  77.00  60.00   74
  7  \w    -53.00  37.00   0.75   17.50    --   15.98 -57.00 -60.00  120
  8  \w    -42.00  15.00   0.75   17.50    --  -14.97 -77.00 120.00   76
  9  \w    -15.00  57.00   0.75   17.50    --   15.98 -99.00   0.00   96
 10  \w    -14.00  41.50   0.75   17.50    --   15.98  77.00-120.00   74
 11  \w    -15.00  57.00   0.75   17.50    --   15.98 -99.00 -90.00   96
 12  \w     -5.00  85.00   0.75   17.50    --   15.98  57.00  30.00  120
 13  \w    -14.00  41.50   0.75   17.50    --   15.98  77.00 150.00   74
 14  \w     -5.00  40.00   0.75   17.50    --   15.98  57.00-150.00   60
;
_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      -0.0257968000
_diffrn_orient_matrix_UB_12      0.0188085000
_diffrn_orient_matrix_UB_13      0.0261148000
_diffrn_orient_matrix_UB_21      0.0090039000
_diffrn_orient_matrix_UB_22      -0.0080062000
_diffrn_orient_matrix_UB_23      0.0792418000
_diffrn_orient_matrix_UB_31      0.0325621000
_diffrn_orient_matrix_UB_32      0.0171138000
_diffrn_orient_matrix_UB_33      0.0083280000
_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  0.1304
_diffrn_reflns_av_unetI/netI     0.0989
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            68979
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.853
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.185
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92753
_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    1.366
_exptl_crystal_description       needle
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.029
_refine_diff_density_min         -2.017
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         7663
_refine_ls_number_restraints     197
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0811
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0769P)^2^+46.7292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.2083
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5183
_reflns_number_total             7663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc07042a2.cif
_cod_data_source_block           sx987
_cod_database_code               1574047
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N4-C30 \\sim N4-C32
 with sigma of 0.02
 La01-O8 \\sim La01-O9
 with sigma of 0.02
 C28-O8 \\sim C33-O9
 with sigma of 0.02
 C28-N4 \\sim C33-N4A
 with sigma of 0.02
 N4-C30 \\sim N4A-C31
 with sigma of 0.02
 N4-C32 \\sim N4A-C29
 with sigma of 0.02
 La01-C28 \\sim La01-C33
 with sigma of 0.04
 C28-C30 \\sim C33-C31
 with sigma of 0.04
 C28-C32 \\sim C33-C29
 with sigma of 0.04
 O8-N4 \\sim O9-N4A
 with sigma of 0.04
 C30-C32 \\sim C31-C29
 with sigma of 0.04
 N1-C35 \\sim N1-C36
 with sigma of 0.02
3. Restrained planarity
 C28, O8, N4, C30, C32
 with sigma of 0.1
 C34, O10, N1, C35, C36
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C28 \\sim O8 \\sim N4 \\sim C30 \\sim C32: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C28 \\sim O8 \\sim N4 \\sim C30 \\sim C32 \\sim C33 \\sim O9 \\sim N4A \\sim
C31 \\sim C29: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
C34 \\sim O10 \\sim N1 \\sim C35 \\sim C36: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 2A
5. Rigid body (RIGU) restrains
 C28, O8, N4, C30, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C33, O9, N4A, C31, C29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C34, O10, N1, C35, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C33)=Sof(H33)=Sof(O9)=Sof(N4A)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=1-FVAR(1)
 Sof(C28)=Sof(H28)=Sof(O8)=Sof(N4)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(1)
 Sof(C34)=Sof(H34)=Sof(O10)=Sof(N1)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=1-FVAR(2)
7.a Free rotating group:
 C28(O8,N4,C30,C32), C33(O9,N4A,C31,C29), C34(O10,N1,C35,C36)
7.b Me refined with riding coordinates:
 C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C29(H29A,H29B,
 H29C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
7.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C26(H26), C19(H19), C11(H11), C25(H25), C3(H3), C23(H23), C15(H15),
 C9(H9), C13(H13), C22(H22), C7(H7), C16(H16), C6(H6), C4(H4), C28(H28),
 C33(H33), C34(H34)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 180 electrons were 
found in a volume of 929\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1[C3H7NO] per formula unit 
which account for 160 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              83757
_shelx_hkl_checksum              2638
_shelx_fab_checksum              29935
_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 1.181
_oxdiff_exptl_absorpt_empirical_full_min 0.866