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_1574048
_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, 0.5(C3 H7 N O), 0.6[C3H7NO]'
_chemical_formula_sum            'C33.3 H29.7 La N2.1 O8.1'
_chemical_formula_weight         727.80
_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                 97.287(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.0013(6)
_cell_length_b                   27.7449(9)
_cell_length_c                   16.1774(9)
_cell_measurement_reflns_used    12428
_cell_measurement_temperature    119.5(8)
_cell_measurement_theta_max      22.5670
_cell_measurement_theta_min      3.0780
_cell_volume                     6678.8(5)
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.5(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.991
_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    -35.00  54.00   1.00   20.00    --  -14.81  57.00 150.00   89
  2  \w    -77.00  -9.00   1.00   20.00    --  -14.81 132.00 158.68   68
  3  \w    -14.00  42.00   1.00   20.00    --   15.75  77.00-120.00   56
  4  \w    -53.00  37.00   1.00   20.00    --   15.75 -57.00-120.00   90
  5  \w     -6.00  85.00   1.00   20.00    --   15.75  57.00  30.00   91
  6  \w    -42.00  46.00   1.00   20.00    --   15.75 -77.00   0.00   88
  7  \w      9.00  78.00   1.00   20.00    --   15.75-132.00 142.55   69
  8  \w    -28.00  89.00   1.00   20.00    --   15.75  19.00 -30.00  117
  9  \w     -6.00  85.00   1.00   20.00    --   15.75  57.00 150.00   91
 10  \w    -91.00 -60.00   1.00   20.00    --  -14.81-178.00  60.00   31
 11  \w    -14.00  42.00   1.00   20.00    --   15.75  77.00  90.00   56
 12  \w    -14.00  42.00   1.00   20.00    --   15.75  77.00 -30.00   56
 13  \w      9.00  78.00   1.00   20.00    --   15.75-132.00  40.74   69
;
_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      -0.0094341000
_diffrn_orient_matrix_UB_12      -0.0161307000
_diffrn_orient_matrix_UB_13      0.0317862000
_diffrn_orient_matrix_UB_21      -0.0359481000
_diffrn_orient_matrix_UB_22      -0.0100166000
_diffrn_orient_matrix_UB_23      -0.0273222000
_diffrn_orient_matrix_UB_31      0.0298584000
_diffrn_orient_matrix_UB_32      -0.0171268000
_diffrn_orient_matrix_UB_33      -0.0139686000
_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  0.125
_diffrn_reflns_av_unetI/netI     0.1741
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20073
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.124
_diffrn_reflns_theta_max         25.124
_diffrn_reflns_theta_min         2.810
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.330
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88264
_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    1.448
_exptl_crystal_description       needle
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.750
_refine_diff_density_min         -1.907
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         20073
_refine_ls_number_restraints     685
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1347
_refine_ls_R_factor_gt           0.0807
_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^)+(0.1310P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2073
_refine_ls_wR_factor_ref         0.2310
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11572
_reflns_number_total             20073
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9982\% 
around [-0.11 0.00 0.99] (reciprocal) or [0.00 0.00 1.00] (direct)
;
_cod_data_source_file            d4sc07042a2.cif
_cod_data_source_block           sx869t_twin1_hklf4
_cod_original_formula_sum        'C33.30 H29.70 La N2.10 O8.10'
_cod_database_code               1574048
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.857
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.56715
 0.43285
2. Restrained distances
 N4-C65 \\sim N4-C66
 with sigma of 0.02
 N3-C63 \\sim N3-C64
 with sigma of 0.02
3. Restrained planarity
 C62, O15, N4, C65, C66
 with sigma of 0.1
 C61, O14, N3, C63, C64
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C62 \\sim O15 \\sim N4 \\sim C65 \\sim C66: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C61 \\sim O14 \\sim N3 \\sim C63 \\sim C64: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C62 \\sim O15 \\sim N4 \\sim C65 \\sim C66 \\sim C61 \\sim O14 \\sim N3 \\sim
C63 \\sim C64: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C14: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C62, O15, N4, C65, C66
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C61, O14, N3, C63, C64
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Sof(C61)=Sof(H61)=Sof(O14)=Sof(N3)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=
 Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=1-FVAR(1)
 Sof(C62)=Sof(H62)=Sof(O15)=Sof(N4)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=
 Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=FVAR(1)
7.a Free rotating group:
 C62(O15,N4,C65,C66), C61(O14,N3,C63,C64)
7.b Me refined with riding coordinates:
 C60(H60A,H60B,H60C), C59(H59A,H59B,H59C), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C63(H63A,H63B,H63C), C64(H64A,
 H64B,H64C)
7.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C36(H36), C43(H43), C9(H9), C34(H34), C11(H11), C50(H50), C40(H40),
 C30(H30), C42(H42), C18(H18), C23(H23), C25(H25), C33(H33), C22(H22), C52(H52),
  C26(H26), C38(H38), C31(H31), C15(H15), C49(H49), C7(H7), C13(H13), C46(H46),
 C53(H53), C16(H16), C58(H58), C45(H45), C55(H55), C6(H6), C4(H4), C3(H3),
 C62(H62), C61(H61)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 196 electrons were 
found in a volume of 1608\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.6[C3H7NO] per formula unit 
which account for 192 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              40361
_shelx_hkl_checksum              44169
_shelx_fab_checksum              62958
_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 1.258
_oxdiff_exptl_absorpt_empirical_full_min 0.830
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2