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_1574046
_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_absolute_configuration ad
_chemical_formula_moiety         'C57 Dy2 N O14, 4(C3 N O), O, 1[C3H7NO]'
_chemical_formula_sum            'C36 H37 Dy N3 O9.5'
_chemical_formula_weight         826.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_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
;
2024-09-27 deposited with the CCDC.	2025-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.297(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0212(5)
_cell_length_b                   26.890(2)
_cell_length_c                   16.3817(18)
_cell_measurement_reflns_used    2722
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      25.1570
_cell_measurement_theta_min      2.9700
_cell_volume                     3530.5(5)
_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  (Sheldrick, 2015)'
_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 0.991
_diffrn_measured_fraction_theta_max 0.937
_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     65.00  92.00   1.00   20.00    --   15.75 178.00-180.00   27
  2  \w    -57.00  63.00   1.00   20.00    --   15.75   0.00-180.00  120
  3  \w      4.00  61.00   1.00   20.00    --   15.75  38.00-150.00   57
;
_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      0.0314554000
_diffrn_orient_matrix_UB_12      -0.0136452000
_diffrn_orient_matrix_UB_13      0.0343397000
_diffrn_orient_matrix_UB_21      -0.0213147000
_diffrn_orient_matrix_UB_22      0.0198817000
_diffrn_orient_matrix_UB_23      0.0260267000
_diffrn_orient_matrix_UB_31      -0.0799117000
_diffrn_orient_matrix_UB_32      -0.0106802000
_diffrn_orient_matrix_UB_33      0.0046550000
_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  0.1312
_diffrn_reflns_av_unetI/netI     0.1774
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12355
_diffrn_reflns_point_group_measured_fraction_full 0.721
_diffrn_reflns_point_group_measured_fraction_max 0.673
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.442
_diffrn_reflns_theta_min         2.874
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.176
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98139
_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    1.554
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.493
_refine_diff_density_min         -0.948
_refine_diff_density_rms         0.183
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.425(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.790
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         12355
_refine_ls_number_restraints     1106
_refine_ls_restrained_S_all      0.760
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0505
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0785
_reflns_Friedel_coverage         0.405
_reflns_Friedel_fraction_full    0.439
_reflns_Friedel_fraction_max     0.397
_reflns_number_gt                9088
_reflns_number_total             12355
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9643\% 
around [1.00 -0.00 -0.08] (reciprocal) or [1.00 -0.00 -0.00] (direct)
;
_cod_data_source_file            d4sc07042a2.cif
_cod_data_source_block           sx875_twin1_hklf4
_cod_original_formula_sum        'C36 H37 Dy N3 O9.50'
_cod_database_code               1574046
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O Dy'
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.938
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.49715
 0.50285
2. Restrained distances
 N4-C57 \\sim N4-C61
 with sigma of 0.02
3. Restrained planarity
 C55, O12, N4, C57, C61
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C52 \\sim C49 \\sim C48 \\sim C53 \\sim C50: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
C27 \\sim C23 \\sim C24 \\sim O3 \\sim C25 \\sim O4: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002 within 2A
C10 \\sim C12 \\sim C11 \\sim C13 \\sim C8 \\sim C9: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01 within 2A
C01Q \\sim N01W \\sim C041 \\sim C56: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 2A
O5 \\sim C20 \\sim C17 \\sim O6: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C55 \\sim O12 \\sim N4 \\sim C57 \\sim C61: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
N4 \\sim C55 \\sim O12 \\sim C57 \\sim C61: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 2A
O14 \\sim C01D \\sim N02J \\sim C03F \\sim C85: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C41 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C23 \\sim C24 \\sim C25 \\sim C22 \\sim C26 \\sim C21: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C34 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.004 within 2A
O5 \\sim O6 \\sim C20 \\sim C17 \\sim C16 \\sim C19 \\sim C18: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C2 \\sim O1 \\sim O2 \\sim C7 \\sim C3 \\sim C1: within 2A with sigma of 0.002
and sigma for terminal atoms of 0.004 within 2A
O5 \\sim O6 \\sim C20 \\sim C17 \\sim C15 \\sim C16 \\sim C19 \\sim C14 \\sim
C18: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004 within
2A
O7 \\sim O8 \\sim C29 \\sim C28: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004 within 2A
C54 \\sim O11 \\sim O13 \\sim C52 \\sim C51 \\sim C50: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.004 within 2A
O11 \\sim O13 \\sim C54 \\sim C51: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004 within 2A
C041 \\sim N01W \\sim C01Q \\sim O00Z \\sim C56: within 2A with sigma of 0.002
and sigma for terminal atoms of 0.004 within 2A
Uanis(O8) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C55, O12, N4, C57, C61
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Riding coordinates:
 O013(H01H,H01I)
6.b Free rotating group:
 C55(O12,N4,C57,C61)
6.c Me refined with riding coordinates:
 C01Z(H01E,H01F,H01G), C02I(H02A,H02B,H02C), C03F(H03A,H03B,H03C), C041(H04A,
 H04B,H04C), C04E(H04E,H04F,H04G), C59(H59A,H59B,H59C), C79(H79A,H79B,H79C),
 C85(H85A,H85B,H85C), C60(H60A,H60B,H60C), C57(H57A,H57B,H57C), C61(H61A,H61B,
 H61C)
6.d Aromatic/amide H refined with riding coordinates:
 C23(H23), C34(H34), C52(H52), C40(H40), C7(H7), C15(H15), C30(H30),
 C01D(H01D), C25(H25), C16(H16), C11(H11), C3(H3), C6(H6), C31(H31), C47(H47),
 C22(H22), C19(H19), C26(H26), C13(H13), C33(H33), C49(H49), C18(H18), C38(H38),
  C9(H9), C02W(H02W), C45(H45), C4(H4), C41(H41), C43(H43), C53(H53), C37(H37),
 C04D(H04D), C50(H50), C56(H56), C58(H58), C55(H55)
6.e Idealised Me refined as rotating group:
 C01Q(H01A,H01B,H01C)
;
_shelx_res_checksum              16010
_shelx_hkl_checksum              10107
_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 1.036
_oxdiff_exptl_absorpt_empirical_full_min 0.976
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2