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_1574052
_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         'C28.5 H19 Ce N0.5 O6.75'
_chemical_formula_sum            'C28.5 H19 Ce N0.5 O6.75'
_chemical_formula_weight         616.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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
;
2024-09-16 deposited with the CCDC.	2025-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.4230(10)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   15.3286(3)
_cell_length_b                   20.5857(4)
_cell_length_c                   32.2184(4)
_cell_measurement_reflns_used    16446
_cell_measurement_temperature    119.4(9)
_cell_measurement_theta_max      19.7890
_cell_measurement_theta_min      3.0320
_cell_volume                     10136.2(3)
_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      119.4(9)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -78.00 -11.00   1.00   11.50    --  -14.81 134.00  53.13   67
  2  \w    -45.00  42.00   1.00   11.50    --  -14.81  77.00-150.00   87
  3  \w    -14.00  42.00   1.00   11.50    --   15.83  77.00  60.00   56
  4  \w    -57.00  41.00   1.00   11.50    --   15.83 -38.00 150.00   98
  5  \w    -53.00  37.00   1.00   11.50    --   15.83 -57.00 -30.00   90
  6  \w     -6.00  85.00   1.00   11.50    --   15.83  57.00 120.00   91
  7  \w     -6.00  85.00   1.00   11.50    --   15.83  57.00 -30.00   91
  8  \w     -6.00  85.00   1.00   11.50    --   15.83  57.00-120.00   91
  9  \w    -42.00  46.00   1.00   11.50    --   15.83 -77.00  90.00   88
 10  \w     11.00  79.00   1.00   11.50    --   15.83-134.00 -57.01   68
 11  \w    -87.00  11.00   1.00   11.50    --  -14.81 -38.00  30.00   98
 12  \w    -79.00 -12.00   1.00   11.50    --  -14.81 136.00 148.96   67
 13  \w    -15.00  58.00   1.00   11.50    --   15.83 -99.00   0.00   73
 14  \w      2.00  71.00   1.00   11.50    --   15.83-121.00  79.78   69
 15  \w    -57.00  89.00   1.00   11.50    --   15.83   0.00-180.00  146
 16  \w      8.00  75.00   1.00   11.50    --   15.83-128.00  26.37   67
 17  \w    -57.00  89.00   1.00   11.50    --   15.83   0.00-120.00  146
 18  \w    -57.00  73.00   1.00   11.50    --   15.83   0.00 -90.00  130
 19  \w    -57.00  89.00   1.00   11.50    --   15.83   0.00-150.00  146
;
_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      -0.0157567000
_diffrn_orient_matrix_UB_12      0.0289965000
_diffrn_orient_matrix_UB_13      -0.0098084000
_diffrn_orient_matrix_UB_21      0.0430386000
_diffrn_orient_matrix_UB_22      0.0129198000
_diffrn_orient_matrix_UB_23      0.0016228000
_diffrn_orient_matrix_UB_31      0.0073610000
_diffrn_orient_matrix_UB_32      -0.0133669000
_diffrn_orient_matrix_UB_33      -0.0197208000
_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  0.1634
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            221389
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        20.812
_diffrn_reflns_theta_max         20.812
_diffrn_reflns_theta_min         2.843
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.842
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84963
_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    1.616
_exptl_crystal_description       plank
_exptl_crystal_F_000             4888
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.174
_refine_diff_density_min         -2.251
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1321
_refine_ls_number_reflns         10599
_refine_ls_number_restraints     1235
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.1181
_refine_ls_R_factor_gt           0.0795
_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^)+(0.1180P)^2^+220.5871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1942
_refine_ls_wR_factor_ref         0.2288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7452
_reflns_number_total             10599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc07042a2.cif
_cod_data_source_block           sx975
_cod_original_formula_sum        'C28.50 H19 Ce N0.50 O6.75'
_cod_database_code               1574052
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O Ce'
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.745
_olex2_refinement_description
;
1. Restrained distances
 Ce3-O27 \\sim Ce3-O28
 with sigma of 0.02
 O27-C110 \\sim O28-C113
 with sigma of 0.02
 C110-N041 \\sim C113-N0
 with sigma of 0.02
 N041-C112 \\sim N0-C115
 with sigma of 0.02
 N041-C111 \\sim N0-C114
 with sigma of 0.02
 Ce3-C110 \\sim Ce3-C113
 with sigma of 0.04
 O27-N041 \\sim O28-N0
 with sigma of 0.04
 C110-C112 \\sim C113-C115
 with sigma of 0.04
 C110-C111 \\sim C113-C114
 with sigma of 0.04
 C112-C111 \\sim C115-C114
 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
O27 \\sim C110 \\sim N041 \\sim C112 \\sim C111 \\sim O28 \\sim C113 \\sim N0
\\sim C115 \\sim C114: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
C115 \\sim N0 \\sim C114: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O27, C110, N041, C112, C111
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O28, C113, N0, C115, C114
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O28)=Sof(C113)=Sof(H113)=Sof(N0)=Sof(C115)=Sof(H11G)=Sof(H11H)=Sof(H11I)=
 Sof(C114)=Sof(H11J)=Sof(H11K)=Sof(H11L)=1-FVAR(1)
 Sof(O27)=Sof(C110)=Sof(H110)=Sof(N041)=Sof(C112)=Sof(H11A)=Sof(H11B)=
 Sof(H11C)=Sof(C111)=Sof(H11D)=Sof(H11E)=Sof(H11F)=FVAR(1)
5.a Rotating group:
 O25(H25A,H25B)
5.b Me refined with riding coordinates:
 C109(H10A,H10B,H10C), C108(H10D,H10E,H10F), C112(H11A,H11B,H11C), C111(H11D,
 H11E,H11F), C115(H11G,H11H,H11I), C114(H11J,H11K,H11L)
5.c Aromatic/amide H refined with riding coordinates:
 C49(H49), C40(H40), C38(H38), C13(H13), C36(H36), C50(H50), C01B(H01B),
 C9(H9), C22(H22), C102(H102), C101(H101), C30(H30), C52(H52), C79(H79),
 C23(H23), C25(H25), C91(H91), C11(H11), C6(H6), C78(H78), C89(H89), C59(H59),
 C98(H98), C26(H26), C76(H76), C53(H53), C87(H87), C83(H83), C19(H19), C84(H84),
  C104(H104), C33(H33), C86(H86), C60(H60), C66(H66), C105(H105), C3(H3),
 C57(H57), C97(H97), C64(H64), C7(H7), C62(H62), C95(H95), C31(H31), C42(H42),
 C56(H56), C43(H43), C34(H34), C18(H18), C4(H4), C16(H16), C45(H45), C46(H46),
 C15(H15), C75(H75), C72(H72), C107(H107), C68(H68), C94(H94), C71(H71),
 C69(H69), C110(H110), C113(H113)
;
_shelx_res_checksum              94207
_shelx_hkl_checksum              64231
_olex2_date_sample_data_collection 2022-01-11
_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 1.226
_oxdiff_exptl_absorpt_empirical_full_min 0.907