Single-molecule magnet behavior in heterometallic decanuclear [Ln<sub>2</sub>Fe<sub>8</sub>] (Ln = Y, Dy, Ho, Tb, Gd) coordination clusters.
Chen, Man-Ting; Zhao, Hai-Xia; Long, La-Sheng; Zheng, Lan-Sun; Dalton transactions (Cambridge, England : 2003) 53 (2024) 3097–3103; doi:10.1039/d3dt03832g

data_7714948
_publ_section_title
;
 Single-molecule magnet behavior in heterometallic decanuclear
 [Ln<sub>2</sub>Fe<sub>8</sub>] (Ln = Y, Dy, Ho, Tb, Gd) coordination
 clusters.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3097
_journal_page_last               3103
_journal_paper_doi               10.1039/d3dt03832g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C61 H80 Fe8 N10 O26 Y2, 6(Cl O4)'
_chemical_formula_sum            'C61 H80 Cl6 Fe8 N10 O50 Y2'
_chemical_formula_weight         2590.67
_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
_audit_creation_date             2022-07-28
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-10 deposited with the CCDC.	2024-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.845(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.7425(3)
_cell_length_b                   13.5084(2)
_cell_length_c                   27.6067(4)
_cell_measurement_reflns_used    13949
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      70.3960
_cell_measurement_theta_min      3.2010
_cell_volume                     5122.23(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.967
_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     28.00  68.00   0.50    0.98    --   92.20 -57.00-180.00   80
  2  \w     20.00  97.00   0.50    0.98    --   92.20 -77.00-180.00  154
  3  \w     78.00 104.00   0.50    0.98    --   92.20 -77.00-120.00   52
  4  \w     29.00  73.00   0.50    0.98    --   92.20 -77.00-120.00   88
  5  \w     25.00  64.00   0.50    0.98    --   92.20 -57.00-120.00   78
  6  \w     22.00  68.00   0.50    0.98    --   92.20 -57.00 120.00   92
  7  \w     82.00 167.00   0.50    0.98    --   92.20  21.00 123.00  170
  8  \w     81.00 163.00   0.50    0.98    --   92.20  38.00  30.00  164
  9  \w    -63.00 -23.00   0.50    0.98    --  -94.70 125.00-180.00   80
 10  \w    -69.00 -44.00   0.50    0.98    --  -94.70 125.00-120.00   50
 11  \w   -110.00 -84.00   0.50    0.98    --  -94.70 125.00-180.00   52
 12  \w   -109.00 -76.00   0.50    0.98    --  -94.70 125.00-120.00   66
 13  \w    -64.00 -34.00   0.50    0.98    --  -94.70  57.00 120.00   60
 14  \w    -61.00 -24.00   0.50    0.98    --  -94.70  57.00  90.00   74
 15  \w    -63.00 -24.00   0.50    0.98    --  -94.70  57.00  60.00   78
 16  \w     14.00  47.00   0.50    0.25    --   -1.25  21.00 123.00   66
 17  \w    -62.00 -26.00   0.50    0.98    --  -94.70  57.00  30.00   72
 18  \w    -63.00 -38.00   0.50    0.98    --  -94.70  57.00   0.00   50
 19  \w    -64.00 -39.00   0.50    0.98    --  -94.70  57.00 -30.00   50
 20  \w   -124.00 -90.00   0.50    0.98    --  -94.70 -21.00 -42.00   68
 21  \w   -161.00-136.00   0.50    0.98    --  -94.70 -21.00 -42.00   50
 22  \w    -76.00   6.00   0.50    0.25    --   -1.25 -21.00 -42.00  164
 23  \w    -18.00  26.00   0.50    0.25    --   -1.25 -99.00-150.00   88
 24  \w    -17.00  29.00   0.50    0.25    --   -1.25 -99.00  90.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0620773000
_diffrn_orient_matrix_UB_12      0.0245331000
_diffrn_orient_matrix_UB_13      0.0458843000
_diffrn_orient_matrix_UB_21      -0.0933417000
_diffrn_orient_matrix_UB_22      0.0210373000
_diffrn_orient_matrix_UB_23      0.0277147000
_diffrn_orient_matrix_UB_31      -0.0040350000
_diffrn_orient_matrix_UB_32      -0.1093477000
_diffrn_orient_matrix_UB_33      0.0156278000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            34779
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.272
_diffrn_reflns_theta_min         3.203
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.514
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_description       block
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.262
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         9628
_refine_ls_number_restraints     260
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0701
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1123P)^2^+19.3620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1879
_refine_ls_wR_factor_ref         0.2089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7204
_reflns_number_total             9628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03832g2.cif
_cod_data_source_block           Y2Fe8
_cod_depositor_comments
'Adding full bibliography for 7714948--7714952.cif.'
_cod_database_code               7714948
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     2205181116
_shelx_estimated_absorpt_t_max   0.368
_shelx_estimated_absorpt_t_min   0.189
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H32 of O32, H31 of O31, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H6A of O6A, All O(H,H) groups
2. Restrained distances
 Y1-H18A \\sim Y1-H18B
 with sigma of 0.02
 Fe1-O6B \\sim Fe1-O6A \\sim Fe3-O6A \\sim Fe3-O6B
 with sigma of 0.01
3. Rigid bond restraints
 C24, N5
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
N2 \\sim C25 \\sim C7 \\sim C27 \\sim C13 \\sim C3: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
O17 \\sim Cl1 \\sim O25 \\sim O2 \\sim O19: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
O21 \\sim Cl2 \\sim O11 \\sim O23 \\sim O3: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
N2 \\sim C25 \\sim C29 \\sim C7 \\sim C27 \\sim C13 \\sim C3 \\sim N32 \\sim
C33 \\sim C37 \\sim C35 \\sim C38 \\sim C34 \\sim O22 \\sim C31 \\sim O6B \\sim
C36: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O6A \\sim O6B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
5. Others
 Fixed Sof: O6B(0.5) N2(0.5) C25(0.5) H25(0.5) C29(0.5) H29(0.5) C7(0.5)
 H7(0.5) C27(0.5) H27(0.5) C13(0.5) C3(0.5) H3A(0.5) H3B(0.5) C36(0.5)
 H36A(0.5) H36B(0.5) C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5) C38(0.5) H38(0.5)
 C33(0.5) H33(0.5) N32(0.5) C31(0.5) C35(0.5) H35(0.5) C34(0.5) H34(0.5)
 O6A(0.5) H6A(0.5)
6.a Riding coordinates:
 O13(H13A,H13B)
6.b Free rotating group:
 O18(H18A,H18B)
6.c Rotating group:
 O20(H20A,H20B)
6.d Ternary CH refined with riding coordinates:
 O6A(H6A)
6.e Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C12(H12A,H12B), C14(H14A,H14B), C19(H19A,H19B), C3(H3A,H3B),
 C36(H36A,H36B)
6.f Me refined with riding coordinates:
 C37(H37A,H37B,H37C)
6.g Aromatic/amide H refined with riding coordinates:
 O31(H31), O32(H32), C10(H10), C25(H25), C29(H29), C7(H7), C27(H27), C16(H16),
 C18(H18), C20(H20), C22(H22), C26(H26), C28(H28), C30(H30), C15(H15), C2(H2),
 C17(H17), C9(H9), C5(H5), C21(H21), C11(H11), C23(H23), C38(H38), C33(H33),
 C35(H35), C34(H34)
6.h Fitted hexagon refined as free rotating group:
 N2(C25,C29,C7,C27,C13), C38(C33,N32,C31,C35,C34)
;
_shelx_res_checksum              30606
_shelx_fab_checksum              84404
_platon_squeeze_void_probe_radius 1.20
_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 2.231
_oxdiff_exptl_absorpt_empirical_full_min 0.702