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_7714949
_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
'C60 H72 Fe8 N10 O26 Tb2, 6(Cl O4), 2(H2 O), 1[], 1[]'
_chemical_formula_sum            'C60 H78 Cl6 Fe8 N10 O49 Tb2'
_chemical_formula_weight         2700.66
_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             2023-12-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-16 deposited with the CCDC.	2024-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.360(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6194(4)
_cell_length_b                   13.4851(3)
_cell_length_c                   27.7249(5)
_cell_measurement_reflns_used    10014
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      65.2490
_cell_measurement_theta_min      3.5680
_cell_volume                     5090.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (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 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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    -95.00 -16.00   1.00    1.35    --  -42.21 -75.00 168.00   79
  2  \w    -72.00  32.00   1.00    1.35    --  -42.21  75.00 -64.00  104
  3  \w     41.00  66.00   1.00    1.35    --   43.14  75.00 -64.00   25
  4  \w     -3.00  22.00   1.00    1.35    --   43.14 -75.00 168.00   25
  5  \w   -135.00-110.00   1.00    5.40    --  -88.58 -75.00 168.00   25
  6  \w    -82.00 -14.00   1.00    5.40    --  -88.58  75.00 -64.00   68
  7  \w     16.00  92.00   1.00    5.40    --   89.52 -75.00 168.00   76
  8  \w     71.00 145.00   1.00    5.40    --   89.52  75.00 -64.00   74
  9  \w   -111.00 -71.00   1.00    1.35    --  -42.21-125.00-120.00   40
 10  \w   -103.00 -77.00   1.00    1.35    --  -42.21-125.00 -60.00   26
 11  \w    -47.00 -13.00   1.00    5.40    --  -88.58  45.00 -60.00   34
 12  \w    -51.00 -14.00   1.00    5.40    --  -88.58  45.00 -90.00   37
 13  \w    -36.00 -11.00   1.00    5.40    --  -88.58  30.00  60.00   25
 14  \w    -36.00 -11.00   1.00    5.40    --  -88.58  30.00 -90.00   25
 15  \w    -36.00  -9.00   1.00    5.40    --  -88.58  30.00 -60.00   27
 16  \w    -50.00 -16.00   1.00    5.40    --  -88.58  45.00 150.00   34
 17  \w    -36.00 -10.00   1.00    5.40    --  -88.58  30.00-120.00   26
 18  \w    -51.00 -13.00   1.00    5.40    --  -88.58  45.00-120.00   38
 19  \w     10.00  36.00   1.00    5.40    --   89.52 -30.00  30.00   26
 20  \w     13.00  39.00   1.00    5.40    --   89.52 -45.00   0.00   26
 21  \w     13.00  51.00   1.00    5.40    --   89.52 -45.00  30.00   38
 22  \w     10.00  35.00   1.00    5.40    --   89.52 -30.00 150.00   25
 23  \w     18.00  70.00   1.00    5.40    --   89.52 -61.00 -30.00   52
 24  \w     10.00  35.00   1.00    5.40    --   89.52 -30.00  60.00   25
 25  \w     10.00  35.00   1.00    5.40    --   89.52 -30.00 -60.00   25
 26  \w     11.00  36.00   1.00    5.40    --   89.52 -30.00   0.00   25
 27  \w     13.00  51.00   1.00    5.40    --   89.52 -45.00 -30.00   38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0798171000
_diffrn_orient_matrix_UB_12      0.0578120000
_diffrn_orient_matrix_UB_13      -0.0285223000
_diffrn_orient_matrix_UB_21      -0.0072059000
_diffrn_orient_matrix_UB_22      0.0744510000
_diffrn_orient_matrix_UB_23      0.0418709000
_diffrn_orient_matrix_UB_31      0.0798545000
_diffrn_orient_matrix_UB_32      0.0645556000
_diffrn_orient_matrix_UB_33      -0.0228696000
_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  0.0520
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            31963
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        65.553
_diffrn_reflns_theta_max         65.553
_diffrn_reflns_theta_min         3.189
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.794
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_description       block
_exptl_crystal_F_000             2680
_refine_diff_density_max         1.417
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         8576
_refine_ls_number_restraints     451
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0816
_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^)+(0.1273P)^2^+39.3001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2179
_refine_ls_wR_factor_ref         0.2413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6426
_reflns_number_total             8576
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03832g2.cif
_cod_data_source_block           Tb2Fe8
_cod_depositor_comments
'Adding full bibliography for 7714948--7714952.cif.'
_cod_database_code               7714949
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 Tb1-H6A \\sim Tb1-H6B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(O23) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(Cl3)
\\sim Ueq, Uanis(O22) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C30) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O26(0.5) O16(0.5) O27(0.5)
5.a Free rotating group:
 O6(H6A,H6B), O18(H18A,H18B)
5.b Rotating group:
 O7(H7A,H7B), O5(H5A,H5B)
5.c Ternary CH refined with riding coordinates:
 O3(H3)
5.d Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C13(H13A,H13B), C24(H24A,H24B), C25(H25A,H25B)
5.e Aromatic/amide H refined with riding coordinates:
 C5(H5), C15(H15), C18(H18), C6(H6), C2(H2), C12(H12), C3(H3A), C11(H11),
 C4(H4), C17(H17), C16(H16), C9(H9), C10(H10), C22(H22), C19(H19), C20(H20),
 C21(H21), C27(H27), C28(H28), C29(H29), C30(H30)
5.f Fitted hexagon refined as free rotating group:
 C22(C23,N4,C19,C20,C21), C26(C27,C28,C29,C30,N5)
5.g Idealised tetrahedral OH refined as rotating group:
 O13(H13)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              99660
_shelx_fab_checksum              31857
_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 1.467
_oxdiff_exptl_absorpt_empirical_full_min 0.768