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_7714952
_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 Dy2 Fe8 N10 O26, 6(Cl O4)'
_chemical_formula_sum            'C61 H80 Cl6 Dy2 Fe8 N10 O50'
_chemical_formula_weight         2737.85
_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                 91.624(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6830(4)
_cell_length_b                   13.4980(3)
_cell_length_c                   27.6595(5)
_cell_measurement_reflns_used    11956
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      70.0550
_cell_measurement_theta_min      3.5840
_cell_volume                     5106.5(2)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.961
_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     79.00 106.00   0.50    1.08    --   92.20 125.00-180.00   54
  2  \w    117.00 164.00   0.50    1.08    --   92.20 125.00-180.00   94
  3  \w    138.00 164.00   0.50    1.08    --   92.20  57.00 -26.00   52
  4  \w     92.00 160.00   0.50    1.08    --   92.20  57.00 -90.00  136
  5  \w    -57.00 -22.00   0.50    0.27    --   -1.25 -57.00-168.00   70
  6  \w   -167.00 -97.00   0.50    1.08    --  -94.70 -57.00-168.00  140
  7  \w   -117.00 -91.00   0.50    1.08    --  -94.70 -38.00  60.00   52
  8  \w   -166.00-123.00   0.50    1.08    --  -94.70 -38.00  60.00   86
  9  \w   -162.00-137.00   0.50    1.08    --  -94.70 -19.00  60.00   50
 10  \w   -120.00 -84.00   0.50    1.08    --  -94.70 -19.00  60.00   72
 11  \w   -141.00 -87.00   0.50    1.08    --  -94.70 -99.00 -60.00  108
 12  \w   -124.00 -99.00   0.50    1.08    --  -94.70 -99.00 -30.00   50
 13  \w    -17.00  23.00   0.50    0.27    --   -1.25 -99.00-120.00   80
 14  \w      0.00  30.00   0.50    0.27    --   -1.25 -99.00  90.00   60
 15  \w    -15.00  70.00   0.50    0.27    --   -1.25  57.00 -26.00  170
 16  \w    -60.00 -22.00   0.50    1.08    --  -94.70  57.00  30.00   76
 17  \w    -63.00 -24.00   0.50    1.08    --  -94.70  57.00 -26.00   78
 18  \w    -60.00 -33.00   0.50    1.08    --  -94.70  57.00 -60.00   54
 19  \w     21.00  68.00   0.50    1.08    --   92.20 -57.00-168.00   94
 20  \w     24.00  50.00   0.50    1.08    --   92.20 -57.00-120.00   52
 21  \w     20.00  55.00   0.50    1.08    --   92.20 -57.00   0.00   70
 22  \w     20.00  67.00   0.50    1.08    --   92.20 -57.00 150.00   94
 23  \w     21.00  68.00   0.50    1.08    --   92.20 -57.00  90.00   94
;
_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      -0.1119132000
_diffrn_orient_matrix_UB_12      -0.0103266000
_diffrn_orient_matrix_UB_13      -0.0050734000
_diffrn_orient_matrix_UB_21      0.0119929000
_diffrn_orient_matrix_UB_22      -0.0769714000
_diffrn_orient_matrix_UB_23      -0.0404957000
_diffrn_orient_matrix_UB_31      0.0024919000
_diffrn_orient_matrix_UB_32      -0.0837576000
_diffrn_orient_matrix_UB_33      0.0379092000
_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  0.0517
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            31379
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.574
_diffrn_reflns_theta_min         3.197
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.773
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16006
_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    1.781
_exptl_crystal_description       block
_exptl_crystal_F_000             2716
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.287
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         9593
_refine_ls_number_restraints     347
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0701
_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^)+(0.1489P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1942
_refine_ls_wR_factor_ref         0.2118
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6806
_reflns_number_total             9593
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03832g2.cif
_cod_data_source_block           Dy2Fe8
_cod_depositor_comments
'Adding full bibliography for 7714948--7714952.cif.'
_cod_database_code               7714952
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     2205181116
_shelx_estimated_absorpt_t_max   0.255
_shelx_estimated_absorpt_t_min   0.071
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H37 of O37, H38 of O38, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H14A of O14A, All O(H,H) groups
2. Restrained distances
 H10A-H22A
 2.22 with sigma of 0.01
 Cl2-O5 \\sim Cl3-O13
 with sigma of 0.02
 Cl2-O11 \\sim Cl3-O27
 with sigma of 0.02
 Cl2-O23 \\sim Cl3-O7
 with sigma of 0.02
 Cl2-O3 \\sim Cl3-O25
 with sigma of 0.02
 O5-O11 \\sim O13-O27
 with sigma of 0.04
 O5-O23 \\sim O13-O7
 with sigma of 0.04
 O5-O3 \\sim O13-O25
 with sigma of 0.04
 O11-O23 \\sim O27-O7
 with sigma of 0.04
 O11-O3 \\sim O27-O25
 with sigma of 0.04
 O23-O3 \\sim O7-O25
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O28 \\sim C24 \\sim C26 \\sim C28 \\sim C29 \\sim O14B \\sim N2 \\sim C20 \\sim
C22 \\sim C15 \\sim N5 \\sim C35 \\sim C31 \\sim C17 \\sim C33 \\sim C2: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Cl3 \\sim O13 \\sim O7 \\sim O25 \\sim O27 \\sim O3 \\sim Cl2 \\sim O5 \\sim
O11 \\sim O23: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
4. Others
 Sof(O25)=Sof(Cl3)=Sof(O13)=Sof(O27)=Sof(O7)=1-FVAR(1)
 Sof(Cl2)=Sof(O5)=Sof(O11)=Sof(O23)=Sof(O3)=FVAR(1)
 Fixed Sof: O14B(0.5) N2(0.5) C20(0.5) H20(0.5) C22(0.5) H22(0.5) C24(0.5)
 H24(0.5) C26(0.5) H26(0.5) C28(0.5) C29(0.5) H29C(0.5) H29D(0.5) C15(0.5)
 H15A(0.5) H15B(0.5) N5(0.5) C31(0.5) C2(0.5) H2(0.5) C33(0.5) H33(0.5)
 C17(0.5) H17(0.5) C35(0.5) H35(0.5) O14A(0.5) H14A(0.5) C37(0.5) H37A(0.5)
 H37B(0.5) H37C(0.5)
5.a Rotating group:
 O16(H16A,H16B), O22(H22A,H22B), O29(H29A,H29B)
5.b Ternary CH refined with riding coordinates:
 O14A(H14A)
5.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C6(H6A,H6B), C10(H10A,H10B), C21(H21A,H21B), C29(H29C,H29D),
 C15(H15A,H15B)
5.d Me refined with riding coordinates:
 C37(H37A,H37B,H37C)
5.e Aromatic/amide H refined with riding coordinates:
 O38(H38), O37(H37), C14(H14), C16(H16), C18(H18), C20(H20), C22(H22),
 C24(H24), C26(H26), C30(H30), C32(H32), C34(H34), C36(H36), C9(H9), C19(H19),
 C11(H11), C23(H23), C3(H3), C25(H25), C13(H13), C27(H27), C7(H7), C2(H2),
 C33(H33), C17(H17), C35(H35)
5.f Fitted hexagon refined as free rotating group:
 N2(C20,C22,C24,C26,C28), N5(C31,C2,C33,C17,C35)
;
_shelx_res_checksum              76723
_shelx_fab_checksum              79295
_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 3.488
_oxdiff_exptl_absorpt_empirical_full_min 0.552