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_7714950
_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 H62 Fe8 Ho2 N10 O26, 6(Cl O4), 2(H2 O), 1[]'
_chemical_formula_sum            'C61 H66 Cl6 Fe8 Ho2 N10 O52'
_chemical_formula_weight         2760.59
_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             2023-12-09
_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                 91.7300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.7852(2)
_cell_length_b                   13.5126(2)
_cell_length_c                   27.5746(3)
_cell_measurement_reflns_used    14440
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      69.1910
_cell_measurement_theta_min      3.1980
_cell_volume                     5134.09(12)
_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)'
_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 0.991
_diffrn_measured_fraction_theta_max 0.976
_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    -82.00 -24.00   0.50    0.50    --  -42.27  97.00-103.00  116
  2  \w     -3.00  27.00   0.50    0.50    --  -42.27  97.00-103.00   60
  3  \w     10.00  46.00   0.50    0.50    --   42.27 -97.00 148.00   72
  4  \w    -78.00 -52.00   0.50    4.00    --  -96.00  97.00-103.00   52
  5  \w     23.00 104.00   0.50    4.00    --   97.05 -97.00 148.00  162
  6  \w    114.00 139.00   0.50    4.00    --   97.05  97.00-103.00   50
  7  \w    -27.00  39.00   0.50    0.50    --  -42.27  19.00  30.00  132
  8  \w    -19.00  38.00   0.50    0.50    --  -42.27  19.00 -30.00  114
  9  \w     59.00 117.00   0.50    0.50    --   42.27  57.00 -30.00  116
 10  \w     57.00  82.00   0.50    0.50    --   42.27 -97.00 148.00   50
 11  \w    -46.00 -21.00   0.50    4.00    --  -96.00  45.00-150.00   50
 12  \w    -51.00 -20.00   0.50    4.00    --  -96.00  45.00 120.00   62
 13  \w    -51.00 -19.00   0.50    4.00    --  -96.00  45.00  60.00   64
 14  \w    -65.00 -24.00   0.50    4.00    --  -96.00  61.00-120.00   82
 15  \w    -51.00 -25.00   0.50    4.00    --  -96.00  45.00  90.00   52
 16  \w    -51.00 -19.00   0.50    4.00    --  -96.00  45.00-120.00   64
 17  \w    -71.00 -33.00   0.50    4.00    --  -96.00  61.00   0.00   76
 18  \w   -153.00 -88.00   0.50    4.00    --  -96.00 -97.00 148.00  130
 19  \w    -50.00 -20.00   0.50    4.00    --  -96.00  45.00-180.00   60
 20  \w    -72.00 -43.00   0.50    4.00    --  -96.00  61.00-150.00   58
 21  \w     25.00  50.00   0.50    4.00    --   97.05 -61.00  90.00   50
 22  \w     28.00  69.00   0.50    4.00    --   97.05 -61.00  30.00   82
 23  \w    141.00 166.00   0.50    4.00    --   97.05 125.00 -30.00   50
 24  \w     24.00  50.00   0.50    4.00    --   97.05 -61.00 -60.00   52
 25  \w     32.00  58.00   0.50    4.00    --   97.05 -61.00   0.00   52
 26  \w     21.00  51.00   0.50    4.00    --   97.05 -45.00-120.00   60
 27  \w     78.00 103.00   0.50    4.00    --   97.05 -77.00-180.00   50
 28  \w    101.00 126.00   0.50    4.00    --   97.05 125.00 -30.00   50
 29  \w     22.00  48.00   0.50    4.00    --   97.05 -77.00-180.00   52
 30  \w     20.00  51.00   0.50    4.00    --   97.05 -45.00 -30.00   62
 31  \w     25.00  50.00   0.50    4.00    --   97.05 -45.00-150.00   50
 32  \w     20.00  45.00   0.50    4.00    --   97.05 -45.00 -60.00   50
;
_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      -0.0271394000
_diffrn_orient_matrix_UB_12      0.0985260000
_diffrn_orient_matrix_UB_13      0.0241563000
_diffrn_orient_matrix_UB_21      0.1011866000
_diffrn_orient_matrix_UB_22      0.0418191000
_diffrn_orient_matrix_UB_23      -0.0106908000
_diffrn_orient_matrix_UB_31      -0.0391166000
_diffrn_orient_matrix_UB_32      0.0392479000
_diffrn_orient_matrix_UB_33      -0.0492498000
_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  0.0430
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            33887
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.353
_diffrn_reflns_theta_min         3.207
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.786
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26705
_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    1.786
_exptl_crystal_description       block
_exptl_crystal_F_000             2724
_refine_diff_density_max         1.377
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         9406
_refine_ls_number_restraints     687
_refine_ls_restrained_S_all      14.016
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1429P)^2^+4.8802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1942
_refine_ls_wR_factor_ref         0.2052
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7727
_reflns_number_total             9406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03832g2.cif
_cod_data_source_block           Ho2Fe8
_cod_depositor_comments
'Adding full bibliography for 7714948--7714952.cif.'
_cod_database_code               7714950
_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
 Cl2-O28 = Cl2-O27_$1 = Cl2-O26 = Cl2-O25
 1.42 with sigma of 0.01
 C25-C01W_$2
 1.52 with sigma of 0.01
 Fe4-O13 \\sim Fe4-O14
 with sigma of 0.02
 O13-C35 \\sim O14-C35
 with sigma of 0.02
 Cl1-O24 \\sim Cl1-O23
 with sigma of 0.02
 Ho1-H11A \\sim Ho1-H11B
 with sigma of 0.02
 Ho1-H9A \\sim Ho1-H9B
 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(O27) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O24)
\\sim Ueq, Uanis(C01W) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C31) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C33)
\\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C35) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(Cl2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: H2(0.5) O13(0.5) O24(0.5) C28(0.5) H28(0.5) C31(0.5) H31(0.5)
 N5(0.5) C34(0.5) C33(0.5) H33(0.5) C32(0.5) H32(0.5) C35(0.5) H35(0.5)
 C01W(0.5) O14(0.5) N4(0.5) C30(0.5) C29(0.5) C27(0.5) C26(0.5) C25(0.5)
 O23(0.5) C36(0.5)
5.a Free rotating group:
 O11(H11A,H11B), O9(H9A,H9B), O15(H,HA)
5.b Rotating group:
 O8(H8A,H8B)
5.c Ternary CH refined with riding coordinates:
 O2(H2)
5.d Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C20(H20A,H20B)
5.e Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C11(H11), C1(H1), C15(H15), C4(H4), C3(H3), C18(H18),
 C12(H12), C2(H2A), C24(H24), C10(H10), C9(H9), C17(H17), C16(H16), C23(H23),
 C21(H21), C22(H22), C28(H28), C31(H31), C33(H33), C32(H32), C35(H35)
5.f Fitted hexagon refined as free rotating group:
 C28(C31,N5,C34,C33,C32), N4(C30,C29,C27,C26,C25)
;
_shelx_res_checksum              93185
_shelx_fab_checksum              9180
_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 2.117
_oxdiff_exptl_absorpt_empirical_full_min 0.669