Synthesis, structures, and magnetic properties of butterfly-shaped hexanuclear [FeIII4LnIII2] single-molecule magnets
Liu, Shujing; Zou, Chen; Wang, Hanjie; Chen, Sihuai; Yuan, Jun; Jia, Lihui; CrystEngComm 25 (2023) 5893–5899; doi:10.1039/D3CE00824J

data_7247427
_publ_section_title
;
 Synthesis, structures, and magnetic properties of butterfly-shaped
 hexanuclear [FeIII4LnIII2] single-molecule magnets
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              5893
_journal_page_last               5899
_journal_paper_doi               10.1039/D3CE00824J
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C30 H72 Fe4 N10 O28 Y2, 4(C H4 O)'
_chemical_formula_sum            'C34 H88 Fe4 N10 O32 Y2'
_chemical_formula_weight         1550.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-01
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-03 deposited with the CCDC.	2023-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                79.542(3)
_cell_angle_beta                 79.911(2)
_cell_angle_gamma                75.815(2)
_cell_formula_units_Z            1
_cell_length_a                   10.8225(3)
_cell_length_b                   11.1813(3)
_cell_length_c                   12.9331(4)
_cell_measurement_reflns_used    22732
_cell_measurement_temperature    293
_cell_measurement_theta_max      73.9390
_cell_measurement_theta_min      4.1180
_cell_volume                     1478.02(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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     61.00  87.00   0.50    0.50    --   12.00  71.00 -73.36   52
  2  \w    -13.00  42.00   0.50    0.50    --   12.00  71.00 -73.36  110
  3  \w    -57.00  52.00   0.50    0.50    --   32.00 -51.00-110.05  218
  4  \w      6.00  58.00   0.50    0.50    --   40.00 -43.00 -25.16  104
  5  \w     57.00 110.00   0.50    0.50    --   44.00  72.00-135.75  106
  6  \w     17.00  45.00   0.50    0.50    --   44.00  72.00-135.75   56
  7  \w     22.00  50.00   0.50    0.50    --   48.00  70.00  36.86   56
  8  \w     32.00  78.00   0.50    0.50    --   52.00  75.00 119.06   92
  9  \w     29.00  58.00   0.50    0.50    --   56.00  73.00 -57.70   58
 10  \w     89.00 116.00   0.50    0.50    --   56.00  73.00 -57.70   54
 11  \w     29.00  54.00   0.50    0.50    --   56.00  73.00  77.91   50
 12  \w     36.00  62.00   0.50    0.50    --   64.00  75.00-169.98   52
 13  \w     41.00  67.00   0.50    0.50    --   68.00  73.00-121.00   52
 14  \w     40.00  67.00   0.50    0.50    --   68.00  74.00 -34.30   54
 15  \w     40.00  66.00   0.50    0.50    --   68.00  75.00 111.92   52
 16  \w     40.00  70.00   0.50    0.50    --   68.00  75.00  72.67   60
 17  \w     44.00  74.00   0.50    0.50    --   72.00  74.00  17.85   60
 18  \w     44.00  81.00   0.50    0.50    --   72.00  75.00-158.46   74
 19  \w     48.00  77.00   0.50    0.50    --   76.00  74.00 138.40   58
 20  \w    129.00 165.00   0.50    0.50    --   76.00  72.00-116.56   72
 21  \w     49.00  78.00   0.50    0.50    --   76.00  74.00 -63.70   58
 22  \w     49.00  79.00   0.50    0.50    --   76.00  72.00-116.56   60
 23  \w     48.00  74.00   0.50    0.50    --   76.00  74.00  35.07   52
 24  \w     48.00  77.00   0.50    0.50    --   76.00  74.00 -15.65   58
 25  \w     57.00  86.00   0.50    0.50    --   80.00  67.00 129.51   58
 26  \w     87.00 156.00   0.50    0.50    --   80.00  69.00 -76.26  138
 27  \w     54.00  82.00   0.50    0.50    --   80.00  69.00 -76.26   56
 28  \w     58.00  96.00   0.50    0.50    --   84.00  70.00 -25.78   76
 29  \w     59.00 132.00   0.50    0.50    --   84.00  68.00  55.54  146
 30  \w    101.00 169.00   0.50    0.50    --   84.00  65.00  73.29  136
 31  \w    115.00 172.00   0.50    0.50    --   84.00  74.00 160.97  114
 32  \w     60.00  87.00   0.50    0.50    --   84.00  65.00  73.29   54
 33  \w     56.00 109.00   0.50    0.50    --   84.00  74.00 160.97  106
 34  \w    102.00 150.00   0.50    0.50    --   84.00  70.00 -25.78   96
 35  \w      6.00 105.00   0.50    0.50    --   95.20 -82.00 -90.00  198
 36  \w     72.00 162.00   0.50    0.50    --   95.20  61.00-150.00  180
 37  \w     77.00 145.00   0.50    0.50    --   95.20  45.00 150.00  136
 38  \w      7.00 104.00   0.50    0.50    --   95.20 -82.00  90.00  194
 39  \w      8.00  95.00   0.50    0.50    --   95.20 -61.00 150.00  174
 40  \w      6.00 106.00   0.50    0.50    --   95.20 -61.00 -30.00  200
 41  \w     72.00 147.00   0.50    0.50    --   95.20  61.00-120.00  150
 42  \w     72.00 184.00   0.50    0.50    --   95.20  64.00   9.58  224
 43  \w     57.00 109.00   0.50    0.50    --   95.20 -82.00-120.00  104
 44  \w     75.00 136.00   0.50    0.50    --   95.20  61.00  90.00  122
 45  \w     30.00 113.00   0.50    0.50    --   95.20 -82.00 150.00  166
 46  \w    160.00 185.00   0.50    0.50    --   95.20  45.00-150.00   50
 47  \w    126.00 151.00   0.50    0.50    --   95.20  45.00-150.00   50
 48  \w      6.00 123.00   0.50    0.50    --   95.20 -82.00 -30.00  234
 49  \w     83.00 108.00   0.50    0.50    --   95.20  45.00-150.00   50
 50  \w    159.00 185.00   0.50    0.50    --   95.20  77.00-120.00   52
 51  \w     89.00 114.00   0.50    0.50    --   95.20  77.00-120.00   50
 52  \w     74.00 100.00   0.50    0.50    --   95.20  61.00   0.00   52
 53  \w    105.00 158.00   0.50    0.50    --   95.20  61.00   0.00  106
 54  \w    141.00 167.00   0.50    0.50    --   95.20  61.00 150.00   52
 55  \w     72.00 122.00   0.50    0.50    --   95.20  61.00 150.00  100
 56  \w     87.00 145.00   0.50    0.50    --   95.20  77.00 -90.00  116
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0350226000
_diffrn_orient_matrix_UB_12      0.0179247000
_diffrn_orient_matrix_UB_13      0.1177245000
_diffrn_orient_matrix_UB_21      0.1439984000
_diffrn_orient_matrix_UB_22      -0.0310320000
_diffrn_orient_matrix_UB_23      0.0120016000
_diffrn_orient_matrix_UB_31      0.0029248000
_diffrn_orient_matrix_UB_32      0.1390936000
_diffrn_orient_matrix_UB_33      -0.0308277000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31026
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.596
_diffrn_reflns_theta_max         66.596
_diffrn_reflns_theta_min         5.012
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.040
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_refine_diff_density_max         3.054
_refine_diff_density_min         -1.261
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         5192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0783
_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^)+58.2538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2215
_refine_ls_wR_factor_ref         0.2218
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5016
_reflns_number_total             5192
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00824j2.cif
_cod_data_source_block           20230629_l-32
_cod_depositor_comments
'Adding full bibliography for 7247426--7247427.cif.'
_cod_database_code               7247427
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Riding coordinates:
 O7(H7A,H7B), O9(H9), C4(H4A,H4B), C5(H5A,H5B), O15(H15)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C6(H6A,H6B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,
 H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C7(H7C,H7D)
2.c Tetrahedral OH refined with riding coordinates:
 O16(H16)
2.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C)
;
_shelx_res_checksum              12513
_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 6.323
_oxdiff_exptl_absorpt_empirical_full_min 0.341