A sandwich-like heterometallic Fe<sub>7</sub>Sn<sub>6</sub> oxo cluster constructed by tessellation of an Anderson-like {Fe<sub>7</sub>} wheel for near-infrared photothermal conversion.
Tian, Xiu-Juan; Lu, Qian; Li, Shi-Li; Zhang, Xian-Ming; Chemical communications (Cambridge, England) 61 (2025) 1140–1143; doi:10.1039/d4cc05796a

data_7134045
_publ_section_title
;
 A sandwich-like heterometallic Fe<sub>7</sub>Sn<sub>6</sub> oxo cluster
 constructed by tessellation of an Anderson-like {Fe<sub>7</sub>} wheel
 for near-infrared photothermal conversion.
;
_journal_issue                   6
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1140
_journal_page_last               1143
_journal_paper_doi               10.1039/d4cc05796a
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety
'C66 H83 Fe7 N6 O42 Sn6, 2(C14 H6 Fe N2 O8), 2(H2 O)'
_chemical_formula_sum            'C94 H99 Fe9 N10 O60 Sn6'
_chemical_formula_weight         3543.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-08-27
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-03-24 deposited with the CCDC.	2024-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 129.2710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.55940(10)
_cell_length_b                   22.4100(2)
_cell_length_c                   23.2623(2)
_cell_measurement_reflns_used    80915
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      75.7830
_cell_measurement_theta_min      3.9140
_cell_volume                     6682.98(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -44.00  27.00   0.50    0.60    --    0.00 -77.00-120.00  142
  2  \w    -33.00  28.00   0.50    0.60    --    0.00 -19.00-120.00  122
  3  \w    -77.00 -34.00   0.50    0.60    --    0.00 -37.00 -30.00   86
  4  \w    -20.00  21.00   0.50    0.60    --    0.00  37.00 -90.00   82
  5  \w    -76.00 -45.00   0.50    0.60    --    0.00 -37.00  90.00   62
  6  \w    -34.00  -5.00   0.50    0.60    --    0.00 -82.00  60.00   58
  7  \w    -27.00  66.00   0.50    0.60    --    0.00  19.00 150.00  186
  8  \w    -14.00  20.00   0.50    0.60    --    0.00 -37.00 -30.00   68
  9  \w    -78.00 -38.00   0.50    0.60    --    0.00 -19.00-120.00   80
 10  \w     38.00  64.00   0.50    0.60    --    0.00  37.00 -90.00   52
 11  \w    -27.00  61.00   0.50    0.60    --    0.00  19.00-120.00  176
 12  \w    -11.00  21.00   0.50    0.60    --    0.00 -37.00  90.00   64
 13  \w      0.00  33.00   0.50    0.60    --    0.00 -82.00  60.00   66
 14  \w    -32.00  33.00   0.50    0.60    --    0.00  82.00  90.00  130
 15  \w    -20.00  80.00   0.50    0.60    --    0.00  37.00  60.00  200
 16  \w     12.00  38.00   0.50    0.60    --    0.00  82.00  30.00   52
 17  \w     74.00 100.00   0.50    3.30    --  101.00  65.00-136.72   52
 18  \w     76.00 120.00   0.50    3.30    --  101.00  59.00-113.12   88
 19  \w     80.00 131.00   0.50    3.30    --  101.00  42.00 -20.38  102
 20  \w     74.00 100.00   0.50    3.30    --  101.00  65.00  39.84   52
 21  \w    157.00 189.00   0.50    3.30    --  101.00  59.00  99.75   64
 22  \w    127.00 153.00   0.50    3.30    --  101.00  60.00 169.29   52
 23  \w     80.00 186.00   0.50    3.30    --  101.00  40.00 135.39  212
 24  \w     76.00 102.00   0.50    3.30    --  101.00  58.00 -74.33   52
 25  \w     72.00  97.00   0.50    3.30    --  101.00  72.00-109.21   50
 26  \w     77.00 103.00   0.50    3.30    --  101.00  55.00 -22.00   52
 27  \w     75.00 100.00   0.50    3.30    --  101.00  61.00  80.11   50
 28  \w    144.00 180.00   0.50    3.30    --  101.00  61.00  80.11   72
 29  \w     71.00  97.00   0.50    3.30    --  101.00  74.00 107.27   52
 30  \w    164.00 190.00   0.50    3.30    --  101.00  74.00 107.27   52
 31  \w     77.00 103.00   0.50    3.30    --  101.00  55.00  29.51   52
 32  \w     76.00 105.00   0.50    3.30    --  101.00  59.00  99.75   58
 33  \w     75.00 101.00   0.50    3.30    --  101.00  61.00 160.08   52
 34  \w     76.00 102.00   0.50    3.30    --  101.00  60.00 169.29   52
 35  \w     74.00 101.00   0.50    3.30    --  101.00  67.00-179.57   54
 36  \w     74.00 100.00   0.50    3.30    --  101.00  65.00-113.42   52
 37  \w    104.00 190.00   0.50    3.30    --  101.00  70.00  51.83  172
 38  \w    116.00 160.00   0.50    3.30    --  101.00  67.00-109.46   88
 39  \w     79.00 189.00   0.50    3.30    --  101.00  47.00  35.49  220
 40  \w     77.00 147.00   0.50    3.30    --  101.00  56.00-168.05  140
 41  \w     74.00  99.00   0.50    3.30    --  101.00  67.00  23.25   50
 42  \w     75.00 101.00   0.50    3.30    --  101.00  62.00 -12.18   52
 43  \w     72.00  97.00   0.50    3.30    --  101.00  72.00 125.82   50
 44  \w     71.00  96.00   0.50    3.30    --  101.00  73.00  22.97   50
 45  \w    133.00 167.00   0.50    3.30    --  101.00  68.00 -83.71   68
 46  \w     73.00  99.00   0.50    3.30    --  101.00  68.00 -83.71   52
 47  \w     73.00  98.00   0.50    3.30    --  101.00  70.00  51.83   50
 48  \w     15.00  75.00   0.50    3.30    --  101.00 -82.00 -30.00  120
 49  \w     90.00 116.00   0.50    3.30    --  101.00 -82.00 -30.00   52
 50  \w     74.00  99.00   0.50    3.30    --  101.00  67.00-168.11   50
 51  \w     77.00 103.00   0.50    3.30    --  101.00  57.00  77.92   52
 52  \w     71.00  97.00   0.50    3.30    --  101.00  73.00-164.02   52
 53  \w     74.00 112.00   0.50    3.30    --  101.00  67.00-109.46   76
 54  \w     32.00 133.00   0.50    3.30    --  101.00 -82.00-120.00  202
 55  \w     25.00 134.00   0.50    3.30    --  101.00 -82.00  30.00  218
 56  \w     79.00 104.00   0.50    3.30    --  101.00  48.00   2.53   50
 57  \w    115.00 190.00   0.50    3.30    --  101.00  67.00 -32.10  150
 58  \w     76.00 101.00   0.50    3.30    --  101.00  58.00 116.37   50
 59  \w     77.00 107.00   0.50    3.30    --  101.00  57.00  60.00   60
 60  \w     77.00 103.00   0.50    3.30    --  101.00  57.00-180.00   52
 61  \w     77.00 103.00   0.50    3.30    --  101.00  57.00 -60.00   52
 62  \w     78.00 105.00   0.50    3.30    --  101.00  57.00 150.00   54
 63  \w     71.00  97.00   0.50    3.30    --  101.00  74.00 -73.25   52
 64  \w     80.00 174.00   0.50    3.30    --  101.00  49.00 150.62  188
 65  \w     78.00 103.00   0.50    3.30    --  101.00  57.00  90.00   50
 66  \w     74.00 100.00   0.50    3.30    --  101.00  67.00 -32.10   52
 67  \w     77.00 103.00   0.50    3.30    --  101.00  57.00-120.00   52
 68  \w     80.00 190.00   0.50    3.30    --  101.00  37.00 -60.00  220
 69  \w     80.00 173.00   0.50    3.30    --  101.00  37.00-120.00  186
 70  \w     12.00 125.00   0.50    3.30    --  101.00 -57.00  30.00  226
 71  \w     80.00 115.00   0.50    3.30    --  101.00  37.00  30.00   70
 72  \w     77.00 104.00   0.50    3.30    --  101.00  57.00 -30.00   54
 73  \w     54.00  80.00   0.50    3.30    --  101.00 -82.00 120.00   52
 74  \w     84.00 109.00   0.50    3.30    --  101.00 -82.00 120.00   50
 75  \w     79.00 106.00   0.50    3.30    --  101.00  49.00-119.02   54
 76  \w    164.00 189.00   0.50    3.30    --  101.00  65.00-136.72   50
 77  \w     73.00  99.00   0.50    3.30    --  101.00  70.00  -5.89   52
 78  \w    157.00 184.00   0.50    3.30    --  101.00  55.00  29.51   54
 79  \w    165.00 190.00   0.50    3.30    --  101.00  51.00-151.82   50
 80  \w     28.00 126.00   0.50    3.30    --  101.00 -82.00-180.00  196
 81  \w     78.00 104.00   0.50    3.30    --  101.00  51.00-151.82   52
;
_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      0.0755828000
_diffrn_orient_matrix_UB_12      -0.0387688000
_diffrn_orient_matrix_UB_13      0.0213071000
_diffrn_orient_matrix_UB_21      0.0400260000
_diffrn_orient_matrix_UB_22      0.0521596000
_diffrn_orient_matrix_UB_23      0.0453907000
_diffrn_orient_matrix_UB_31      -0.0377746000
_diffrn_orient_matrix_UB_32      -0.0223180000
_diffrn_orient_matrix_UB_33      0.0693681000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            166234
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.594
_diffrn_reflns_theta_max         66.594
_diffrn_reflns_theta_min         3.972
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.121
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'orangish orange'
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_description       block
_exptl_crystal_F_000             3494
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.729
_refine_diff_density_min         -1.541
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         11769
_refine_ls_number_restraints     691
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0769
_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^)+(0.1654P)^2^+22.6668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2373
_refine_ls_wR_factor_ref         0.2405
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10674
_reflns_number_total             11769
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc05796a2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7134045.cif.'
_cod_original_cell_volume        6682.97(12)
_cod_database_code               7134045
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Fe Sn'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C02A-C2
 1.49 with sigma of 0.01
 C02E-C01N
 1.49 with sigma of 0.01
 C1AA-C01E
 1.49 with sigma of 0.01
 C8-C0AA
 1.49 with sigma of 0.01
 C02D-C02C
 1.49 with sigma of 0.01
 C02E-C01N = C0AA-C02E = C8-C0AA
 1.51 with sigma of 0.01
 C02C-C01W
 2.51 with sigma of 0.01
 C37B-C1AA
 2.8 with sigma of 0.01
 C37B-C13
 1.49 with sigma of 0.01
 C1AA-C13 = C37B-C13 = C1AA-C01E
 1.51 with sigma of 0.01
 C37A-C1AA
 2.58 with sigma of 0.01
 C37A-C13 = C37B-C13
 1.53 with sigma of 0.01
 O00J-H00J
 0.82 with sigma of 0.01
 O009-H009
 0.82 with sigma of 0.01
 H00H-O00H
 0.82 with sigma of 0.01
 H00L-O00L
 0.85 with sigma of 0.01
 O00D-H00D
 0.85 with sigma of 0.01
 H00I-O00I
 0.85 with sigma of 0.01
 C3AA-C02C = C3AA-C01W = C02D-C02C
 1.49 with sigma of 0.01
 C1-C2 \\sim N5-C2
 with sigma of 0.02
 O027-C2 \\sim O01A-C2 \\sim O012-C024 \\sim O020-C024 \\sim O00O-C00W \\sim
O00F-C00W \\sim O00G-C01D
 \\sim O00V-C01D \\sim O00N-C01O \\sim O017-C01O \\sim O00M-C01Q \\sim
O013-C01Q \\sim O00C-C01B \\sim O00Z-
 C01B \\sim O00K-C01L \\sim O00Y-C01L \\sim O014-C01Y \\sim O00X-C01Y \\sim
O00T-C01M \\sim O00U-C01M
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C01W: within 1.5A with sigma of 0.005 and sigma for terminal atoms of 0.01
within 1.5A
C0AA \\sim C8: within 1.6A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 1.6A
All non-hydrogen atoms have similar U: within -2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within -2A
4. Others
 Fixed Sof: H00I(0.5) H13C(0.5) H13D(0.5) H13A(0.5) H13B(0.5) C37B(0.5)
 H37A(0.5) H37B(0.5) H37C(0.5) C37A(0.5) H37D(0.5) H37E(0.5) H37F(0.5)
5.a Riding coordinates:
 O009(H009), O00D(H00D), O00H(H00H), O00I(H00I), O00J(H00J), O00L(H00L),
 O01V(H01K,H01L), C02D(H02C,H02D,H02E), C8(H8A,H8B,H8C), C37B(H37A,H37B,H37C),
 C37A(H37D,H37E,H37F)
5.b Secondary CH2 refined with riding coordinates:
 C01E(H01A,H01B), C01N(H01C,H01D), C01W(H01E,H01G), C02C(H02A,H02B), C02E(H02F,
 H02G), C0AA(H0AA,H0AB), C1AA(H1AA,H1AB), C13(H13C,H13D), C13(H13A,H13B),
 C3AA(H3AA,H3AB)
5.c Aromatic/amide H refined with riding coordinates:
 C018(H018), C019(H019), C01F(H01F), C01H(H01H), C01I(H01I), C01J(H01J),
 C01P(H01P), C4(H4), C5(H5), C1(H1), C01T(H01T), C01U(H01U), C01Z(H01Z),
 C026(H026), C028(H028)
5.d Fitted hexagon refined as free rotating group:
 N5(C022,C4,C5,C1,C02A)
;
_shelx_res_checksum              6829
_shelx_hkl_checksum              20540
_shelx_fab_checksum              14882
_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 4.112
_oxdiff_exptl_absorpt_empirical_full_min 0.511