Degrees of distortion: synthesis, structure and bonding in approximately icosahedral [Ru@Sn<sub>12</sub>]<sup>4</sup>.
Mondal, Sourav; Huang, Ya-Shan; Sun, Zhong-Ming; McGrady, John E.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 16986–16992; doi:10.1039/d5dt02068a

data_7719691
_publ_section_title
;
 Degrees of distortion: synthesis, structure and bonding in approximately
 icosahedral [Ru@Sn<sub>12</sub>]<sup>4</sup>.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16986
_journal_page_last               16992
_journal_paper_doi               10.1039/d5dt02068a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         '4(C18 H36 K N2 O6), Ru Sn12, 2(C2 H8 N2)'
_chemical_formula_sum            'C76 H160 K4 N12 O24 Ru Sn12'
_chemical_formula_weight         3308.164
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     dual
_audit_creation_date             2025-08-23
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-08-23 deposited with the CCDC.	2025-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                62.384(2)
_cell_angle_beta                 63.923(2)
_cell_angle_gamma                86.703(2)
_cell_formula_units_Z            1
_cell_length_a                   14.4728(3)
_cell_length_b                   15.3959(3)
_cell_length_c                   16.2884(3)
_cell_measurement_reflns_used    20256
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      75.4220
_cell_measurement_theta_min      5.4980
_cell_volume                     2839.37(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'CMOS-PHOTONII area detector'
_diffrn_measured_fraction_theta_full 0.9940
_diffrn_measured_fraction_theta_max 0.9586
_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    -32.00  46.00   0.50    0.50    --    0.00  77.00 120.00  156
  2  \w    -48.00   3.00   0.50    0.50    --    0.00 -77.00   0.00  102
  3  \w     -1.00  36.00   0.50    0.50    --    0.00 -82.00 -60.00   74
  4  \w      0.00  82.00   0.50    0.50    --    0.00  57.00  90.00  164
  5  \w     -6.00  37.00   0.50    0.50    --    0.00  82.00   0.00   86
  6  \w     12.00  45.00   0.50    0.50    --  101.30 -82.00 -60.00   66
  7  \w    128.00 189.00   0.50    0.50    --  101.30  38.00 -30.00  122
  8  \w     23.00 125.00   0.50    0.50    --  101.30 -57.00 150.00  204
  9  \w     87.00 146.00   0.50    0.50    --  101.30  82.00  30.00  118
 10  \w     67.00 189.00   0.50    0.50    --  101.30  19.00  30.00  244
 11  \w     66.00 110.00   0.50    0.50    --  101.30 -82.00  90.00   88
 12  \w     23.00 133.00   0.50    0.50    --  101.30 -82.00 150.00  220
 13  \w     86.00 123.00   0.50    0.50    --  101.30  38.00 -30.00   74
 14  \w     65.00 128.00   0.50    0.50    --  101.30  19.00 150.00  126
 15  \w     18.00  47.00   0.50    0.50    --  101.30 -82.00  90.00   58
 16  \w     99.00 125.00   0.50    0.50    --  101.30  38.00  60.00   52
 17  \w     92.00 138.00   0.50    0.50    --  101.30 -82.00   0.00   92
 18  \w     95.00 121.00   0.50    0.50    --  101.30 -82.00-150.00   52
 19  \w     60.00 138.00   0.50    0.50    --  101.30 -82.00 -60.00  156
 20  \w     82.00 185.00   0.50    0.50    --  101.30  82.00-120.00  206
 21  \w     13.00 127.00   0.50    0.50    --  101.30 -57.00 -60.00  228
;
_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      -0.0120265000
_diffrn_orient_matrix_UB_12      0.0109417000
_diffrn_orient_matrix_UB_13      -0.0935684000
_diffrn_orient_matrix_UB_21      -0.0207175000
_diffrn_orient_matrix_UB_22      0.1066255000
_diffrn_orient_matrix_UB_23      -0.0261895000
_diffrn_orient_matrix_UB_31      0.1181582000
_diffrn_orient_matrix_UB_32      0.0413491000
_diffrn_orient_matrix_UB_33      -0.0716006000
_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  0.0598
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_Laue_measured_fraction_full 0.9940
_diffrn_reflns_Laue_measured_fraction_max 0.9586
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28684
_diffrn_reflns_point_group_measured_fraction_full 0.9940
_diffrn_reflns_point_group_measured_fraction_max 0.9586
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         75.77
_diffrn_reflns_theta_min         5.54
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    23.482
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism-like
_exptl_crystal_F_000             1621.781
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.4307
_refine_diff_density_min         -1.7762
_refine_diff_density_rms         0.2337
_refine_ls_d_res_high            0.7953
_refine_ls_d_res_low             7.9830
_refine_ls_goodness_of_fit_ref   1.0425
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    120
_refine_ls_number_parameters     749
_refine_ls_number_reflns         11345
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.0395
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          -0.0012
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0838P)^2^+8.9509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1373
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              18
_reflns_limit_h_min              -15
_reflns_limit_k_max              19
_reflns_limit_k_min              -17
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                10285
_reflns_number_total             11345
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5dt02068a2.cif
_cod_data_source_block           RuSn12-1
_cod_depositor_comments          'Adding full bibliography for 7719691.cif.'
_cod_database_code               7719691
_exptl_crystal_mounting_method
;
 Crystals were removed from the crystallisation vial and immediately coated
 with PDMS (polydimethylsiloxane/Dimethicone, CAS: 9006-65-9 on a glass slide.
 A suitable single crystal was selected and mounted on a glass fiber using
 vacuum silicone grease as adhesive. The glass fiber with single crystal was
 mounted on copper pin with solid paraffin. Operator: DJ_Tokyo.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C34) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N4)
\\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O11) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Rotating group:
 N6(H6c,H6d)
3.b Secondary CH2 refined with riding coordinates:
 C24(H24a,H24b), C23(H23a,H23b), C30(H30a,H30b), C6(H6a,H6b), C36(H36a,H36b),
 C33(H33a,H33b), C34(H34a,H34b), C3(H3a,H3b), C5(H5a,H5b), C29(H29a,H29b),
 C12(H12a,H12b), C18(H18a,H18b), C9(H9a,H9b), C17(H17a,H17b), C31(H31a,H31b),
 C10(H10a,H10b), C15(H15a,H15b), C14(H14a,H14b), C4(H4a,H4b), C27(H27a,H27b),
 C28(H28a,H28b), C20(H20a,H20b), C32(H32a,H32b), C26(H26a,H26b), C2(H2a,H2b),
 C11(H11a,H11b), C7(H7a,H7b), C13(H13a,H13b), C1(H1a,H1b), C16(H16a,H16b),
 C21(H21a,H21b), C25(H25a,H25b), C35(H35a,H35b), C22(H22a,H22b), C19(H19a,H19b),
  C8(H8a,H8b), C37(H37a,H37b), C38(H38a,H38b)
3.c X=CH2 refined with riding coordinates:
 N5(H5c,H5d)
;
_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 2.394
_oxdiff_exptl_absorpt_empirical_full_min 0.421