Modulated assembly and structural diversity of heterometallic Sn–Ti oxo clusters from inorganic tin precursors
Zhao, Hui-Fang; Liu, Fang-Fang; Ding, Qing-Rong; Wang, Di; Zhang, Jian; Zhang, Lei; Nanoscale 16 (2024) 16451–16457; doi:10.1039/D4NR02644F

data_1572314
_publ_section_title
;
 Modulated assembly and structural diversity of heterometallic Sn--Ti oxo
 clusters from inorganic tin precursors
;
_journal_issue                   35
_journal_name_full               Nanoscale
_journal_page_first              16451
_journal_page_last               16457
_journal_paper_doi               10.1039/D4NR02644F
_journal_volume                  16
_journal_year                    2024
_chemical_formula_moiety         'C66 H130 Cl18 O46 Sn6 Ti10, 2(C4 H8 O2)'
_chemical_formula_sum            'C74 H146 Cl18 O50 Sn6 Ti10'
_chemical_formula_weight         3665.14
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-06
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-06-25 deposited with the CCDC.	2024-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.5800(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.60310(10)
_cell_length_b                   18.1016(2)
_cell_length_c                   29.8915(2)
_cell_measurement_reflns_used    49700
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.1010
_cell_measurement_theta_min      2.4810
_cell_volume                     8386.97(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (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 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_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     73.00  99.00   0.50    0.09    --   76.11 138.00 125.00   52
  2  \w     88.00 113.00   0.50    0.09    --   76.11 131.00 -50.00   50
  3  \w     60.00 150.00   0.50    0.09    --   76.11  57.00 -60.00  180
  4  \w     -3.00  37.00   0.50    0.05    --   -0.94 -99.00 150.00   80
  5  \w     12.00  39.00   0.50    0.05    --   -0.94 -99.00 -30.00   54
  6  \w     -8.00  17.00   0.50    0.05    --   -0.94 -99.00-120.00   50
  7  \w     46.00  71.00   0.50    0.09    --   76.11-131.00-120.00   50
  8  \w     20.00 110.00   0.50    0.09    --   76.11-125.00-180.00  180
  9  \w     29.00  66.00   0.50    0.09    --   76.11-125.00  90.00   74
 10  \w     79.00 112.00   0.50    0.09    --   76.11-125.00  90.00   66
 11  \w    -46.00  -1.00   0.50    0.09    --  -77.99  38.00-180.00   90
 12  \w    -37.00  -1.00   0.50    0.09    --  -77.99  38.00 -60.00   72
 13  \w    -95.00  -8.00   0.50    0.09    --  -77.99  57.00 -30.00  174
 14  \w    -85.00  -6.00   0.50    0.09    --  -77.99  57.00  30.00  158
 15  \w   -105.00 -73.00   0.50    0.09    --  -77.99 138.00 125.00   64
 16  \w   -116.00 -69.00   0.50    0.09    --  -77.99 131.00 -50.00   94
 17  \w    -73.00  17.00   0.50    0.05    --   -0.94 -57.00-150.00  180
 18  \w   -138.00-113.00   0.50    0.09    --  -77.99-131.00-120.00   50
 19  \w   -144.00 -74.00   0.50    0.09    --  -77.99-138.00  63.00  140
 20  \w   -151.00 -86.00   0.50    0.09    --  -77.99-125.00  90.00  130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0783624000
_diffrn_orient_matrix_UB_12      0.0058149000
_diffrn_orient_matrix_UB_13      -0.0233008000
_diffrn_orient_matrix_UB_21      -0.0051094000
_diffrn_orient_matrix_UB_22      -0.0736687000
_diffrn_orient_matrix_UB_23      -0.0029067000
_diffrn_orient_matrix_UB_31      -0.0362098000
_diffrn_orient_matrix_UB_32      -0.0019787000
_diffrn_orient_matrix_UB_33      0.0384985000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ga K\a'
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            75852
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.143
_diffrn_reflns_theta_min         2.485
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    9.473
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       block
_exptl_crystal_F_000             3632
_exptl_crystal_size_max          0.001
_exptl_crystal_size_mid          0.001
_exptl_crystal_size_min          0.001
_refine_diff_density_max         3.802
_refine_diff_density_min         -1.919
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     738
_refine_ls_number_reflns         18686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0584
_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^)+(0.0941P)^2^+39.1048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.1766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15921
_reflns_number_total             18686
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02644f2.cif
_cod_data_source_block           TOC-52
_cod_depositor_comments
'Adding full bibliography for 1572311--1572318.cif.'
_cod_database_code               1572314
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Ti Sn Cl C O'
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.991
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H11 of O11, H20 of O20, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H9 of O9, All O(H,H) groups
2. Others
 Fixed Sof: C9(0.5) H9a(0.5) H9b(0.5) H9c(0.5) H11a(0.5) H11b(0.5) H11c(0.5)
 H11d(0.5) H12c(0.5) H12d(0.5) H12a(0.5) H12b(0.5) C19(0.5) H19c(0.5) H19d(0.5)
 H19e(0.5) C33(0.5) H33a(0.5) H33b(0.5) H33c(0.5) C37(0.5) H37a(0.5) H37b(0.5)
 H37c(0.5)
3.a Riding coordinates:
 O20(H20)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C6(H6a,H6b), C7(H7a,H7b), C8(H8a,H8b), C10(H10a,H10b), C11(H11a,
 H11b), C11(H11c,H11d), C12(H12c,H12d), C12(H12a,H12b), C13(H13a,H13b),
 C18(H18a,H18b), C21(H21a,H21b), C22(H22a,H22b), C23(H23a,H23b), C24(H24a,H24b),
  C26(H26a,H26b), C28(H28a,H28b), C30(H30a,H30b), C32(H32a,H32b), C34(H34a,
 H34b), C36(H36a,H36b), C38(H38a,H38b), C39(H39a,H39b), C15(H15a,H15b),
 C17(H17a,H17b), C31(H31a,H31b), C35(H35a,H35b)
3.c Aromatic/amide H refined with riding coordinates:
 O11(H11)
3.d Tetrahedral OH refined with riding coordinates:
 O9(H9)
3.e X=CH2 refined with riding coordinates:
 O19(H19a,H19b)
3.f Idealised Me refined as rotating group:
 C2(H2a,H2b,H2c), C3(H3a,H3b,H3c), C9(H9a,H9b,H9c), C19(H19c,H19d,H19e),
 C27(H27a,H27b,H27c), C29(H29a,H29b,H29c), C33(H33a,H33b,H33c), C37(H37a,H37b,
 H37c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              51121
_shelx_hkl_checksum              61302
_shelx_fab_checksum              83952
_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 2.428
_oxdiff_exptl_absorpt_empirical_full_min 0.567