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_1572316
_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         'C48 H88 Cl6 O26 Sn2 Ti6'
_chemical_formula_sum            'C48 H88 Cl6 O26 Sn2 Ti6'
_chemical_formula_weight         1818.66
_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   geom
_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                110.064(2)
_cell_angle_beta                 92.418(2)
_cell_angle_gamma                112.772(3)
_cell_formula_units_Z            1
_cell_length_a                   12.3168(4)
_cell_length_b                   14.0058(4)
_cell_length_c                   15.4344(3)
_cell_measurement_reflns_used    17563
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      60.1170
_cell_measurement_theta_min      3.2530
_cell_volume                     2258.45(13)
_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_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.977
_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    110.00 148.00   0.50    0.05    --   75.32 125.00-120.00   76
  2  \w     93.00 147.00   0.50    0.05    --   75.32 106.00 -52.00  108
  3  \w     90.00 148.00   0.50    0.05    --   75.32 125.00 -30.00  116
  4  \w     56.00 145.00   0.50    0.05    --   75.32  57.00  60.00  178
  5  \w   -149.00 -56.00   0.50    0.05    --  -78.14 -57.00-120.00  186
  6  \w      9.00  35.00   0.50    0.05    --   -1.41 -99.00  30.00   52
  7  \w     -6.00  38.00   0.50    0.05    --   -1.41 -99.00  90.00   88
  8  \w   -147.00-106.00   0.50    0.05    --  -78.14 -99.00-180.00   82
  9  \w   -149.00 -79.00   0.50    0.05    --  -78.14-125.00-180.00  140
 10  \w   -137.00 -89.00   0.50    0.05    --  -78.14-106.00-151.00   96
 11  \w   -106.00 -50.00   0.50    0.05    --  -78.14 106.00 -52.00  112
 12  \w   -100.00 -41.00   0.50    0.05    --  -78.14 125.00 -60.00  118
 13  \w   -101.00 -21.00   0.50    0.05    --  -78.14 125.00  30.00  160
 14  \w   -108.00 -58.00   0.50    0.05    --  -78.14 125.00  60.00  100
 15  \w    -53.00 -28.00   0.50    0.05    --  -78.14 125.00  60.00   50
 16  \w    -68.00  -1.00   0.50    0.05    --  -78.14  38.00  60.00  134
 17  \w    -16.00  73.00   0.50    0.05    --   -1.41  57.00-150.00  178
 18  \w    -96.00 -10.00   0.50    0.05    --  -78.14  57.00-150.00  172
 19  \w    -18.00  53.00   0.50    0.05    --   -1.41  57.00 -60.00  142
 20  \w      2.00  71.00   0.50    0.05    --   75.32 -38.00  90.00  138
 21  \w     21.00  46.00   0.50    0.05    --   75.32-125.00 -60.00   50
 22  \w     71.00  97.00   0.50    0.05    --   75.32-125.00 -60.00   52
 23  \w     46.00  98.00   0.50    0.05    --   75.32-125.00 -90.00  104
 24  \w     63.00  96.00   0.50    0.05    --   75.32-106.00-151.00   66
 25  \w      2.00  41.00   0.50    0.05    --   75.32 -38.00-120.00   78
;
_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      -0.1203902000
_diffrn_orient_matrix_UB_12      -0.0466426000
_diffrn_orient_matrix_UB_13      -0.0184260000
_diffrn_orient_matrix_UB_21      -0.0003864000
_diffrn_orient_matrix_UB_22      -0.0103150000
_diffrn_orient_matrix_UB_23      -0.0895578000
_diffrn_orient_matrix_UB_31      -0.0017913000
_diffrn_orient_matrix_UB_32      -0.1019923000
_diffrn_orient_matrix_UB_33      -0.0231484000
_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  0.0727
_diffrn_reflns_av_unetI/netI     0.0659
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27705
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.164
_diffrn_reflns_theta_min         3.231
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    7.285
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.05630
_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    1.337
_exptl_crystal_description       block
_exptl_crystal_F_000             918
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.889
_refine_diff_density_min         -1.903
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         9981
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0620
_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^)+(0.1231P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1759
_refine_ls_wR_factor_ref         0.1815
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8403
_reflns_number_total             9981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02644f2.cif
_cod_data_source_block           TOC-56
_cod_depositor_comments
'Adding full bibliography for 1572311--1572318.cif.'
_cod_original_cell_volume        2258.45(12)
_cod_database_code               1572316
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Ti Sn C O'
_shelx_estimated_absorpt_t_max   0.529
_shelx_estimated_absorpt_t_min   0.529
_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
2. Rigid bond restraints
 C47, C41
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C4(H4a,H4b), C8(H8a,H8b), C12(H12a,H12b), C16(H16a,H16b), C25(H25a,H25b),
 C27(H27a,H27b), C28(H28a,H28b), C29(H29a,H29b), C32(H32a,H32b), C33(H33a,H33b),
  C35(H35a,H35b), C36(H36a,H36b), C37(H37a,H37b), C41(H41a,H41b), C44(H44a,
 H44b), C48(H48a,H48b)
3.b Idealised Me refined as rotating group:
 C39(H39a,H39b,H39c), C43(H43a,H43b,H43c), C45(H45a,H45b,H45c), C47(H47a,H47b,
 H47c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              32372
_shelx_hkl_checksum              52317
_shelx_fab_checksum              5667
_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 7.304
_oxdiff_exptl_absorpt_empirical_full_min 0.372