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_1572313
_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         'C15 H27 Cl3 O7 Sn Ti'
_chemical_formula_sum            'C15 H27 Cl3 O7 Sn Ti'
_chemical_formula_weight         592.30
_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             2023-03-18
_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                73.634(2)
_cell_angle_beta                 89.391(2)
_cell_angle_gamma                67.044(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0964(2)
_cell_length_b                   9.3132(2)
_cell_length_c                   14.5943(3)
_cell_measurement_reflns_used    11893
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      59.8840
_cell_measurement_theta_min      2.7560
_cell_volume                     1085.42(5)
_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      100.00(10)
_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 0.979
_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      6.00  36.00   0.50    0.05    --   76.11 -77.00 120.00   60
  2  \w     13.00 103.00   0.50    0.05    --   76.11 -77.00  60.00  180
  3  \w     53.00 148.00   0.50    0.05    --   76.11  57.00-180.00  190
  4  \w     94.00 119.00   0.50    0.05    --   76.11 112.00-151.00   50
  5  \w     97.00 136.00   0.50    0.05    --   76.11 125.00 -60.00   78
  6  \w      9.00  62.00   0.50    0.05    --   76.11 -38.00-180.00  106
  7  \w     72.00 102.00   0.50    0.05    --   76.11 -77.00 120.00   60
  8  \w     40.00  81.00   0.50    0.05    --   76.11-112.00 115.00   82
  9  \w     20.00  54.00   0.50    0.05    --   76.11-125.00  60.00   68
 10  \w     60.00  86.00   0.50    0.05    --   76.11-125.00  60.00   52
 11  \w     12.00  37.00   0.50    0.05    --   76.11-112.00 115.00   50
 12  \w     32.00 112.00   0.50    0.05    --   76.11-125.00  30.00  160
 13  \w     75.00 112.00   0.50    0.05    --   76.11-125.00 -90.00   74
 14  \w     39.00  71.00   0.50    0.05    --   76.11-125.00 -90.00   64
 15  \w    -76.00 -21.00   0.50    0.05    --  -77.99 125.00-120.00  110
 16  \w   -104.00 -58.00   0.50    0.05    --  -77.99 112.00-151.00   92
 17  \w   -150.00 -63.00   0.50    0.05    --  -77.99 -57.00   0.00  174
 18  \w   -152.00 -50.00   0.50    0.05    --  -77.99 -77.00 -30.00  204
 19  \w    -72.00 -40.00   0.50    0.05    --   -0.94 -57.00-180.00   64
 20  \w    -28.00  16.00   0.50    0.05    --   -0.94 -57.00-180.00   88
 21  \w     -6.00  36.00   0.50    0.05    --   -0.94 -99.00-120.00   84
 22  \w     -6.00  29.00   0.50    0.05    --   -0.94 -99.00 -90.00   70
 23  \w      4.00  29.00   0.50    0.05    --   -0.94 -99.00 -60.00   50
 24  \w      9.00  36.00   0.50    0.05    --   -0.94 -99.00   0.00   54
 25  \w     -8.00  39.00   0.50    0.05    --   -0.94 -99.00  90.00   94
 26  \w   -152.00-120.00   0.50    0.05    --  -77.99-125.00 150.00   64
 27  \w   -128.00 -87.00   0.50    0.05    --  -77.99-112.00 115.00   82
 28  \w   -128.00 -94.00   0.50    0.05    --  -77.99 -99.00 -30.00   68
 29  \w   -138.00 -89.00   0.50    0.05    --  -77.99 -99.00 -90.00   98
;
_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      0.0196446000
_diffrn_orient_matrix_UB_12      0.0043841000
_diffrn_orient_matrix_UB_13      0.0898371000
_diffrn_orient_matrix_UB_21      -0.0865737000
_diffrn_orient_matrix_UB_22      0.1618739000
_diffrn_orient_matrix_UB_23      -0.0289353000
_diffrn_orient_matrix_UB_31      -0.1341993000
_diffrn_orient_matrix_UB_32      -0.0245653000
_diffrn_orient_matrix_UB_33      0.0188510000
_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  0.0310
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13333
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         59.966
_diffrn_reflns_theta_min         2.761
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    10.846
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24366
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         4791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0241
_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^)+(0.0339P)^2^+0.9229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0616
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4692
_reflns_number_total             4791
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02644f2.cif
_cod_data_source_block           TOC-54
_cod_depositor_comments
'Adding full bibliography for 1572311--1572318.cif.'
_cod_original_cell_volume        1085.42(4)
_cod_database_code               1572313
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Ti Sn C O'
_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.a Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C5(H5a,H5b), C6(H6a,H6b), C8(H8a,H8b), C9(H9a,H9b), C10(H10a,
 H10b), C11(H11a,H11b), C13(H13a,H13b), C14(H14a,H14b)
2.b Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C4(H4a,H4b,H4c), C15(H15a,H15b,H15c)
;
_shelx_res_checksum              66272
_shelx_hkl_checksum              4542
_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 2.263
_oxdiff_exptl_absorpt_empirical_full_min 0.507