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_1572315
_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         'C24 H48 Cl6 O13 Sn2 Ti2'
_chemical_formula_sum            'C24 H48 Cl6 O13 Sn2 Ti2'
_chemical_formula_weight         1090.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-07
_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                 95.5520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.98520(10)
_cell_length_b                   18.3443(2)
_cell_length_c                   25.5115(2)
_cell_measurement_reflns_used    13215
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      59.9720
_cell_measurement_theta_min      3.0250
_cell_volume                     4185.26(7)
_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 0.999
_diffrn_measured_fraction_theta_max 0.976
_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     68.00 102.00   0.50    0.08    --   75.49-128.00 134.00   68
  2  \w     79.00 104.00   0.50    0.08    --   75.49-125.00  60.00   50
  3  \w     52.00  77.00   0.50    0.08    --   75.49-142.00 -35.00   50
  4  \w      1.00  68.00   0.50    0.08    --   75.49 -38.00 150.00  134
  5  \w     91.00 117.00   0.50    0.08    --   75.49 142.00  20.00   52
  6  \w     -6.00  24.00   0.50    0.05    --   -1.25 -99.00  30.00   60
  7  \w     -8.00  26.00   0.50    0.05    --   -1.25 -99.00-150.00   68
  8  \w     -5.00  20.00   0.50    0.05    --   -1.25 -99.00 -30.00   50
  9  \w   -114.00 -70.00   0.50    0.08    --  -77.99 128.00-150.00   88
 10  \w    -70.00 -17.00   0.50    0.08    --  -77.99  38.00 -30.00  106
 11  \w   -106.00  -4.00   0.50    0.08    --  -77.99  77.00  30.00  204
 12  \w    -92.00  -9.00   0.50    0.08    --  -77.99  57.00  60.00  166
 13  \w     41.00  67.00   0.50    0.05    --   -1.25  57.00-120.00   52
 14  \w    -22.00  38.00   0.50    0.05    --   -1.25  57.00-120.00  120
 15  \w   -139.00 -91.00   0.50    0.08    --  -77.99 -99.00-120.00   96
 16  \w   -120.00 -67.00   0.50    0.08    --  -77.99-142.00 -35.00  106
 17  \w   -146.00-121.00   0.50    0.08    --  -77.99-142.00 -35.00   50
 18  \w   -104.00 -79.00   0.50    0.08    --  -77.99-125.00  90.00   50
 19  \w   -147.00-121.00   0.50    0.08    --  -77.99-125.00  90.00   52
 20  \w   -139.00-114.00   0.50    0.08    --  -77.99-128.00 134.00   50
;
_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      -0.0074566000
_diffrn_orient_matrix_UB_12      -0.0722086000
_diffrn_orient_matrix_UB_13      -0.0074573000
_diffrn_orient_matrix_UB_21      0.0030311000
_diffrn_orient_matrix_UB_22      0.0099364000
_diffrn_orient_matrix_UB_23      -0.0518958000
_diffrn_orient_matrix_UB_31      0.1495431000
_diffrn_orient_matrix_UB_32      -0.0038349000
_diffrn_orient_matrix_UB_33      0.0057694000
_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  0.0320
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            15569
_diffrn_reflns_point_group_measured_fraction_full 0.598
_diffrn_reflns_point_group_measured_fraction_max 0.578
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.082
_diffrn_reflns_theta_min         3.026
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    11.200
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39786
_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            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_description       block
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.174
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.238(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         5471
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0507P)^2^+27.8812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.182
_reflns_Friedel_fraction_full    0.195
_reflns_Friedel_fraction_max     0.178
_reflns_number_gt                5386
_reflns_number_total             5471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02644f2.cif
_cod_data_source_block           TOC-55
_cod_depositor_comments
'Adding full bibliography for 1572311--1572318.cif.'
_cod_database_code               1572315
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.400
_shelx_estimated_absorpt_t_min   0.134
_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, All O(H,H) groups
2.a Rotating group:
 O2(H2a,H2b), O13(H13a,H13b)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C3(H3a,H3b), C4(H4a,H4b), C6(H6a,H6b), C7(H7a,H7b), C8(H8a,H8b),
 C10(H10a,H10b), C11(H11a,H11b), C13(H13c,H13d), C15(H15a,H15b), C16(H16a,H16b),
  C17(H17a,H17b), C18(H18a,H18b), C19(H19a,H19b), C22(H22a,H22b), C24(H24a,H24b)
2.c Idealised Me refined as rotating group:
 C2(H2c,H2d,H2e), C9(H9a,H9b,H9c), C12(H12a,H12b,H12c), C23(H23a,H23b,H23c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              61486
_shelx_hkl_checksum              41580
_shelx_fab_checksum              52537
_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 2.027
_oxdiff_exptl_absorpt_empirical_full_min 0.589