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_1572312
_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         'C14 H25 Cl3 O7 Sn Ti'
_chemical_formula_sum            'C14 H25 Cl3 O7 Sn Ti'
_chemical_formula_weight         578.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-19
_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                 92.6740(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.85680(10)
_cell_length_b                   16.8341(3)
_cell_length_c                   12.5136(2)
_cell_measurement_reflns_used    11330
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      60.0690
_cell_measurement_theta_min      3.8140
_cell_volume                     2074.13(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 1.000
_diffrn_measured_fraction_theta_max 0.980
_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     90.00 115.00   0.50    0.05    --   76.11 126.00 -89.00   50
  2  \w     83.00 108.00   0.50    0.05    --   76.11 145.00  78.00   50
  3  \w     28.00  68.00   0.50    0.05    --   76.11 -38.00  60.00   80
  4  \w     54.00  79.00   0.50    0.05    --   76.11-145.00  26.00   50
  5  \w     10.00  71.00   0.50    0.05    --   76.11 -38.00-150.00  122
  6  \w    -65.00 -30.00   0.50    0.05    --  -77.99 145.00  78.00   70
  7  \w   -126.00 -79.00   0.50    0.05    --  -77.99 145.00  78.00   94
  8  \w   -103.00 -72.00   0.50    0.05    --  -77.99 126.00 -89.00   62
  9  \w   -106.00  -4.00   0.50    0.05    --  -77.99  77.00 -90.00  204
 10  \w    -38.00  -4.00   0.50    0.05    --  -77.99  57.00 -60.00   68
 11  \w    -96.00 -56.00   0.50    0.05    --  -77.99  57.00 -60.00   80
 12  \w    -23.00  26.00   0.50    0.05    --   -0.94  57.00 -60.00   98
 13  \w     43.00  73.00   0.50    0.05    --   -0.94  57.00 -60.00   60
 14  \w     -6.00  20.00   0.50    0.05    --   -0.94 -99.00 150.00   52
 15  \w      1.00  27.00   0.50    0.05    --   -0.94 -99.00  90.00   52
 16  \w     -8.00  23.00   0.50    0.05    --   -0.94 -99.00 -60.00   62
 17  \w   -151.00 -79.00   0.50    0.05    --  -77.99-126.00-166.00  144
 18  \w   -141.00-116.00   0.50    0.05    --  -77.99 -99.00 -30.00   50
 19  \w   -114.00 -89.00   0.50    0.05    --  -77.99 -99.00 -30.00   50
 20  \w   -140.00 -88.00   0.50    0.05    --  -77.99 -99.00 -60.00  104
 21  \w   -120.00 -79.00   0.50    0.05    --  -77.99-125.00 -30.00   82
 22  \w   -133.00-108.00   0.50    0.05    --  -77.99-145.00  26.00   50
 23  \w   -135.00 -79.00   0.50    0.05    --  -77.99-125.00  90.00  112
;
_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      0.1068999000
_diffrn_orient_matrix_UB_12      0.0486393000
_diffrn_orient_matrix_UB_13      -0.0061575000
_diffrn_orient_matrix_UB_21      -0.0837154000
_diffrn_orient_matrix_UB_22      0.0627244000
_diffrn_orient_matrix_UB_23      -0.0045387000
_diffrn_orient_matrix_UB_31      0.0089449000
_diffrn_orient_matrix_UB_32      0.0054192000
_diffrn_orient_matrix_UB_33      0.1068075000
_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  0.0490
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            17404
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.171
_diffrn_reflns_theta_min         3.829
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    11.341
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57750
_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    1.852
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.003
_exptl_crystal_size_mid          0.002
_exptl_crystal_size_min          0.001
_refine_diff_density_max         1.364
_refine_diff_density_min         -1.558
_refine_diff_density_rms         0.149
_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     238
_refine_ls_number_reflns         4619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0612P)^2^+2.5030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1051
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4195
_reflns_number_total             4619
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02644f2.cif
_cod_data_source_block           TOC-53
_cod_depositor_comments
'Adding full bibliography for 1572311--1572318.cif.'
_cod_database_code               1572312
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Sn Ti 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), C3(H3a,H3b), C4(H4a,H4b), C6(H6a,H6b), C9(H9a,H9b), C10(H10a,
 H10b), C11(H11a,H11b), C13(H13a,H13b)
2.b Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C7(H7a,H7b,H7c), C14(H14a,H14b,H14c)
;
_shelx_res_checksum              78731
_shelx_hkl_checksum              65065
_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 3.583
_oxdiff_exptl_absorpt_empirical_full_min 0.496