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_1572318
_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         'C144 H264 Cl12 O82 Sn8 Ti20'
_chemical_formula_sum            'C144 H264 Cl12 O82 Sn8 Ti20'
_chemical_formula_weight         5640.46
_space_group_crystal_system      cubic
_space_group_IT_number           220
_space_group_name_Hall           'I -4bd 2c 3'
_space_group_name_H-M_alt        'I -4 3 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-19
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   41.7993(2)
_cell_length_b                   41.7993(2)
_cell_length_c                   41.7993(2)
_cell_measurement_reflns_used    18777
_cell_measurement_temperature    100.00(17)
_cell_measurement_theta_max      60.0840
_cell_measurement_theta_min      2.2420
_cell_volume                     73031.0(6)
_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(17)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.978
_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   -151.00 -72.34   0.38    5.96    --  -78.14-144.00 -60.00  207
  2  \w      5.00  32.36   0.38    1.49    --   -1.41 -99.00-180.00   72
  3  \w   -116.00 -92.06   0.38    5.96    --  -78.14-103.00 148.00   63
;
_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      0.0069982000
_diffrn_orient_matrix_UB_12      0.0167875000
_diffrn_orient_matrix_UB_13      -0.0263648000
_diffrn_orient_matrix_UB_21      0.0133828000
_diffrn_orient_matrix_UB_22      0.0228233000
_diffrn_orient_matrix_UB_23      0.0180607000
_diffrn_orient_matrix_UB_31      0.0282297000
_diffrn_orient_matrix_UB_32      -0.0150017000
_diffrn_orient_matrix_UB_33      -0.0020272000
_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  0.0541
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            37310
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.223
_diffrn_reflns_theta_min         2.251
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    9.164
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13730
_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 reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       block
_exptl_crystal_F_000             33936
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.672
_refine_diff_density_min         -1.198
_refine_diff_density_rms         0.225
_refine_ls_abs_structure_details
;
 Flack x determined using 3924 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.032(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         12754
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_gt           0.0936
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1105P)^2^+3797.6565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2343
_refine_ls_wR_factor_ref         0.2620
_reflns_Friedel_coverage         0.808
_reflns_Friedel_fraction_full    0.922
_reflns_Friedel_fraction_max     0.859
_reflns_number_gt                10128
_reflns_number_total             12754
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02644f2.cif
_cod_data_source_block           TOC-58
_cod_depositor_comments
'Adding full bibliography for 1572311--1572318.cif.'
_cod_original_cell_volume        73031.0(10)
_cod_database_code               1572318
_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. Restrained distances
 C141-C126
 1.52 with sigma of 0.02
 C144-C118
 1.52 with sigma of 0.02
 C106-C127
 1.52 with sigma of 0.02
 C126-C127
 1.52 with sigma of 0.02
 C115-C98
 1.52 with sigma of 0.02
 C133-C130
 1.52 with sigma of 0.02
 C82-C133 = C139-C142
 1.52 with sigma of 0.02
 C142-C139 = C133-C125
 1.52 with sigma of 0.002
 C139-C133 = C133-C130
 1.52 with sigma of 0.002
 C82-C133
 1.52 with sigma of 0.002
 C144-C118 = C123-C121
 1.52 with sigma of 0.002
 C118-C123 = C123-C110
 1.52 with sigma of 0.002
 C141-C126 = C127-C106
 1.52 with sigma of 0.002
 C126-C127 = C127-C113
 1.52 with sigma of 0.002
 C127-C131
 1.52 with sigma of 0.002
 C129-C98 = C98-C115
 1.52 with sigma of 0.002
 C111-C98 = C98-C137
 1.52 with sigma of 0.002
 C134-C119 = C90-C94
 1.52 with sigma of 0.002
 C86-C90 = C90-C119
 1.52 with sigma of 0.002
 C90-C74
 1.52 with sigma of 0.002
 C138-C114 = C117-C109
 1.52 with sigma of 0.002
 C114-C117 = C117-C102
 1.52 with sigma of 0.002
 C117-C78
 1.52 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C126) \\sim Ueq, Uanis(C141) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C144) \\sim Ueq, Uanis(C118) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C74(H74a,H74b), C78(H78a,H78b), C82(H82a,H82b), C86(H86a,H86b), C94(H94a,
 H94b), C102(H10a,H10b), C106(H10c,H10d), C109(H10e,H10f), C110(H11a,H11b),
 C111(H11c,H11d), C113(H11e,H11f), C114(H11g,H11h), C115(H11i,H11j), C118(H11k,
 H11l), C119(H11m,H11n), C121(H12a,H12b), C122(H12c,H12d), C125(H12e,H12f),
 C126(H12g,H12h), C129(H12i,H12j), C130(H13a,H13b), C131(H13c,H13d), C137(H13k,
 H13l), C139(H13p,H13q)
4.b Idealised Me refined as rotating group:
 C134(H13e,H13f,H13g), C135(H13h,H13i,H13j), C138(H13m,H13n,H13o), C141(H14a,
 H14b,H14c), C142(H14d,H14e,H14f), C144(H14g,H14h,H14i)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              24549
_shelx_hkl_checksum              10099
_shelx_fab_checksum              70580
_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 4.919
_oxdiff_exptl_absorpt_empirical_full_min 0.423