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_1572317
_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         'C96 H178 Cl14 O54 Sn6 Ti14'
_chemical_formula_sum            'C96 H178 Cl14 O54 Sn6 Ti14'
_chemical_formula_weight         4075.41
_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             2023-03-27
_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                 106.9090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.2738(2)
_cell_length_b                   23.1167(2)
_cell_length_c                   23.1453(2)
_cell_measurement_reflns_used    38257
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      60.1440
_cell_measurement_theta_min      3.0890
_cell_volume                     7818.84(15)
_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(13)
_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 0.980
_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     59.00  96.00   0.50    0.19    --   76.57 154.00 -61.00   74
  2  \w     93.00 118.00   0.50    0.19    --   76.57 120.00 140.00   50
  3  \w     99.00 127.00   0.50    0.19    --   76.57  77.00 120.00   56
  4  \w     58.00  83.00   0.50    0.19    --   76.57  77.00 120.00   50
  5  \w      3.00  66.00   0.50    0.19    --   76.57 -38.00  30.00  126
  6  \w     40.00  65.00   0.50    0.19    --   76.57-120.00  57.00   50
  7  \w     37.00  63.00   0.50    0.19    --   76.57-125.00 -30.00   52
  8  \w     80.00 110.00   0.50    0.19    --   76.57-125.00 -30.00   60
  9  \w   -131.00 -63.00   0.50    0.19    --  -78.14 154.00 -61.00  136
 10  \w    -97.00 -20.00   0.50    0.19    --  -78.14 120.00 140.00  154
 11  \w    -95.00 -53.00   0.50    0.19    --  -78.14  57.00 150.00   84
 12  \w    -34.00  -4.00   0.50    0.19    --  -78.14  57.00 150.00   60
 13  \w      2.00  73.00   0.50    0.05    --   -0.78  57.00   0.00  142
 14  \w    -71.00  11.00   0.50    0.05    --   -0.78 -57.00-120.00  164
 15  \w   -130.00-105.00   0.50    0.19    --  -78.14-154.00-101.00   50
 16  \w   -108.00 -82.00   0.50    0.19    --  -78.14-125.00 -60.00   52
 17  \w   -152.00 -83.00   0.50    0.19    --  -78.14-125.00   0.00  138
 18  \w   -141.00-116.00   0.50    0.19    --  -78.14-120.00  57.00   50
 19  \w   -128.00 -88.00   0.50    0.19    --  -78.14 -99.00 120.00   80
 20  \w   -146.00-115.00   0.50    0.19    --  -78.14-125.00 -60.00   62
 21  \w   -140.00 -88.00   0.50    0.19    --  -78.14 -99.00-120.00  104
 22  \w   -148.00-101.00   0.50    0.19    --  -78.14 -99.00-150.00   94
;
_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      -0.0858621000
_diffrn_orient_matrix_UB_12      -0.0085387000
_diffrn_orient_matrix_UB_13      -0.0348983000
_diffrn_orient_matrix_UB_21      -0.0092566000
_diffrn_orient_matrix_UB_22      0.0569101000
_diffrn_orient_matrix_UB_23      -0.0109491000
_diffrn_orient_matrix_UB_31      0.0307942000
_diffrn_orient_matrix_UB_32      -0.0066510000
_diffrn_orient_matrix_UB_33      -0.0481408000
_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  0.0651
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            67350
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.199
_diffrn_reflns_theta_min         2.402
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    10.899
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45149
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_description       block
_exptl_crystal_F_000             4064
_exptl_crystal_size_max          0.001
_exptl_crystal_size_mid          0.001
_exptl_crystal_size_min          0.001
_refine_diff_density_max         2.873
_refine_diff_density_min         -3.487
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         17394
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0638
_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^)+(0.1005P)^2^+47.6922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1778
_refine_ls_wR_factor_ref         0.1872
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14378
_reflns_number_total             17394
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02644f2.cif
_cod_data_source_block           TOC-57
_cod_depositor_comments
'Adding full bibliography for 1572311--1572318.cif.'
_cod_database_code               1572317
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Ti Sn C O'
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.989
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C45-C49
 1.52 with sigma of 0.02
 C45-C49A
 1.52 with sigma of 0.02
 C49A-C45 \\sim C49-C45
 with sigma of 0.02
3. Rigid bond restraints
 C35, C45
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O8, C48
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 Sn2, Cl5, Cl3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C45) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O8) \\sim Ueq, Uanis(C48) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Cl7) \\sim Ueq, Uanis(Sn3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Sn2) \\sim Ueq, Uanis(Cl3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Cl5) \\sim Ueq, Uanis(Sn2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 O8, C48
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Others
 Fixed Sof: H45a(0.5) H45b(0.5) H45c(0.5) H45d(0.5) C49(0.5) H49a(0.5)
 H49b(0.5) H49c(0.5) C49A(0.5) H49d(0.5) H49e(0.5) H49f(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C8(H8a,H8b), C10(H10a,H10b), C12(H12a,H12b), C14(H14a,H14b),
 C18(H18a,H18b), C20(H20a,H20b), C22(H22a,H22b), C24(H24a,H24b), C28(H28a,H28b),
  C30(H30a,H30b), C34(H34a,H34b), C36(H36a,H36b), C38(H38a,H38b), C40(H40a,
 H40b), C44(H44a,H44b), C46(H46a,H46b), C48(H48a,H48b), C3(H3a,H3b), C25(H25a,
 H25b), C13(H13a,H13b), C15(H15a,H15b), C31(H31a,H31b), C2(H2a,H2b), C33(H33a,
 H33b), C17(H17a,H17b), C9(H9a,H9b), C19(H19a,H19b), C39(H39a,H39b), C41(H41a,
 H41b), C21(H21a,H21b), C45(H45a,H45b), C45(H45c,H45d)
7.b Aromatic/amide H refined with riding coordinates:
 O15(H15)
7.c Idealised Me refined as rotating group:
 C32(H32a,H32b,H32c), C42(H42a,H42b,H42c), C27(H27a,H27b,H27c), C5(H5a,H5b,
 H5c), C43(H43a,H43b,H43c), C11(H11a,H11b,H11c), C23(H23a,H23b,H23c), C49(H49a,
 H49b,H49c), C49A(H49d,H49e,H49f)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              30773
_shelx_hkl_checksum              89323
_shelx_fab_checksum              21851
_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 1.695
_oxdiff_exptl_absorpt_empirical_full_min 0.603