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_1572311
_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         '2(C32 H63 Cl9 O23 Sn3 Ti5), 2(C4 H8 O2)'
_chemical_formula_sum            'C72 H142 Cl18 O50 Sn6 Ti10'
_chemical_formula_weight         3637.09
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-08
_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                111.5130(10)
_cell_angle_beta                 96.0020(10)
_cell_angle_gamma                96.3570(10)
_cell_formula_units_Z            2
_cell_length_a                   12.9762(2)
_cell_length_b                   22.6922(3)
_cell_length_c                   26.2336(3)
_cell_measurement_reflns_used    64995
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      60.3770
_cell_measurement_theta_min      1.9640
_cell_volume                     7053.79(18)
_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      100.0(3)
_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     49.00 112.00   0.50    0.11    --   76.57  77.00 -60.00  126
  2  \w     84.00 110.00   0.50    0.11    --   76.57 153.00 121.00   52
  3  \w     92.00 137.00   0.50    0.11    --   76.57 121.00 -37.00   90
  4  \w     79.00 150.00   0.50    0.11    --   76.57 125.00-180.00  142
  5  \w     54.00 151.00   0.50    0.11    --   76.57  57.00 -60.00  194
  6  \w      1.00  62.00   0.50    0.11    --   76.57 -38.00 -30.00  122
  7  \w     52.00 107.00   0.50    0.11    --   76.57-121.00-120.00  110
  8  \w     78.00 108.00   0.50    0.11    --   76.57-153.00  80.00   60
  9  \w     20.00 110.00   0.50    0.11    --   76.57-125.00 120.00  180
 10  \w    -17.00  75.00   0.50    0.05    --   -0.78  38.00  60.00  184
 11  \w    -96.00 -65.00   0.50    0.11    --  -78.14  57.00 -30.00   62
 12  \w    -71.00  -1.00   0.50    0.11    --  -78.14  38.00 -60.00  140
 13  \w    -39.00 -13.00   0.50    0.11    --  -78.14  57.00 -30.00   52
 14  \w    -79.00  -9.00   0.50    0.11    --  -78.14  57.00 150.00  140
 15  \w    -92.00 -21.00   0.50    0.11    --  -78.14  77.00 150.00  142
 16  \w   -131.00 -88.00   0.50    0.11    --  -78.14 153.00 121.00   86
 17  \w    -73.00   6.00   0.50    0.05    --   -0.78 -57.00 -90.00  158
 18  \w   -108.00 -18.00   0.50    0.11    --  -78.14 121.00 -37.00  180
 19  \w    -18.00  21.00   0.50    0.05    --   -0.78 -57.00  90.00   78
 20  \w    -70.00 -44.00   0.50    0.05    --   -0.78 -57.00  90.00   52
 21  \w   -151.00-126.00   0.50    0.11    --  -78.14 -77.00 -30.00   50
 22  \w   -140.00-115.00   0.50    0.11    --  -78.14 -77.00 -60.00   50
 23  \w   -152.00 -55.00   0.50    0.11    --  -78.14 -57.00-180.00  194
 24  \w    -96.00 -49.00   0.50    0.11    --  -78.14 -77.00 -60.00   94
 25  \w   -131.00-104.00   0.50    0.11    --  -78.14 -57.00 120.00   54
 26  \w   -151.00 -88.00   0.50    0.11    --  -78.14 -99.00  90.00  126
 27  \w   -106.00 -74.00   0.50    0.11    --  -78.14-153.00  80.00   64
 28  \w   -141.00-116.00   0.50    0.11    --  -78.14-121.00-120.00   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      -0.0421341000
_diffrn_orient_matrix_UB_12      -0.0504263000
_diffrn_orient_matrix_UB_13      0.0101213000
_diffrn_orient_matrix_UB_21      -0.0348175000
_diffrn_orient_matrix_UB_22      -0.0318972000
_diffrn_orient_matrix_UB_23      -0.0542909000
_diffrn_orient_matrix_UB_31      0.0898235000
_diffrn_orient_matrix_UB_32      -0.0238958000
_diffrn_orient_matrix_UB_33      -0.0060859000
_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  0.0480
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            101285
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.427
_diffrn_reflns_theta_min         1.843
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    11.260
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26942
_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    1.712
_exptl_crystal_description       block
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.001
_exptl_crystal_size_mid          0.001
_exptl_crystal_size_min          0.001
_refine_diff_density_max         3.483
_refine_diff_density_min         -2.271
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1417
_refine_ls_number_reflns         31498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+21.4931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26925
_reflns_number_total             31498
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02644f2.cif
_cod_data_source_block           TOC-51
_cod_depositor_comments
'Adding full bibliography for 1572311--1572318.cif.'
_cod_original_cell_volume        7053.79(17)
_cod_database_code               1572311
_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, H41 of O41, H50 of O50, H43 of O43, H40 of O40
 At 1.5 times of:
  All C(H,H,H) groups, H23 of O23, H47 of O47, All O(H,H) groups
2.a Riding coordinates:
 O47(H47), O23(H23)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C10(H10A,H10B), C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B),
 C18(H18A,H18B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B), C30(H30A,H30B),
  C36(H36A,H36B), C40(H40A,H40B), C48(H48A,H48B), C52(H52A,H52B), C54(H54A,
 H54B), C58(H58A,H58B), C60(H60A,H60B), C62(H62A,H62B), C68(H68A,H68B),
 C70(H70A,H70B), C3(H3A,H3B), C9(H9A,H9B), C12(H12A,H12B), C15(H15A,H15B),
 C21(H21A,H21B), C25(H25A,H25B), C27(H27C,H27D), C32(H32A,H32B), C34(H34A,H34B),
  C37(H37A,H37B), C41(H41A,H41B), C42(H42A,H42B), C44(H44A,H44B), C45(H45A,
 H45B), C46(H46A,H46B), C47(H47A,H47B), C49(H49A,H49B), C50(H50A,H50B),
 C64(H64A,H64B), C72(H72A,H72B), C33(H33A,H33B), C35(H35A,H35B), C69(H69A,H69B),
  C71(H71A,H71B), C29(H29A,H29B), C61(H61A,H61B), C63(H63A,H63B), C65(H65A,H65B)
2.c Aromatic/amide H refined with riding coordinates:
 O40(H40), O43(H43), O41(H41), O50(H50)
2.d X=CH2 refined with riding coordinates:
 O27(H27A,H27B), O39(H39A,H39B)
2.e Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C19(H19A,H19B,H19C), C51(H51A,H51B,H51C), C53(H53A,H53B,
 H53C), C55(H55A,H55B,H55C), C66(H66A,H66B,H66C), C7(H7A,H7B,H7C), C17(H17A,
 H17B,H17C), C31(H31A,H31B,H31C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C),
 C67(H67A,H67B,H67C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              67362
_shelx_hkl_checksum              75239
_shelx_fab_checksum              41308
_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 2.243
_oxdiff_exptl_absorpt_empirical_full_min 0.601