Two Titanium(IV)-Oxo-Clusters: Synthesis, Structures, Character-ization and Recycling Catalytic Activity in Oxygenation of Sulfide
Zhu, Long-Guan; Wu, Rong-Hui; Guo, Ming; Yu, Mingxin; Dalton Trans.  (2017) –; doi:10.1039/C7DT02516E

data_7044329
_publ_section_title
;
 Two Titanium(IV)-Oxo-Clusters: Synthesis, Structures, Character-ization
 and Recycling Catalytic Activity in Oxygenation of Sulfide
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02516E
_journal_year                    2017
_chemical_formula_moiety         'C76 H48 N8 O28 S4 Ti4'
_chemical_formula_sum            'C76 H48 N8 O28 S4 Ti4'
_chemical_formula_weight         1841.06
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2017-09-25 deposited with the CCDC.
2017-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.5404(3)
_cell_length_b                   13.5404(3)
_cell_length_c                   27.7844(10)
_cell_measurement_reflns_used    5878
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.3871
_cell_measurement_theta_min      3.0028??
_cell_volume                     5094.1(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics
;
 Ortep-3 for Windows (Farrugia, 1997)
;
_computing_publication_material
;
 WinGX (Farrugia, 2014)
;
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18723
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.452
_diffrn_reflns_theta_min         3.009
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.453
_exptl_absorpt_correction_T_max  0.8686
_exptl_absorpt_correction_T_min  0.8396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.320
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details
;
 Flack x determined using 1756 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.977(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.721
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         6231
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.730
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0945
_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^)+(0.0960P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2565
_refine_ls_wR_factor_ref         0.2631
_reflns_Friedel_coverage         0.895
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.848
_reflns_number_gt                4586
_reflns_number_total             6231
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02516e2.cif
_cod_data_source_block           2_sqd
_cod_original_cell_volume        5094.1(3)
_cod_database_code               7044329
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.840
_shelx_estimated_absorpt_t_max   0.869
_shelx_res_checksum              91259
_shelx_fab_checksum              96251