Large Titanium-Oxo Clusters as Precursors to Synthesize the Single Crystals of Ti-MOFs
Sun, Yayong; Lu, Dong-Fei; Sun, Yuexin; Gao, Mei-Yan; Zheng, Nan; Gu, Cheng; Wang, Fei; Zhang, Jian; ACS Materials Letters  (2020) 64–68; doi:10.1021/acsmaterialslett.0c00456

data_4518320
_publ_section_title
;
 Large Titanium-Oxo Clusters as Precursors to Synthesize the Single
 Crystals of Ti-MOFs
;
_journal_name_full               'ACS Materials Letters'
_journal_page_first              64
_journal_page_last               68
_journal_paper_doi               10.1021/acsmaterialslett.0c00456
_journal_year                    2020
_chemical_formula_moiety         'C14 H8 O7 S Ti'
_chemical_formula_sum            'C14 H8 O7 S Ti'
_chemical_formula_weight         368.16
_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_Hall           'I 4 2'
_space_group_name_H-M_alt        'I 4 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-09-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   18.7537(3)
_cell_length_b                   18.7537(3)
_cell_length_c                   21.8194(5)
_cell_measurement_reflns_used    6651
_cell_measurement_temperature    99.9(6)
_cell_measurement_theta_max      53.8480
_cell_measurement_theta_min      2.7040
_cell_volume                     7673.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     43.00  70.00   0.50    5.00    --   -1.17  57.00-120.00   54
  2  \w     -6.00  20.00   0.50    5.00    --   -1.17  57.00-120.00   52
  3  \w    -15.00  22.00   0.50   16.00    --   59.36 -19.00-150.00   74
  4  \w   -123.00 -57.00   0.50   16.00    --  -61.71 -46.00-162.00  132
  5  \w     -4.00  22.00   0.50   16.00    --   59.36 -19.00 120.00   52
  6  \w    -23.00   3.00   0.50   16.00    --  -61.71  19.00 150.00   52
  7  \w   -113.00 -23.00   0.50   16.00    --  -61.71 130.00  41.00  180
;
_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      0.0068276000
_diffrn_orient_matrix_UB_12      -0.0019227000
_diffrn_orient_matrix_UB_13      -0.0610265000
_diffrn_orient_matrix_UB_21      -0.0580814000
_diffrn_orient_matrix_UB_22      0.0410271000
_diffrn_orient_matrix_UB_23      -0.0057986000
_diffrn_orient_matrix_UB_31      0.0410225000
_diffrn_orient_matrix_UB_32      0.0584464000
_diffrn_orient_matrix_UB_33      0.0019993000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10587
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        52.043
_diffrn_reflns_theta_max         52.043
_diffrn_reflns_theta_min         2.701
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    3.249
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84032
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46c (Rigaku Oxford Diffraction, 2018)
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    1.275
_exptl_crystal_description       block
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
;
 Flack x determined using 1173 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3283
_refine_ls_number_restraints     177
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0529
_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^)+(0.1151P)^2^+13.0541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1621
_refine_ls_wR_factor_ref         0.1669
_reflns_Friedel_coverage         0.745
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                2986
_reflns_number_total             3283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tz0c00456_si_002.cif
_cod_data_source_block           FIR-126
_cod_original_cell_volume        7673.9(3)
_cod_database_code               4518320
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H O Ti S'
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.881
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     51.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C12, C11, C8, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C10, C9, C8, C7, C12, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O5, S1, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S1, O5, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C8 \\sim C9 \\sim C11 \\sim C12: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C12 \\sim C11 \\sim C10 \\sim C9 \\sim C8 \\sim C7: within 3.8A with sigma of
0.04 and sigma for terminal atoms of 0.08
O5 \\sim S1 \\sim O6: within 3.8A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O6) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(S1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C2(H2), C3(H3), C8(H8), C9(H9), C11(H11), C12(H12)
;
_shelx_res_checksum              7680
_shelx_hkl_checksum              23777
_shelx_fab_checksum              45270
_platon_squeeze_void_probe_radius 1.20
_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 2.438
_oxdiff_exptl_absorpt_empirical_full_min 0.441