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_4518321
_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         'C19 H28 O9 S2 Ti'
_chemical_formula_sum            'C19 H28 O9 S2 Ti'
_chemical_formula_weight         512.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-08-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.551(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3196(3)
_cell_length_b                   22.1225(5)
_cell_length_c                   11.2683(3)
_cell_measurement_reflns_used    11259
_cell_measurement_temperature    110.88(11)
_cell_measurement_theta_max      60.5240
_cell_measurement_theta_min      3.4950
_cell_volume                     2358.22(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.88(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.972
_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      8.00  43.00   0.50    0.50    --   72.03 -57.00 -30.00   70
  2  \w      3.00  54.00   0.50    0.50    --   72.03 -57.00   0.00  102
  3  \w      5.00  42.00   0.50    0.50    --   72.03 -38.00   0.00   74
  4  \w     -2.00  24.00   0.50    0.50    --   72.03 -38.00 -30.00   52
  5  \w      1.00  43.00   0.50    0.50    --   72.03 -38.00-180.00   84
  6  \w     62.00 112.00   0.50    0.50    --   72.03  38.00 -67.00  100
  7  \w     -3.00  26.00   0.50    0.50    --   72.03 -19.00  60.00   58
  8  \w     11.00  37.00   0.50    0.50    --   72.03 -38.00 137.00   52
  9  \w    -15.00  72.00   0.50    0.10    --   -1.72  38.00   0.00  174
 10  \w    -15.00  37.00   0.50    0.10    --   -1.72  38.00 -67.00  104
 11  \w     62.00  99.00   0.50    0.50    --   72.03-125.00  30.00   74
 12  \w     21.00  49.00   0.50    0.50    --   72.03-125.00  30.00   56
 13  \w    -40.00 -13.00   0.50    0.10    --   -1.72 -38.00 137.00   54
 14  \w   -149.00 -61.00   0.50    0.50    --  -75.46 -38.00 137.00  176
 15  \w    -65.00  -2.00   0.50    0.50    --  -75.46  57.00  90.00  126
 16  \w    -27.00  -2.00   0.50    0.50    --  -75.46  38.00 120.00   50
 17  \w    -42.00  -9.00   0.50    0.50    --  -75.46  38.00  90.00   66
 18  \w    -31.00  -2.00   0.50    0.50    --  -75.46  38.00 -67.00   58
 19  \w    -26.00   0.00   0.50    0.50    --  -75.46  19.00 -90.00   52
 20  \w    -42.00 -14.00   0.50    0.50    --  -75.46  38.00-120.00   56
;
_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      -0.1292984000
_diffrn_orient_matrix_UB_12      0.0240129000
_diffrn_orient_matrix_UB_13      -0.0576261000
_diffrn_orient_matrix_UB_21      0.0041537000
_diffrn_orient_matrix_UB_22      0.0166216000
_diffrn_orient_matrix_UB_23      0.1157261000
_diffrn_orient_matrix_UB_31      0.0574226000
_diffrn_orient_matrix_UB_32      0.0530182000
_diffrn_orient_matrix_UB_33      -0.0103482000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19296
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.577
_diffrn_reflns_theta_min         3.474
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    3.309
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
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    1.443
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5273
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0347P)^2^+1.5469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0762
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4736
_reflns_number_total             5273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tz0c00456_si_002.cif
_cod_data_source_block           FIR-127
_cod_database_code               4518321
_shelx_shelxl_version_number     2017/1
_diffrn_oxdiff_digest_frames
;
0120a555cfef0b7e46c0bb349fc20df3c800031ae8d
;
_diffrn_oxdiff_digest_hkl
;
01c0e0c25770f6f12c002c614db61e779ab83e
;
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O9-H9
 0.85 with sigma of 0.01
 C17-H9
 1.928152 with sigma of 0.02
 Ti1-H9
 2.643656 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C11(H11), C17(H17), C14(H14)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9A), C2(H2), C7(H7), C4(H4), C3(H3), C8(H8)
3.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C16(H16A,H16B,H16C), C12(H12A,H12B,
 H12C), C15(H15A,H15B,H15C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              77070
_shelx_hkl_checksum              99372
_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 2.160
_oxdiff_exptl_absorpt_empirical_full_min 0.392