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_4518319
_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 O6 Ti'
_chemical_formula_sum            'C14 H8 O6 Ti'
_chemical_formula_weight         320.10
_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     dual
_audit_creation_date             2020-08-21
_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                   16.6433(2)
_cell_length_b                   16.6433(2)
_cell_length_c                   23.8476(4)
_cell_measurement_reflns_used    15571
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.9960
_cell_measurement_theta_min      3.2730
_cell_volume                     6605.77(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -13.00  31.00   0.50    0.62    --    0.00  72.00 -30.00   88
  2  \w    -86.00 -43.00   0.50    0.62    --    0.00 -19.00 -90.00   86
  3  \w    -72.00   8.00   0.50    0.62    --    0.00 -72.00-120.00  160
  4  \w     48.00  84.00   0.50    0.62    --    0.00  72.00 -30.00   72
  5  \w     55.00  89.00   0.50    0.62    --    0.00  19.00-150.00   68
  6  \w    -31.00  12.00   0.50    0.62    --    0.00 -38.00 -60.00   86
  7  \w     -3.00  23.00   0.50    0.62    --    0.00  19.00-150.00   52
  8  \w   -108.00 -48.00   0.50    2.46    --  -98.80  72.00 -90.00  120
  9  \w   -113.00 -78.00   0.50    2.46    --  -98.80  72.00 150.00   70
 10  \w   -111.00 -12.00   0.50    2.46    --  -98.80  19.00-180.00  198
 11  \w   -188.00 -89.00   0.50    2.46    --  -98.80 -38.00-120.00  198
 12  \w   -106.00 -17.00   0.50    2.46    --  -98.80  72.00-180.00  178
 13  \w   -111.00 -22.00   0.50    2.46    --  -98.80  72.00 -30.00  178
 14  \w   -111.00 -59.00   0.50    2.46    --  -98.80  72.00  30.00  104
 15  \w   -188.00 -95.00   0.50    2.46    --  -98.80 -19.00 -60.00  186
 16  \w   -187.00 -85.00   0.50    2.46    --  -98.80 -38.00-150.00  204
 17  \w    -41.00 -15.00   0.50    2.46    --  -98.80  57.00 -60.00   52
 18  \w   -109.00 -59.00   0.50    2.46    --  -98.80  57.00 -60.00  100
 19  \w    -96.00 -38.00   0.50    2.46    --  -98.80  72.00  60.00  116
 20  \w    -99.00 -73.00   0.50    2.46    --  -98.80  72.00-150.00   52
 21  \w   -102.00 -42.00   0.50    2.46    --  -98.80  72.00  90.00  120
 22  \w   -104.00 -52.00   0.50    2.46    --  -98.80  57.00-180.00  104
 23  \w    -41.00 -12.00   0.50    2.46    --  -98.80  57.00-180.00   58
 24  \w   -138.00-113.00   0.50    2.46    --  -98.80 -19.00-120.00   50
 25  \w   -111.00 -86.00   0.50    2.46    --  -98.80  72.00-120.00   50
 26  \w    -35.00 -10.00   0.50    2.46    --  -98.80  72.00 -90.00   50
 27  \w   -106.00 -23.00   0.50    2.46    --  -98.80  72.00   0.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0031959500
_diffrn_orient_matrix_UB_12      -0.0217945500
_diffrn_orient_matrix_UB_13      -0.0627009500
_diffrn_orient_matrix_UB_21      -0.0148937500
_diffrn_orient_matrix_UB_22      0.0885977500
_diffrn_orient_matrix_UB_23      -0.0153941500
_diffrn_orient_matrix_UB_31      0.0913993000
_diffrn_orient_matrix_UB_32      0.0153487000
_diffrn_orient_matrix_UB_33      -0.0003290000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            25763
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.791
_diffrn_reflns_theta_min         3.238
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.599
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 1272 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.034(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         3329
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0658P)^2^+5.2637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.734
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                3168
_reflns_number_total             3329
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tz0c00456_si_002.cif
_cod_data_source_block           FIR-125
_cod_original_cell_volume        6605.77(19)
_cod_database_code               4518319
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.770
_shelx_estimated_absorpt_t_min   0.710
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C9(H9), C3(H3), C6(H6), C11(H11), C12(H12), C8(H8), C2(H2)
;
_shelx_res_checksum              15366
_shelx_hkl_checksum              32238
_shelx_fab_checksum              43459
_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 1.881
_oxdiff_exptl_absorpt_empirical_full_min 0.506