Effects of organic ammonium cations on the isolation of {Ti<sub>4</sub>} cyclic clusters from water: an <sup>17</sup>O NMR study.
Liu, Weiming; Liu, Caiyun; Wu, Wenli; Zhang, Guanyun; Zhang, Jian; Tung, Chen-Ho; Wang, Yifeng; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5957–5964; doi:10.1039/d0dt00165a

data_7703976
_publ_section_title
;
 Effects of organic ammonium cations on the isolation of {Ti<sub>4</sub>}
 cyclic clusters from water: an <sup>17</sup>O NMR study.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5957
_journal_page_last               5964
_journal_paper_doi               10.1039/d0dt00165a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'H8 O40 S8 Ti4, 10[H2O]'
_chemical_formula_sum            'H28 O50 S8 Ti4'
_chemical_formula_weight         1276.30
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2020-03-09
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2020.03.04 svn.rc2590c38 for OlexSys, GUI svn.r5830)
;
_audit_update_record
;
2020-04-01 deposited with the CCDC.	2020-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   24.0919(2)
_cell_length_b                   24.0919(2)
_cell_length_c                   23.1592(3)
_cell_measurement_reflns_used    11452
_cell_measurement_temperature    173
_cell_measurement_theta_max      76.4890
_cell_measurement_theta_min      2.5990
_cell_volume                     13442.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17257
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.480
_diffrn_reflns_theta_min         2.647
_exptl_absorpt_coefficient_mu    10.586
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.53281
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_description       block
_exptl_crystal_F_000             7728
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 2505 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         6388
_refine_ls_number_restraints     359
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0396P)^2^+117.7442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1175
_reflns_Friedel_coverage         0.810
_reflns_Friedel_fraction_full    0.963
_reflns_Friedel_fraction_max     0.927
_reflns_number_gt                6032
_reflns_number_total             6388
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00165a2.cif
_cod_data_source_block           ti4-hmta
_cod_depositor_comments
'Adding full bibliography for 7703974--7703977.cif.'
_cod_original_cell_volume        13442.1(3)
_cod_database_code               7703976
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O17-O1A \\sim O17-O1B \\sim O1A-O1B \\sim O1B-O1C
 with sigma of 0.002
 S1-O17 \\sim S1-O1A \\sim S1-O1B \\sim S1-O1C
 with sigma of 0.001
 O17-O1A \\sim O17A-O31
 with sigma of 0.04
 Ti1-O17 \\sim Ti1-O17A
 with sigma of 0.02
 S1-O17 \\sim S1A-O17A
 with sigma of 0.02
 S1-O1A \\sim S1A-O31
 with sigma of 0.02
 S1-O1B \\sim S1A-O1D
 with sigma of 0.02
 O1A-O1C \\sim O31-O1E
 with sigma of 0.04
 S1-O1C \\sim S1A-O1E
 with sigma of 0.02
 O17-O1C \\sim O17A-O1E
 with sigma of 0.04
 O17-O1B \\sim O17A-O1D
 with sigma of 0.04
 O1A-O1B \\sim O31-O1D
 with sigma of 0.04
 O1B-O1C \\sim O1D-O1E
 with sigma of 0.04
 Ti1-S1 \\sim Ti1-S1A
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(S1A)=Sof(O17A)=Sof(O31)=Sof(O1D)=Sof(O1E)=1-FVAR(1)
 Sof(S1)=Sof(O17)=Sof(O1A)=Sof(O1B)=Sof(O1C)=FVAR(1)
5.a Rotating group:
 O24(H24A,H24B), O9(H9A,H9B), O4(H4A,H4B)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1249 electrons were
found in a volume of 2687\%A^3 in 1 void per unit cell.
This is consistent with the presence of 10[H2O] per Formula Unit 
which account for 1200 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.1
_smtbx_masks_void_truncation_radius 0.8
_shelx_res_checksum              55832
_shelx_fab_checksum              3780
_olex2_submission_special_instructions 'No special instructions were received'