Tartrate-stabilized titanium–oxo clusters containing sulfonate chromophore ligands: synthesis, crystal structures and photochemical properties
Mou, Wen-Yu; Xie, Bin; Li, Xiao-Long; Lai, Chuan; Li, Tao; Chen, Luo; Feng, Jian-Shen; Bai, Xiao-Xue; Wu, Yu; Wu, Wei-Ping; Zhang, Dong-Liang; Gu, Yun-Tian; New Journal of Chemistry 45 (2021) 10930–10939; doi:10.1039/D1NJ01540K

data_7060677
_publ_section_title
;
 Tartrate-stabilized titanium--oxo clusters containing sulfonate
 chromophore ligands: synthesis, crystal structures and photochemical
 properties
;
_journal_issue                   24
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10930
_journal_page_last               10939
_journal_paper_doi               10.1039/D1NJ01540K
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C24 H44 N O11 S Ti2'
_chemical_formula_sum            'C24 H44 N O11 S Ti2'
_chemical_formula_weight         650.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc26pln5
_audit_creation_date             2020-09-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2020-11-26 deposited with the CCDC.	2021-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                80.698(2)
_cell_angle_beta                 84.378(2)
_cell_angle_gamma                75.812(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0196(13)
_cell_length_b                   11.0526(14)
_cell_length_c                   13.9779(17)
_cell_measurement_reflns_used    1998
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.34
_cell_volume                     1625.8(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.1237
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8253
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.371
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0804 before and 0.0319 after correction.
The Ratio of minimum to maximum transmission is 0.8623.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       block
_exptl_crystal_F_000             686
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         5683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1374
_refine_ls_R_factor_gt           0.0665
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0718P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2952
_reflns_number_total             5683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01540k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7060677--7060678.cif.'
_cod_database_code               7060677
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Rotating group:
 N1(H1A,H1B)
2.b Ternary CH refined with riding coordinates:
 C4(H4), C9(H9), C10(H10), C11(H11), C14(H14), C16(H16)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C8(H8)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,
 H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              40327
_olex2_submission_special_instructions 'No special instructions were received'