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_7060678
_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         'C56 H90 O26 P2 Ti6'
_chemical_formula_sum            'C56 H90 O26 P2 Ti6'
_chemical_formula_weight         1528.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc26plp6
_audit_creation_date             2019-10-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-26 deposited with the CCDC.	2021-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.7660(3)
_cell_length_b                   13.94118(18)
_cell_length_c                   24.7923(3)
_cell_measurement_reflns_used    5654
_cell_measurement_temperature    250.00(10)
_cell_measurement_theta_max      73.5630
_cell_measurement_theta_min      4.1440
_cell_volume                     7177.43(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      250.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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   -112.00 -20.00   1.00    1.50    --  -40.08 -57.00 150.00   92
  2  \w   -114.00 -17.00   1.00    1.50    --  -40.08 -38.00-120.00   97
  3  \w     45.00 118.00   1.00    2.50    --  105.48-125.00 -90.00   73
  4  \w     39.00  65.00   1.00    2.50    --  105.48-125.00  60.00   26
  5  \w     82.00 117.00   1.00    2.50    --  105.48-125.00  60.00   35
  6  \w     83.00 108.00   1.00    2.50    --  105.48  45.00-120.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0552634000
_diffrn_orient_matrix_UB_12      0.0541017000
_diffrn_orient_matrix_UB_13      -0.0282251000
_diffrn_orient_matrix_UB_21      -0.0489075000
_diffrn_orient_matrix_UB_22      -0.0487809000
_diffrn_orient_matrix_UB_23      0.0377000000
_diffrn_orient_matrix_UB_31      0.0071982000
_diffrn_orient_matrix_UB_32      0.0828865000
_diffrn_orient_matrix_UB_33      0.0406579000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            22139
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.584
_diffrn_reflns_theta_max         66.584
_diffrn_reflns_theta_min         3.566
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.473
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       block
_exptl_crystal_F_000             3184
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       0.00017(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         6325
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0641
_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^)+(0.1300P)^2^+7.0422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1786
_refine_ls_wR_factor_ref         0.1956
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5155
_reflns_number_total             6325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01540k2.cif
_cod_data_source_block           ti
_cod_depositor_comments
'Adding full bibliography for 7060677--7060678.cif.'
_cod_original_cell_volume        7177.41(16)
_cod_database_code               7060678
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.536
_shelx_estimated_absorpt_t_min   0.487
_reflns_odcompleteness_completeness 79.36
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 C(H,H,H,H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
C28 \\sim C27A \\sim C27 \\sim C26 \\sim C7 \\sim C8 \\sim C9 \\sim C12 \\sim
C11 \\sim C10 \\sim C13 \\sim C17 \\sim C18 \\sim C16: within 3.8A with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C27) \\sim Ueq, Uanis(C27A) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C26)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C19) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C19A) \\sim Ueq,
Uanis(C25A) \\sim Ueq, Uanis(C24A) \\sim Ueq, Uanis(C23A) \\sim Ueq,
Uanis(C22A) \\sim Ueq, Uanis(C21A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C18) \\sim
Ueq, Uanis(C17) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C7) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
3. Others
 Sof(O13A)=Sof(H13D)=Sof(C19A)=Sof(C25A)=Sof(C24A)=Sof(H24A)=Sof(C23A)=
 Sof(H23A)=Sof(C22A)=Sof(H22A)=Sof(C21A)=Sof(H21A)=1-FVAR(1)
 Sof(O13)=Sof(H13)=Sof(C19)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=Sof(C23)=
 Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=FVAR(1)
 Fixed Sof: H26A(0.5) H26B(0.5) H26C(0.5) H26D(0.5) H26E(0.5) H26F(0.5)
 H28A(0.5) H28B(0.5) H28C(0.5) H28D(0.5) H28E(0.5) H28F(0.5) C27(0.5) H27(0.5)
 C27A(0.5) H27A(0.5)
4.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C14(H14), C17(H17), C27(H27), C27A(H27A)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C21(H21), C22(H22), C23(H23),
 C24(H24), C24A(H24A), C23A(H23A), C22A(H22A), C21A(H21A)
4.c Fitted hexagon refined as free rotating group:
 C19(C21,C22,C23,C24,C25), C19A(C25A,C24A,C23A,C22A,C21A)
4.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C26(H26A,H26B,H26C), C26(H26D,H26E,H26F), C28(H28A,H28B,H28C), C28(H28D,
 H28E,H28F)
4.e Idealised tetrahedral OH refined as rotating group:
 O13(H13), O13A(H13D)
;
_shelx_res_checksum              78568
_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 2.995
_oxdiff_exptl_absorpt_empirical_full_min 0.414