Phenolato Ti(IV) Hexacoordinate Complexes as Anticancer Chemotherapy: Enhancement of Solubility, Hydrolytic Stability, and Cytotoxicity
Taha, Mohammad; Tshuva, Edit Y.; Dalton Transactions  (2023) –; doi:10.1039/D3DT00984J

data_7712921
_publ_section_title
;
 Phenolato Ti(IV) Hexacoordinate Complexes as Anticancer Chemotherapy:
 Enhancement of Solubility, Hydrolytic Stability, and Cytotoxicity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00984J
_journal_year                    2023
_chemical_formula_moiety         'C22 H26 F2 N2 O4 Ti'
_chemical_formula_sum            'C22 H26 F2 N2 O4 Ti'
_chemical_formula_weight         468.35
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-31
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-03-31 deposited with the CCDC.	2023-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.8328(2)
_cell_length_b                   10.7428(2)
_cell_length_c                   28.2055(4)
_cell_measurement_reflns_used    44612
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      32.5840
_cell_measurement_theta_min      2.5080
_cell_volume                     4191.42(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_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 0.899
_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    -66.00   3.00   0.50   30.00    --    8.37 -14.00 -88.00  138
  2  \w     10.00  84.00   0.50   30.00    --    8.37  14.00  82.00  148
  3  \w     21.00  54.00   0.50   30.00    --   -9.62  14.00  82.00   66
  4  \w    -59.00 -10.00   0.50   30.00    --    8.37 -37.00 150.00   98
  5  \w     -4.00  82.00   0.50   30.00    --    8.37  37.00 -90.00  172
  6  \w    -23.00  15.00   0.50   30.00    --    8.37 -99.00 -90.00   76
  7  \w    -16.00  17.00   0.50   30.00    --    8.37 -99.00 -60.00   66
  8  \w    -48.00  -9.00   0.50   30.00    --   -9.62 108.00 147.63   78
  9  \w    -48.00  -5.00   0.50   30.00    --   -9.62 108.00 161.49   86
 10  \w    -51.00 -26.00   0.50   30.00    --   -9.62 113.00 178.72   50
 11  \w    -50.00 -25.00   0.50   30.00    --   -9.62 111.00 115.42   50
 12  \w    -46.00 -21.00   0.50   30.00    --   -9.62 104.00  90.73   50
 13  \w    -51.00 -26.00   0.50   30.00    --   -9.62 113.00  79.46   50
 14  \w     -8.00  18.00   0.50   30.00    --   -9.62 -99.00 -90.00   52
 15  \w    -54.00 -29.00   0.50   30.00    --   -9.62 118.00  87.92   50
 16  \w    -57.00 -32.00   0.50   30.00    --   -9.62 125.00 133.01   50
 17  \w    -16.00   9.00   0.50   30.00    --   -9.62  37.00  60.00   50
 18  \w    -16.00  14.00   0.50   30.00    --   -9.62 -99.00  90.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0095602000
_diffrn_orient_matrix_UB_12      -0.0648667000
_diffrn_orient_matrix_UB_13      0.0000245000
_diffrn_orient_matrix_UB_21      -0.0002507000
_diffrn_orient_matrix_UB_22      -0.0000090000
_diffrn_orient_matrix_UB_23      0.0251472000
_diffrn_orient_matrix_UB_31      -0.0503784000
_diffrn_orient_matrix_UB_32      -0.0123112000
_diffrn_orient_matrix_UB_33      -0.0001173000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            99574
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.446
_diffrn_reflns_theta_min         2.062
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.375
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DCM'
_exptl_crystal_size_max          0.787
_exptl_crystal_size_mid          0.345
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         6793
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0495P)^2^+1.4513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5727
_reflns_number_total             6793
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00984j2.cif
_cod_data_source_block           mohammadt3
_cod_database_code               7712921
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C40 H30 N6 O6 Ti '
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.714
_olex2_refinement_description
;
;
_shelx_res_checksum              55262
_shelx_hkl_checksum              35852
_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 1.672
_oxdiff_exptl_absorpt_empirical_full_min 0.764