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_7712920
_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         'C26 H36 N2 O6 Ti, C2 H3 N'
_chemical_formula_sum            'C28 H39 N3 O6 Ti'
_chemical_formula_weight         561.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-25
_audit_creation_method
;
Olex2 1.5-ac5-023
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2022-05-25 deposited with the CCDC.	2023-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.781(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7034(5)
_cell_length_b                   13.0271(3)
_cell_length_c                   11.6836(3)
_cell_measurement_reflns_used    17696
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      32.2770
_cell_measurement_theta_min      2.2830
_cell_volume                     2710.74(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (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 0.999
_diffrn_measured_fraction_theta_max 0.809
_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    -20.00  23.00   0.50    5.00    --   -9.62 -99.00 150.00   86
  2  \w    -23.00   7.00   0.50    5.00    --   -9.62 -99.00  90.00   60
  3  \w    -34.00  39.00   0.50    5.00    --    8.37 -93.00 -56.00  146
  4  \w    -31.00  -3.00   0.50    5.00    --   -9.62 -93.00 -56.00   56
  5  \w    -15.00  31.00   0.50    5.00    --   -9.62  93.00  55.00   92
  6  \w     -2.00  75.00   0.50    5.00    --    8.37  37.00  90.00  154
;
_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      -0.0000704000
_diffrn_orient_matrix_UB_12      0.0502731000
_diffrn_orient_matrix_UB_13      0.0232551000
_diffrn_orient_matrix_UB_21      -0.0398176000
_diffrn_orient_matrix_UB_22      -0.0005299000
_diffrn_orient_matrix_UB_23      -0.0182293000
_diffrn_orient_matrix_UB_31      0.0008909000
_diffrn_orient_matrix_UB_32      -0.0209158000
_diffrn_orient_matrix_UB_33      0.0564778000
_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  0.0306
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.809
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28204
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.809
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.379
_diffrn_reflns_theta_min         2.287
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.363
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.55a (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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: ACN'
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         7874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+1.1434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6365
_reflns_number_total             7874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00984j2.cif
_cod_data_source_block           mohammadt6a
_cod_database_code               7712920
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C28 H39 N3 O6 Ti'
_chemical_oxdiff_usercomment     L2Ti
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.851
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,
 H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C24(H24A,H24B,H24C),
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C2S(H2SA,H2SB,H2SC)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              68500
_shelx_hkl_checksum              95887
_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 1.211
_oxdiff_exptl_absorpt_empirical_full_min 0.833