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_7712918
_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         'C24 H32 N2 O6 Ti, 1.4[CH4O]'
_chemical_formula_sum            'C25.4 H37.6 N2 O7.4 Ti'
_chemical_formula_weight         537.27
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-25
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2023-04-25 deposited with the CCDC.	2023-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.423(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9857(6)
_cell_length_b                   11.4712(4)
_cell_length_c                   15.6851(5)
_cell_measurement_reflns_used    9385
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      31.9430
_cell_measurement_theta_min      2.2610
_cell_volume                     2510.04(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (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      149.99(1)
_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 0.828
_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     11.00  55.00   0.50   40.00    --    8.37  77.00 120.00   88
  2  \w    -62.00 -29.00   0.50   40.00    --    8.37 -19.00  60.00   66
  3  \w    -26.00   1.00   0.50   40.00    --    8.37 -19.00  60.00   54
  4  \w    -65.00  21.00   0.50   40.00    --    8.37 -37.00-180.00  172
  5  \w    -20.00  20.00   0.50   40.00    --   -9.62 -99.00 -90.00   80
  6  \w     -5.00  21.00   0.50   40.00    --   -9.62 -99.00-150.00   52
;
_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      -0.0013698000
_diffrn_orient_matrix_UB_12      -0.0617558000
_diffrn_orient_matrix_UB_13      0.0009846000
_diffrn_orient_matrix_UB_21      0.0507242000
_diffrn_orient_matrix_UB_22      -0.0014966000
_diffrn_orient_matrix_UB_23      0.0208731000
_diffrn_orient_matrix_UB_31      -0.0035532000
_diffrn_orient_matrix_UB_32      0.0021128000
_diffrn_orient_matrix_UB_33      0.0438434000
_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  0.0318
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.828
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22173
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.251
_diffrn_reflns_theta_min         2.299
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
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    1.422
_exptl_crystal_description       plate
_exptl_crystal_F_000             1141
_exptl_crystal_size_max          0.512
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         7369
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0620P)^2^+0.3288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1164
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5442
_reflns_number_total             7369
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00984j2.cif
_cod_data_source_block           mohammadt
_cod_original_formula_sum        'C25.40 H37.60 N2 O7.40 Ti'
_cod_database_code               7712918
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H32 N2 O6 Ti'
_chemical_oxdiff_usercomment     L1Ti
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.825
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C20(H20), C22(H22)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              54653
_shelx_hkl_checksum              34485
_shelx_fab_checksum              81087
_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 1.466
_oxdiff_exptl_absorpt_empirical_full_min 0.736