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_7712919
_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 Cl2 N2 O4 Ti'
_chemical_formula_sum            'C22 H26 Cl2 N2 O4 Ti'
_chemical_formula_weight         501.25
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-23
_audit_creation_method
;
Olex2 1.5-ac5-023
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2022-05-23 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            4
_cell_length_a                   9.2345(2)
_cell_length_b                   9.4706(2)
_cell_length_c                   24.6581(5)
_cell_measurement_reflns_used    19791
_cell_measurement_temperature    199.99(10)
_cell_measurement_theta_max      32.0140
_cell_measurement_theta_min      2.3490
_cell_volume                     2156.51(8)
_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      199.99(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 0.905
_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    -21.00   5.00   0.50    2.00    --    8.37 -99.00   0.00   52
  2  \w      8.00  36.00   0.50    2.00    --    8.37 -99.00 -60.00   56
  3  \w     -3.00  80.00   0.50    2.00    --    8.37  57.00 -90.00  166
  4  \w      1.00  59.00   0.50    2.00    --    8.37  57.00 150.00  116
  5  \w    -51.00   5.00   0.50    2.00    --    8.37 -19.00  30.00  112
  6  \w     16.00  42.00   0.50    2.00    --    8.37 -99.00   0.00   52
  7  \w    -12.00  13.00   0.50    2.00    --    8.37 -99.00  90.00   50
  8  \w    -23.00  23.00   0.50    2.00    --   -9.62 -99.00 150.00   92
  9  \w    -19.00  64.00   0.50    2.00    --   -9.62  19.00   0.00  166
;
_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      0.0764214000
_diffrn_orient_matrix_UB_12      -0.0066162000
_diffrn_orient_matrix_UB_13      0.0013336000
_diffrn_orient_matrix_UB_21      -0.0043283000
_diffrn_orient_matrix_UB_22      -0.0080390000
_diffrn_orient_matrix_UB_23      0.0285480000
_diffrn_orient_matrix_UB_31      -0.0063933000
_diffrn_orient_matrix_UB_32      -0.0741812000
_diffrn_orient_matrix_UB_33      -0.0032210000
_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  0.0348
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            33608
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.290
_diffrn_reflns_theta_min         2.304
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.422
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM  -  Methanol'
_exptl_crystal_size_max          0.477
_exptl_crystal_size_mid          0.253
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         6723
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0461P)^2^+0.6207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.903
_reflns_number_gt                6013
_reflns_number_total             6723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00984j2.cif
_cod_data_source_block           mohammadt5
_cod_original_cell_volume        2156.50(8)
_cod_database_code               7712919
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C22H26Cl2N2O4Ti
_chemical_oxdiff_usercomment     L3Ti
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.738
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.53(3)
 0.47(3)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C19(H19), C21(H21)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              95294
_shelx_hkl_checksum              13792
_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 1.405
_oxdiff_exptl_absorpt_empirical_full_min 0.775