Anti-breast cancer stem cell activity of titanocene complexes of non-steroidal anti-inflammatory drugs.
Mouriki, Olympia; Passeri, Ginevra; Singh, Karampal; Lamorte, Sarah D.; Singh, Kuldip; Suntharalingam, Kogularamanan; Kilpatrick, Alexander F. R.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 15389–15394; doi:10.1039/d5dt01491c

data_1575691
_publ_section_title
;
 Anti-breast cancer stem cell activity of titanocene complexes of
 non-steroidal anti-inflammatory drugs.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15389
_journal_page_last               15394
_journal_paper_doi               10.1039/d5dt01491c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C40 H38 N2 O4 Ti'
_chemical_formula_sum            'C40 H38 N2 O4 Ti'
_chemical_formula_weight         658.62
_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             2023-01-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6403)
;
_audit_update_record
;
2024-07-23 deposited with the CCDC.	2025-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6103(6)
_cell_length_b                   15.0673(11)
_cell_length_c                   28.670(2)
_cell_measurement_reflns_used    6924
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      72.010
_cell_measurement_theta_min      3.083
_cell_volume                     3287.5(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker D8 Quest Photon III'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1200
_diffrn_reflns_av_unetI/netI     0.0829
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            24807
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.296
_diffrn_reflns_theta_min         3.083
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.565
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.4857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1849 before and 0.0725 after correction.
The Ratio of minimum to maximum transmission is 0.6445.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       plate
_exptl_crystal_F_000             1384
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene, Hexane'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.414(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         6234
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0616
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+2.2773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1606
_refine_ls_wR_factor_ref         0.1671
_reflns_Friedel_coverage         0.716
_reflns_Friedel_fraction_full    0.951
_reflns_Friedel_fraction_max     0.925
_reflns_number_gt                5189
_reflns_number_total             6234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01491c2.cif
_cod_data_source_block           q23004om_0m
_cod_depositor_comments
'Adding full bibliography for 1575690--1575692.cif.'
_cod_original_cell_volume        3287.4(4)
_cod_database_code               1575691
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.853
_shelx_estimated_absorpt_t_min   0.459
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.586(14)
 0.414(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim Ti1: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C9 \\sim C8 \\sim C7 \\sim Ti1: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
4.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C1(H1A), C2(H2A), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7),
 C8(H8), C9(H9), C10(H10), C14(H14), C15(H15), C16(H16), C17(H17), C21(H21),
 C22(H22), C23(H23), C29(H29), C30(H30), C31(H31), C32(H32), C36(H36), C37(H37),
  C38(H38)
4.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C)
;
_shelx_res_checksum              7892
_shelx_hkl_checksum              1339
_olex2_submission_special_instructions 'No special instructions were received'