Fine-tuning the cytotoxicity of ruthenium(II) arene compounds to enhance selectivity against breast cancers
Pereira, Sarah; Romano-deGea, Jan; Barbosa, Ana Isabel; Costa Lima, Sofia A.; Dyson, Paul Joseph; Saraiva, M. Lúcia M.F.S.; Dalton Transactions  (2023) –; doi:10.1039/D3DT02037A

data_7713588
_publ_section_title
;
 Fine-tuning the cytotoxicity of ruthenium(II) arene compounds to enhance
 selectivity against breast cancers
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02037A
_journal_year                    2023
_chemical_formula_moiety         'C43 H38 Cl P2 Ru, F6 Sb'
_chemical_formula_sum            'C43 H38 Cl F6 P2 Ru Sb'
_chemical_formula_weight         988.94
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-06-08
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-09-29 deposited with the CCDC.	2023-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.752(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3243(4)
_cell_length_b                   10.3143(3)
_cell_length_c                   30.4650(9)
_cell_measurement_reflns_used    8869
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      29.2430
_cell_measurement_theta_min      3.3920
_cell_volume                     3816.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.58a (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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.859
_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    -40.00  32.00   1.00   20.00    --  -11.81  29.00 -28.00   72
  2  \w    -44.00 -18.00   1.00   20.00    --  -11.81 -29.00 170.00   26
  3  \w     39.00  96.00   1.00   20.00    --   11.50 178.00 150.00   57
  4  \w     40.00  67.00   1.00   20.00    --   11.50 178.00  30.00   27
  5  \w    -24.00  21.00   1.00   20.00    --  -11.81  77.00-150.00   45
  6  \w    -40.00  21.00   1.00   20.00    --  -11.81  77.00   0.00   61
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0189690000
_diffrn_orient_matrix_UB_12      -0.0083088000
_diffrn_orient_matrix_UB_13      0.0231399000
_diffrn_orient_matrix_UB_21      -0.0523082000
_diffrn_orient_matrix_UB_22      -0.0245995000
_diffrn_orient_matrix_UB_23      0.0025689000
_diffrn_orient_matrix_UB_31      0.0177449000
_diffrn_orient_matrix_UB_32      -0.0636599000
_diffrn_orient_matrix_UB_33      -0.0040177000
_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  0.0827
_diffrn_reflns_av_unetI/netI     0.0974
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.859
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            28482
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.599
_diffrn_reflns_theta_min         2.749
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.319
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.807
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.58a (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            'clear intense orange'
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_description       prism
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.945
_refine_diff_density_min         -1.274
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.00018(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         9225
_refine_ls_number_restraints     288
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0269P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6469
_reflns_number_total             9225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02037a2.cif
_cod_data_source_block           jr-iii-185-sbf6
_cod_database_code               7713588
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C43 H38 F6 P2 Cl1 Sb1 Ru1'
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.791
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Sb1 \\sim F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim Sb2 \\sim F7
\\sim F8 \\sim F9 \\sim F10 \\sim F11 \\sim F12: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 2A
3. Rigid body (RIGU) restrains
 Sb1, F1, F2, F3, F4, F5, F6, Sb2, F7, F8, F9, F10, F11, F12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(Sb2)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=1-FVAR(1)
 Sof(Sb1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30),
 C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40),
  C41(H41), C42(H42), C43(H43)
5.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              74122
_olex2_date_sample_data_collection 2022-06-03
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 3.184
_oxdiff_exptl_absorpt_empirical_full_min 0.210