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_7713586
_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, C H2 Cl2, F6 P'
_chemical_formula_sum            'C44 H40 Cl3 F6 P3 Ru'
_chemical_formula_weight         983.09
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-09-02
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.10287(19)
_cell_length_b                   16.6186(2)
_cell_length_c                   17.2511(3)
_cell_measurement_reflns_used    12737
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.3280
_cell_measurement_theta_min      3.6300
_cell_volume                     4329.83(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (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 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_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    -60.00 -35.00   1.00    4.00    --  -42.88 109.00-107.00   25
  2  \w     74.00 168.00   1.00   16.00    --  103.49  22.00 151.00   94
  3  \w     37.00  87.00   1.00   16.00    --  103.49-109.00 157.00   50
  4  \w    145.00 172.00   1.00   16.00    --  103.49 111.00 -15.00   27
  5  \w   -109.00 -32.00   1.00    4.00    --  -42.88 -37.00-120.00   77
  6  \w   -113.00 -21.00   1.00    4.00    --  -42.88 -37.00 150.00   92
  7  \w    -61.00 -34.00   1.00    4.00    --  -42.88 125.00-180.00   27
  8  \w     38.00  66.00   1.00   16.00    --  103.49 -45.00 -90.00   28
  9  \w    110.00 146.00   1.00   16.00    --  103.49 178.00 -60.00   36
 10  \w     65.00 140.00   1.00   16.00    --  103.49 178.00   0.00   75
 11  \w    119.00 150.00   1.00   16.00    --  103.49 111.00-180.00   31
 12  \w     91.00 129.00   1.00   16.00    --  103.49 -45.00 -90.00   38
 13  \w     35.00 128.00   1.00   16.00    --  103.49 -30.00 120.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0901802000
_diffrn_orient_matrix_UB_12      0.0099379000
_diffrn_orient_matrix_UB_13      0.0406035000
_diffrn_orient_matrix_UB_21      -0.0421177000
_diffrn_orient_matrix_UB_22      0.0254286000
_diffrn_orient_matrix_UB_23      -0.0775350000
_diffrn_orient_matrix_UB_31      -0.0222569000
_diffrn_orient_matrix_UB_32      -0.0886068000
_diffrn_orient_matrix_UB_33      -0.0177269000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19149
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.474
_diffrn_reflns_theta_min         3.693
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.174
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.241
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.67a (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 yellow'
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       needle
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.514
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.071
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 3263 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         8383
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0404
_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^)+(0.0601P)^2^+2.9742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1025
_reflns_Friedel_coverage         0.784
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                7948
_reflns_number_total             8383
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02037a2.cif
_cod_data_source_block           jr-iii-185-pf6
_cod_original_cell_volume        4329.83(10)
_cod_database_code               7713586
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C44 H40 F6 P3 Cl3 Ru1'
_shelx_estimated_absorpt_t_max   0.705
_shelx_estimated_absorpt_t_min   0.144
_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. Restrained distances
 Cl5-C45 \\sim Cl4-C45 \\sim Cl2-C44 \\sim Cl3-C44
 with sigma of 0.02
 Cl2-Cl3 \\sim Cl5-Cl4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl2 \\sim Cl3 \\sim C44 \\sim Cl4 \\sim Cl5 \\sim C45: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 2A
Uanis(F5) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
4. Others
 Sof(Cl4)=Sof(Cl5)=Sof(C45)=Sof(H45A)=Sof(H45B)=1-FVAR(1)
 Sof(Cl2)=Sof(Cl3)=Sof(C44)=Sof(H44A)=Sof(H44B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C45(H45A,H45B)
5.b 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.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              10056
_olex2_date_sample_data_collection 2022-09-02
_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 1.361
_oxdiff_exptl_absorpt_empirical_full_min 0.792