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_7713584
_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 F3 O3 S'
_chemical_formula_sum            'C44 H38 Cl F3 O3 P2 Ru S'
_chemical_formula_weight         902.26
_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             2022-07-29
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-07-29 deposited with the CCDC.	2023-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.8863(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.47399(8)
_cell_length_b                   10.42115(6)
_cell_length_c                   30.03284(18)
_cell_measurement_reflns_used    25456
_cell_measurement_temperature    139.99(10)
_cell_measurement_theta_max      76.2890
_cell_measurement_theta_min      2.9850
_cell_volume                     3846.09(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.61a (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 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      139.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_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     44.00 109.00   0.50    0.50    --   79.00-144.00  82.74  130
  2  \w     55.00  84.00   0.50    0.50    --   77.03-125.00  90.00   58
  3  \w     50.00  96.00   0.50    0.50    --   79.00-137.00  -9.79   92
  4  \w     42.00  90.00   0.50    0.50    --   77.03-125.00 -60.00   96
  5  \w     49.00  74.00   0.50    0.50    --   77.03-125.00 -90.00   50
  6  \w     46.00  90.00   0.50    0.50    --   77.03-125.00-180.00   88
  7  \w     40.00  99.00   0.50    0.50    --   75.35-125.00   0.00  118
  8  \w     39.00  87.00   0.50    0.50    --   77.03-125.00 120.00   96
  9  \w     65.00  97.00   0.50    0.50    --   77.03-125.00 150.00   64
 10  \w     41.00 102.00   0.50    0.50    --   75.35   0.00  30.00  122
 11  \w     94.00 119.00   0.50    0.50    --   79.00  54.00 -65.43   50
 12  \w     94.00 119.00   0.50    0.50    --   79.00  57.00-150.86   50
 13  \w     49.00 104.00   0.50    0.50    --   75.35  15.00-180.00  110
 14  \w     49.00  74.00   0.50    0.50    --   75.35  15.00-120.00   50
 15  \w     43.00  89.00   0.50    0.50    --   65.71  15.00-180.00   92
 16  \w     83.00 112.00   0.50    0.50    --   75.35  15.00-120.00   58
 17  \w     76.00 104.00   0.50    0.50    --   75.35   0.00-120.00   56
 18  \w     56.00  99.00   0.50    0.50    --   77.03  15.00 -60.00   86
 19  \w     55.00  95.00   0.50    0.50    --   75.35   0.00 -30.00   80
 20  \w     81.00 106.00   0.50    0.50    --   77.03  15.00 -30.00   50
 21  \w     54.00 100.00   0.50    0.50    --   77.03  15.00  60.00   92
 22  \w   -109.00 -68.00   0.50    0.50    --  -70.18 -15.00 -90.00   82
 23  \w   -104.00 -73.00   0.50    0.50    --  -70.18   0.00-150.00   62
 24  \w   -104.00 -73.00   0.50    0.50    --  -70.18   0.00 -60.00   62
 25  \w   -104.00 -73.00   0.50    0.50    --  -70.18   0.00 -30.00   62
 26  \w   -104.00 -73.00   0.50    0.50    --  -70.18   0.00   0.00   62
 27  \w    -67.00 -41.00   0.50    0.50    --  -67.98 125.00  60.00   52
 28  \w    -90.00 -45.00   0.50    0.50    --  -70.18 125.00   0.00   90
 29  \w    -91.00 -41.00   0.50    0.50    --  -67.98 125.00 -90.00  100
 30  \w    -94.00 -66.00   0.50    0.50    --  -75.50 137.00-154.12   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1058512000
_diffrn_orient_matrix_UB_12      0.0116617000
_diffrn_orient_matrix_UB_13      -0.0347424000
_diffrn_orient_matrix_UB_21      0.0552636000
_diffrn_orient_matrix_UB_22      0.0982477000
_diffrn_orient_matrix_UB_23      -0.0270154000
_diffrn_orient_matrix_UB_31      0.0381844000
_diffrn_orient_matrix_UB_32      -0.1097953000
_diffrn_orient_matrix_UB_33      -0.0278482000
_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  0.0176
_diffrn_reflns_av_unetI/netI     0.0137
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            40600
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.592
_diffrn_reflns_theta_min         2.987
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.705
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.632
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.61a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            'clear intense yellow'
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       prism
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.000122(17)
_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   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         7930
_refine_ls_number_restraints     250
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0226
_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^)+(0.0275P)^2^+3.0553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0583
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7431
_reflns_number_total             7930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02037a2.cif
_cod_data_source_block           jr-iii-185_otf
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_cell_volume        3846.10(4)
_cod_database_code               7713584
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C44 H38 Cl F3 O3 P2 Ru S'
_shelx_estimated_absorpt_t_max   0.726
_shelx_estimated_absorpt_t_min   0.548
_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. Restrained distances
 C44B-F2B = C44B-F3B = C44B-F1B
 1.33 with sigma of 0.02
 C44B-S1B
 1.82 with sigma of 0.02
 S1B-O1B = S1B-O2B = S1B-O3B
 1.44 with sigma of 0.02
 C44B-O2B
 2.56 with sigma of 0.04
 C44B-O1B
 2.58 with sigma of 0.04
 C44B-O3B
 2.57 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
S1A \\sim S1B \\sim F1A \\sim F1B \\sim F2A \\sim F2B \\sim F3A \\sim F3B \\sim
O1A \\sim O1B \\sim O2B \\sim O3A \\sim O3B \\sim O4 \\sim C44A \\sim C44B:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
4. Others
 Sof(S1B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(O1B)=Sof(O2B)=Sof(O3B)=Sof(C44B)=1-
 FVAR(1)
 Sof(S1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(O1A)=Sof(O3A)=Sof(O4)=Sof(C44A)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
  C40(H40), C41(H41), C42(H42)
5.b Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C)
;
_shelx_res_checksum              2234
_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 1.309
_oxdiff_exptl_absorpt_empirical_full_min 0.784