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_7713587
_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_absolute_configuration rmad
_chemical_formula_moiety         'C31 H35 Cl N3 P2 Ru, F6 P'
_chemical_formula_sum            'C31 H35 Cl F6 N3 P3 Ru'
_chemical_formula_weight         793.05
_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             2022-08-17
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-17 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                   9.30092(8)
_cell_length_b                   10.67827(8)
_cell_length_c                   32.0935(2)
_cell_measurement_reflns_used    22184
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      75.0420
_cell_measurement_theta_min      2.7510
_cell_volume                     3187.45(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.65a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.65a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.65a (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      140.00(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 0.989
_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   -116.00 -33.00   0.50    0.20    --  -76.75 140.00-147.00  166
  2  \w   -117.00 -85.00   0.50    0.20    --  -80.00 -74.00-157.36   64
  3  \w   -119.00 -94.00   0.50    0.20    --  -81.00-123.00 -86.53   50
  4  \w   -125.00 -99.00   0.50    0.20    --  -81.00 -34.00 -10.69   52
  5  \w   -116.00 -83.00   0.50    0.20    --  -81.00 -77.00 138.31   66
  6  \w   -126.00 -64.00   0.50    0.20    --  -76.75 -25.00  16.00  124
  7  \w   -101.00 -76.00   0.50    0.20    --  -62.09   0.00 -90.00   50
  8  \w     44.00  88.00   0.50    0.20    --   79.82 -95.00 -30.00   88
  9  \w     43.00  76.00   0.50    0.20    --   79.82-111.00 -60.00   66
 10  \w     44.00 127.00   0.50    0.20    --   83.00-147.00 -47.49  166
 11  \w     44.00 121.00   0.50    0.20    --   83.00-137.00-125.96  154
 12  \w     19.00  72.00   0.50    0.20    --   59.54 -98.00-140.00  106
 13  \w     42.00  67.00   0.50    0.20    --   79.82 -98.00-140.00   50
 14  \w     45.00  71.00   0.50    0.20    --   79.82 -95.00-120.00   52
 15  \w     44.00  70.00   0.50    0.20    --   79.82 -95.00 -60.00   52
 16  \w     66.00  91.00   0.50    0.20    --   79.82 -95.00 -90.00   50
 17  \w     40.00  72.00   0.50    0.20    --   79.82 -95.00  90.00   64
 18  \w     55.00  90.00   0.50    0.20    --   79.82 -95.00 120.00   70
 19  \w     52.00  78.00   0.50    0.20    --   83.00   3.00 150.48   52
 20  \w     91.00 118.00   0.50    0.20    --   83.00  76.00  46.62   54
 21  \w     82.00 107.00   0.50    0.20    --   68.00  74.00 -61.78   50
 22  \w     92.00 117.00   0.50    0.20    --   83.00  46.00  -7.65   50
 23  \w     84.00 119.00   0.50    0.20    --   83.00  77.00 -97.90   70
 24  \w     97.00 124.00   0.50    0.20    --   83.00  54.00-117.28   54
 25  \w     81.00 106.00   0.50    0.20    --   68.00  74.00-142.90   50
 26  \w     92.00 129.00   0.50    0.20    --   83.00  53.00-179.99   74
 27  \w     95.00 122.00   0.50    0.20    --   79.82  25.00-179.00   54
 28  \w    102.00 128.00   0.50    0.20    --   79.82  30.00 -90.00   52
 29  \w     85.00 111.00   0.50    0.20    --   79.82  30.00   0.00   52
 30  \w     87.00 127.00   0.50    0.20    --   79.82  30.00 120.00   80
 31  \w     88.00 113.00   0.50    0.20    --   83.00   3.00 150.48   50
 32  \w     76.00 101.00   0.50    0.20    --   79.82 130.00  38.00   50
 33  \w     70.00 117.00   0.50    0.20    --   73.46 140.00-147.00   94
 34  \w     72.00  97.00   0.50    0.20    --   79.82 140.00-147.00   50
;
_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      -0.1652958000
_diffrn_orient_matrix_UB_12      0.0073676000
_diffrn_orient_matrix_UB_13      -0.0017819000
_diffrn_orient_matrix_UB_21      -0.0085774000
_diffrn_orient_matrix_UB_22      -0.0469599000
_diffrn_orient_matrix_UB_23      0.0453235000
_diffrn_orient_matrix_UB_31      0.0059328000
_diffrn_orient_matrix_UB_32      0.1361986000
_diffrn_orient_matrix_UB_33      0.0157359000
_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  0.0282
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            33963
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.220
_diffrn_reflns_theta_min         2.754
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.739
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.665
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.65a (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 light orange'
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description       prism
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.143(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         6575
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0215
_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^)+(0.0255P)^2^+1.6012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0517
_reflns_Friedel_coverage         0.758
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                6374
_reflns_number_total             6575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02037a2.cif
_cod_data_source_block           jr-iii-188
_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        3187.46(4)
_cod_database_code               7713587
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C31 H35 Cl F6 N3 P3 Ru'
_shelx_estimated_absorpt_t_max   0.729
_shelx_estimated_absorpt_t_min   0.582
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.857(7)
 0.143(7)
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. Restrained distances
 F3B-F4B \\sim F1B-F2B \\sim F2B-F3B
 with sigma of 0.02
 P3-F1A \\sim P3-F1B \\sim P3-F5A \\sim P3-F5B \\sim P3-F3A \\sim P3-F3B \\sim
P3-F6A \\sim P3-F6B \\sim P3-
 F2A \\sim P3-F2B \\sim P3-F4A \\sim P3-F4B
 with sigma of 0.02
 F3B-F5B \\sim F1B-F6B \\sim F6B-F3B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
P3 \\sim F1A \\sim F2A \\sim F3A \\sim F4A \\sim F5A \\sim F6A: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
P3 \\sim F1A \\sim F1B \\sim F2A \\sim F2B \\sim F3A \\sim F3B \\sim F4A \\sim
F4B \\sim F5A \\sim F5B \\sim F6A \\sim F6B: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
5. Others
 Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
6.b Aromatic/amide H refined with riding coordinates:
 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)
6.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C)
;
_shelx_res_checksum              66677
_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 1.197
_oxdiff_exptl_absorpt_empirical_full_min 0.846