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_7713589
_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, C24 H20 B'
_chemical_formula_sum            'C67 H58 B Cl P2 Ru'
_chemical_formula_weight         1072.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-08-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-18 deposited with the CCDC.	2023-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.9266(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.47706(6)
_cell_length_b                   16.55786(10)
_cell_length_c                   15.24231(9)
_cell_measurement_reflns_used    35211
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      75.8430
_cell_measurement_theta_min      2.9340
_cell_volume                     2612.17(3)
_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 0.985
_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    -64.00 -39.00   0.50    0.30    --  -81.00 138.00 133.89   50
  2  \w    -94.00 -69.00   0.50    0.30    --  -62.09 156.00  19.00   50
  3  \w   -105.00 -80.00   0.50    0.30    --  -75.91 156.00  19.00   50
  4  \w   -106.00 -81.00   0.50    0.30    --  -76.75 156.00  19.00   50
  5  \w   -120.00 -84.00   0.50    0.30    --  -81.00 139.00  -7.25   72
  6  \w   -119.00 -94.00   0.50    0.30    --  -81.00 138.00  66.35   50
  7  \w   -119.00 -85.00   0.50    0.30    --  -81.00 138.00 133.89   68
  8  \w    -62.00 -37.00   0.50    0.30    --  -81.00 138.00  66.35   50
  9  \w    -67.00 -42.00   0.50    0.30    --  -75.91 120.00-136.00   50
 10  \w   -117.00 -76.00   0.50    0.30    --  -81.00 135.00-173.03   82
 11  \w   -118.00 -91.00   0.50    0.30    --  -81.00 136.00-158.86   54
 12  \w    -99.00 -63.00   0.50    0.30    --  -81.00 118.00-101.92   72
 13  \w    -87.00 -18.00   0.50    0.30    --  -62.09 120.00-136.00  138
 14  \w    -99.00 -74.00   0.50    0.30    --  -62.09   0.00-180.00   50
 15  \w    -73.00 -40.00   0.50    0.30    --  -76.75 111.00  30.00   66
 16  \w   -113.00 -74.00   0.50    0.30    --  -75.91   0.00 150.00   78
 17  \w   -104.00 -75.00   0.50    0.30    --  -72.00 -73.00  41.68   58
 18  \w   -102.00 -67.00   0.50    0.30    --  -60.00 -59.00  51.81   70
 19  \w   -116.00 -90.00   0.50    0.30    --  -81.00 -57.00  85.84   52
 20  \w   -114.00 -88.00   0.50    0.30    --  -80.00 -57.00 122.88   52
 21  \w   -124.00 -89.00   0.50    0.30    --  -81.00 -57.00 116.87   70
 22  \w   -116.00 -81.00   0.50    0.30    --  -72.00 -49.00 160.53   70
 23  \w   -122.00 -97.00   0.50    0.30    --  -81.00 -52.00  13.65   50
 24  \w   -121.00 -90.00   0.50    0.30    --  -81.00 -70.00   2.49   62
 25  \w   -108.00 -74.00   0.50    0.30    --  -64.00 -58.00 -61.06   68
 26  \w   -120.00 -94.00   0.50    0.30    --  -81.00 -45.00-145.07   52
 27  \w   -117.00 -80.00   0.50    0.30    --  -81.00 -85.00 -34.87   74
 28  \w   -107.00 -82.00   0.50    0.30    --  -75.91-156.00 -16.00   50
 29  \w    -98.00 -67.00   0.50    0.30    --  -62.09-156.00 -16.00   62
 30  \w     62.00  88.00   0.50    0.30    --   59.54-156.00 -16.00   52
 31  \w     79.00 112.00   0.50    0.30    --   73.46-156.00 -16.00   66
 32  \w     61.00  86.00   0.50    0.30    --   79.82-156.00 -16.00   50
 33  \w     87.00 121.00   0.50    0.30    --   83.00-138.00  27.65   68
 34  \w     64.00 116.00   0.50    0.30    --   83.00-130.00  60.22  104
 35  \w     40.00  72.00   0.50    0.30    --   79.82-111.00   0.00   64
 36  \w     60.00  86.00   0.50    0.30    --   79.82-120.00 139.00   52
 37  \w     40.00  65.00   0.50    0.30    --   73.46-120.00 139.00   50
 38  \w     43.00  68.00   0.50    0.30    --   59.54-120.00 139.00   50
 39  \w     73.00  99.00   0.50    0.30    --   79.82-111.00  90.00   52
 40  \w     71.00 100.00   0.50    0.30    --   79.82-111.00  60.00   58
 41  \w     75.00 100.00   0.50    0.30    --   79.82-111.00 -60.00   50
 42  \w     39.00  98.00   0.50    0.30    --   79.82-111.00-120.00  118
 43  \w     41.00  94.00   0.50    0.30    --   79.82-111.00-180.00  106
 44  \w     45.00  77.00   0.50    0.30    --   79.82 -95.00-120.00   64
 45  \w     39.00  66.00   0.50    0.30    --   79.82-111.00 -60.00   54
 46  \w     40.00  71.00   0.50    0.30    --   79.82 -95.00 -90.00   62
 47  \w     40.00  67.00   0.50    0.30    --   79.82 -95.00-150.00   54
 48  \w     41.00  86.00   0.50    0.30    --   79.82 -95.00-180.00   90
 49  \w     40.00  65.00   0.50    0.30    --   79.82 -95.00 -30.00   50
 50  \w     41.00  68.00   0.50    0.30    --   79.82 -95.00 -60.00   54
 51  \w     56.00  90.00   0.50    0.30    --   83.00-107.00   9.37   68
 52  \w     43.00 103.00   0.50    0.30    --   83.00-110.00 144.05  120
 53  \w     40.00  65.00   0.50    0.30    --   79.82 -95.00 150.00   50
 54  \w     46.00  74.00   0.50    0.30    --   83.00 -62.00 148.46   56
 55  \w     43.00  86.00   0.50    0.30    --   79.82 -95.00  90.00   86
 56  \w     22.00  62.00   0.50    0.30    --   59.54 -95.00-180.00   80
 57  \w     43.00 113.00   0.50    0.30    --   79.82   0.00   0.00  140
 58  \w     55.00  91.00   0.50    0.30    --   48.00  62.00-132.85   72
 59  \w     50.00  80.00   0.50    0.30    --   44.00  71.00 -40.83   60
 60  \w     61.00  86.00   0.50    0.30    --   52.00  65.00  -6.50   50
 61  \w     92.00 126.00   0.50    0.30    --   83.00  53.00 -23.78   68
 62  \w     82.00 128.00   0.50    0.30    --   79.82  30.00 -90.00   92
 63  \w     86.00 126.00   0.50    0.30    --   79.82  30.00  60.00   80
 64  \w     69.00 131.00   0.50    0.30    --   83.00  24.00 145.61  124
 65  \w     89.00 114.00   0.50    0.30    --   83.00  67.00 164.53   50
 66  \w     81.00 107.00   0.50    0.30    --   79.82  30.00 120.00   52
 67  \w     47.00 115.00   0.50    0.30    --   83.00   8.00  33.65  136
 68  \w     56.00 116.00   0.50    0.30    --   79.82   0.00-120.00  120
 69  \w     66.00  92.00   0.50    0.30    --   79.82   0.00-180.00   52
 70  \w     65.00 122.00   0.50    0.30    --   83.00  23.00-120.99  114
 71  \w     88.00 113.00   0.50    0.30    --   79.82 156.00  19.00   50
 72  \w     72.00  98.00   0.50    0.30    --   79.82 178.00 -30.00   52
 73  \w     61.00  86.00   0.50    0.30    --   73.46 156.00  19.00   50
 74  \w     53.00  85.00   0.50    0.30    --   79.82 178.00  60.00   64
 75  \w     60.00  86.00   0.50    0.30    --   79.82 178.00 120.00   52
 76  \w     67.00 120.00   0.50    0.30    --   79.82 178.00 150.00  106
;
_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      0.0182692000
_diffrn_orient_matrix_UB_12      0.0923308000
_diffrn_orient_matrix_UB_13      0.0003538000
_diffrn_orient_matrix_UB_21      -0.0446419000
_diffrn_orient_matrix_UB_22      0.0020315000
_diffrn_orient_matrix_UB_23      -0.1011767000
_diffrn_orient_matrix_UB_31      -0.1407939000
_diffrn_orient_matrix_UB_32      0.0113243000
_diffrn_orient_matrix_UB_33      0.0152902000
_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  0.0268
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            59800
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.069
_diffrn_reflns_theta_min         2.935
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.798
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.761
_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    1.363
_exptl_crystal_description       prism
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Flack x determined using 4835 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0220(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         10685
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0190
_refine_ls_R_factor_gt           0.0181
_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^)+(0.0201P)^2^+0.5962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0426
_refine_ls_wR_factor_ref         0.0428
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                10430
_reflns_number_total             10685
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02037a2.cif
_cod_data_source_block           jr-iii-185-bph4
_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_database_code               7713589
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C67 H58 B Cl P2 Ru'
_shelx_estimated_absorpt_t_max   0.895
_shelx_estimated_absorpt_t_min   0.703
_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.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), C45(H45), C46(H46), C47(H47), C48(H48),
 C49(H49), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C57(H57), C58(H58),
  C59(H59), C60(H60), C61(H61), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67)
2.b Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C)
;
_shelx_res_checksum              12496
_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 1.209
_oxdiff_exptl_absorpt_empirical_full_min 0.896