Ru(II)-diphosphine/N,S-mercapto complexes and their anti-melanoma properties.
da Silva, Nádija N P; Palmeira-Mello, Marcos V; Acésio, Nathália O; Moraes, Carlos A. F.; Honorato, João; Castellano, Eduardo E.; Tavares, Denise C.; Oliveira, Katia M.; Batista, Alzir A.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 605–615; doi:10.1039/d4dt02575j

data_7717504
_publ_section_title
;
 Ru(II)-diphosphine/N,S-mercapto complexes and their anti-melanoma
 properties.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              605
_journal_page_last               615
_journal_paper_doi               10.1039/d4dt02575j
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C28 H21 N6 O Ru S, F6 P, 0.9[H2O], 0.1[H2O]'
_chemical_formula_sum            'C28 H23 F6 N6 O2 P Ru S'
_chemical_formula_weight         753.629
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_audit_creation_date             2024-05-14
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-14 deposited with the CCDC.	2024-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.6637(13)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.8405(3)
_cell_length_b                   13.02075(15)
_cell_length_c                   21.5213(3)
_cell_measurement_reflns_used    19493
_cell_measurement_temperature    100
_cell_measurement_theta_max      79.0610
_cell_measurement_theta_min      2.1970
_cell_volume                     5798.38(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9975
_diffrn_measured_fraction_theta_max 0.9841
_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    -25.00  22.00   0.50    0.05    --  -48.82  19.00 -90.00   94
  2  \w    -51.00 -20.00   0.50    0.17    --  -90.00  45.00  30.00   62
  3  \w    -73.00 -48.00   0.50    0.17    --  -90.00  90.00 170.00   50
  4  \w    -76.00  20.00   0.50    0.05    --  -48.82  90.00 170.00  192
  5  \w    143.00 169.00   0.50    0.17    --  111.50  90.00 170.00   52
  6  \w    103.00 175.00   0.50    0.17    --  111.50 125.00 -60.00  144
  7  \w    152.00 178.00   0.50    0.17    --  111.50 125.00-120.00   52
  8  \w    136.00 177.00   0.50    0.17    --  111.50 125.00 -90.00   82
  9  \w     97.00 134.00   0.50    0.17    --  111.50 125.00-120.00   74
 10  \w     97.00 122.00   0.50    0.17    --  111.50 125.00 -90.00   50
 11  \w    102.00 128.00   0.50    0.17    --  111.50  90.00 170.00   52
 12  \w    139.00 165.00   0.50    0.17    --  111.50  77.00 120.00   52
 13  \w    148.00 174.00   0.50    0.17    --  111.50  45.00 120.00   52
 14  \w    118.00 143.00   0.50    0.17    --  111.50  45.00 120.00   50
 15  \w    101.00 126.00   0.50    0.17    --  111.50  77.00 120.00   50
 16  \w    115.00 178.00   0.50    0.17    --  111.50  45.00  60.00  126
 17  \w    108.00 133.00   0.50    0.17    --  111.50  45.00  90.00   50
 18  \w    109.00 136.00   0.50    0.17    --  111.50  45.00   0.00   54
 19  \w    117.00 143.00   0.50    0.17    --  111.50  30.00  30.00   52
 20  \w    117.00 143.00   0.50    0.17    --  111.50  45.00 -60.00   52
 21  \w    118.00 151.00   0.50    0.17    --  111.50  61.00-180.00   66
 22  \w    138.00 163.00   0.50    0.17    --  111.50  30.00-120.00   50
 23  \w    153.00 178.00   0.50    0.17    --  111.50  45.00 -60.00   50
 24  \w    101.00 148.00   0.50    0.17    --  111.50  15.00  30.00   94
 25  \w    119.00 162.00   0.50    0.17    --  111.50  15.00 120.00   86
 26  \w     41.00  66.00   0.50    0.17    --  111.50 -61.00  90.00   50
 27  \w     45.00 100.00   0.50    0.17    --  111.50 -77.00  90.00  110
 28  \w     44.00  69.00   0.50    0.17    --  111.50 -61.00  30.00   50
 29  \w     42.00  68.00   0.50    0.17    --  111.50 -61.00   0.00   52
 30  \w     44.00  95.00   0.50    0.17    --  111.50 -77.00   0.00  102
 31  \w     42.00  69.00   0.50    0.17    --  111.50 -61.00 -60.00   54
 32  \w     42.00 103.00   0.50    0.17    --  111.50 -77.00-150.00  122
 33  \w     42.00  86.00   0.50    0.17    --  111.50 -77.00 -90.00   88
 34  \w     42.00  70.00   0.50    0.17    --  111.50 -61.00 120.00   56
 35  \w     42.00  67.00   0.50    0.17    --  111.50-125.00   0.00   50
 36  \w     82.00 107.00   0.50    0.17    --  111.50-125.00-120.00   50
 37  \w     76.00 110.00   0.50    0.17    --  111.50-125.00   0.00   68
 38  \w     72.00 101.00   0.50    0.17    --  111.50-125.00  30.00   58
 39  \w     86.00 111.00   0.50    0.17    --  111.50-125.00  60.00   50
 40  \w     86.00 111.00   0.50    0.17    --  111.50-125.00 120.00   50
 41  \w     64.00  99.00   0.50    0.17    --  111.50 -95.00  90.00   70
 42  \w     62.00  91.00   0.50    0.17    --  111.50 -90.00  56.00   58
 43  \w     47.00  95.00   0.50    0.17    --  111.50-125.00-150.00   96
 44  \w     58.00  83.00   0.50    0.17    --  111.50 -95.00 -90.00   50
 45  \w      3.00  53.00   0.50    0.05    --   48.82 -90.00  56.00  100
 46  \w   -113.00 -76.00   0.50    0.05    --  -48.82-125.00   0.00   74
 47  \w   -114.00 -88.00   0.50    0.05    --  -48.82-125.00-120.00   52
 48  \w   -102.00 -76.00   0.50    0.05    --  -48.82-125.00-150.00   52
 49  \w   -144.00-119.00   0.50    0.17    --  -90.00 -90.00  56.00   50
 50  \w   -120.00 -74.00   0.50    0.05    --  -48.82-125.00 150.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0606858000
_diffrn_orient_matrix_UB_12      0.0431372000
_diffrn_orient_matrix_UB_13      0.0124926000
_diffrn_orient_matrix_UB_21      -0.0050227000
_diffrn_orient_matrix_UB_22      -0.0984152000
_diffrn_orient_matrix_UB_23      0.0378777000
_diffrn_orient_matrix_UB_31      0.0428540000
_diffrn_orient_matrix_UB_32      0.0495163000
_diffrn_orient_matrix_UB_33      0.0641694000
_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  0.0537
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.9975
_diffrn_reflns_Laue_measured_fraction_max 0.9841
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33080
_diffrn_reflns_point_group_measured_fraction_full 0.9975
_diffrn_reflns_point_group_measured_fraction_max 0.9841
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         79.43
_diffrn_reflns_theta_min         4.01
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.280
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_description       block
_exptl_crystal_F_000             3041.133
_exptl_crystal_size_max          0.251
_exptl_crystal_size_mid          0.192
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.9441
_refine_diff_density_min         -1.2206
_refine_diff_density_rms         0.0973
_refine_ls_d_res_high            0.7842
_refine_ls_d_res_low             11.0204
_refine_ls_goodness_of_fit_ref   1.0370
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    42
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0370
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          -0.0008
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+20.1700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0916
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              26
_reflns_limit_h_min              -27
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                5903
_reflns_number_total             6203
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt02575j2.cif
_cod_data_source_block           Ru5-nadija
_cod_depositor_comments
'Adding full bibliography for 7717503--7717505.cif.'
_cod_original_cell_volume        5798.37(13)
_cod_original_formula_sum        'C28 H23 F6 N6 O2 P1 Ru1 S1'
_cod_database_code               7717504
_chemical_oxdiff_formula         'Ru1 N4 C33 H6 S1'
_chemical_oxdiff_usercomment     'Alzir Nadija'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
  C25(H25), C26(H26), C27(H27), C28(H28)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.130
_oxdiff_exptl_absorpt_empirical_full_min 0.606