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_7717503
_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         'C58 H50 Cl N2 O P4 Ru S, F6 P, 2.6[H2O]'
_chemical_formula_sum            'C58 H55.2 Cl F6 N2 O3.6 P5 Ru S'
_chemical_formula_weight         1275.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-10
_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                 99.3892(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7150(2)
_cell_length_b                   11.48250(12)
_cell_length_c                   28.1918(3)
_cell_measurement_reflns_used    28588
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.9610
_cell_measurement_theta_min      1.9120
_cell_volume                     5657.74(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.55a (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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_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    -29.00   5.00   0.50   92.58    --   -4.60 -27.00 -59.00   68
  2  \w    -78.00 -46.00   0.50   92.58    --   -4.60 -27.00 -59.00   64
  3  \w    -23.00   2.00   0.50   92.58    --   -4.60 -99.00-180.00   50
  4  \w    -15.00  24.00   0.50   92.58    --   -4.60 -99.00 -60.00   78
  5  \w    -17.00  20.00   0.50   92.58    --   -4.60 -99.00-120.00   74
  6  \w    -14.00  68.00   0.50   92.58    --   -4.60  27.00 103.00  164
  7  \w    -20.00   5.00   0.50   92.58    --    5.15 -19.00 -90.00   50
;
_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      -0.0343481000
_diffrn_orient_matrix_UB_12      0.0202463000
_diffrn_orient_matrix_UB_13      0.0070426000
_diffrn_orient_matrix_UB_21      -0.0162241000
_diffrn_orient_matrix_UB_22      0.0080617000
_diffrn_orient_matrix_UB_23      -0.0244940000
_diffrn_orient_matrix_UB_31      -0.0142919000
_diffrn_orient_matrix_UB_32      -0.0578044000
_diffrn_orient_matrix_UB_33      -0.0009419000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            43832
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.750
_diffrn_reflns_theta_min         1.919
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.55a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       block
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.128
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         10730
_refine_ls_number_restraints     948
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+15.3108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1047
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9724
_reflns_number_total             10730
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02575j2.cif
_cod_data_source_block           Ru1-nadija
_cod_depositor_comments
'Adding full bibliography for 7717503--7717505.cif.'
_cod_original_cell_volume        5657.75(12)
_cod_original_formula_sum        'C58 H55.20 Cl F6 N2 O3.60 P5 Ru S'
_cod_database_code               7717503
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'RU1 C20 H20 P3 F6 S1 N3'
_chemical_oxdiff_usercomment     'Cristal NAD'
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.931
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
C420 \\sim C430 \\sim C431 \\sim C432 \\sim C433 \\sim C434: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C211 \\sim C231 \\sim C232 \\sim C233 \\sim C234 \\sim C235: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C211 \\sim C212 \\sim C213 \\sim C214 \\sim C215 \\sim C216: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C221 \\sim C241 \\sim C242 \\sim C243 \\sim C244 \\sim C245: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C221 \\sim C222 \\sim C223 \\sim C224 \\sim C225 \\sim C226: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C212(0.5) H212(0.5) C213(0.5) H213(0.5) C214(0.5) H214(0.5)
 C215(0.5) H215(0.5) C216(0.5) H216(0.5) C222(0.5) H222(0.5) C223(0.5)
 H223(0.5) C224(0.5) H224(0.5) C225(0.5) H225(0.5) C226(0.5) H226(0.5)
 C231(0.5) H231(0.5) C232(0.5) H232(0.5) C233(0.5) H233(0.5) C234(0.5)
 H234(0.5) C235(0.5) H235(0.5) C241(0.5) H241(0.5) C242(0.5) H242(0.5)
 C243(0.5) H243(0.5) C244(0.5) H244(0.5) C245(0.5) H245(0.5) C421(0.5)
 H421(0.5) C422(0.5) H422(0.5) C423(0.5) H423(0.5) C424(0.5) H424(0.5)
 C425(0.5) H425(0.5) C430(0.5) H430(0.5) C431(0.5) H431(0.5) C432(0.5)
 H432(0.5) C433(0.5) H433(0.5) C434(0.5) H434(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C60(H60A,H60B)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C112(H112), C113(H113),
 C114(H114), C115(H115), C116(H116), C122(H122), C123(H123), C124(H124),
 C125(H125), C126(H126), C212(H212), C213(H213), C214(H214), C215(H215),
 C216(H216), C222(H222), C223(H223), C224(H224), C225(H225), C226(H226),
 C231(H231), C232(H232), C233(H233), C234(H234), C235(H235), C241(H241),
 C242(H242), C243(H243), C244(H244), C245(H245), C311(H311), C312(H312),
 C313(H313), C314(H314), C315(H315), C321(H321), C322(H322), C323(H323),
 C324(H324), C325(H325), C411(H411), C412(H412), C413(H413), C414(H414),
 C415(H415), C421(H421), C422(H422), C423(H423), C424(H424), C425(H425),
 C430(H430), C431(H431), C432(H432), C433(H433), C434(H434)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              73322
_shelx_hkl_checksum              39159
_shelx_fab_checksum              19525
_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 1.155
_oxdiff_exptl_absorpt_empirical_full_min 0.899