The coordination chemistry and anticancer activity of organo-ruthenium(II), -iridium(III) and -rhodium(III) complexes with sulfonyl-substituted thiourea ligands.
Risi, Matthew C.; Stjärnhage, Julia; Henderson, William; Lane, Joseph R.; Hartinger, Christian G.; Saunders, Graham C.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 539–549; doi:10.1039/d4dt02733g

data_7717544
_publ_section_title
;
 The coordination chemistry and anticancer activity of
 organo-ruthenium(II), -iridium(III) and -rhodium(III) complexes with
 sulfonyl-substituted thiourea ligands.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              539
_journal_page_last               549
_journal_paper_doi               10.1039/d4dt02733g
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C48 H52 N4 O4 Ru2 S4'
_chemical_formula_sum            'C48 H52 N4 O4 Ru2 S4'
_chemical_formula_weight         1079.367
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-10-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-10-25 deposited with the CCDC.	2024-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.177(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.1894(6)
_cell_length_b                   9.2198(2)
_cell_length_c                   23.8717(5)
_cell_measurement_reflns_used    10809
_cell_measurement_temperature    120.0(4)
_cell_measurement_theta_max      72.0270
_cell_measurement_theta_min      3.9690
_cell_volume                     4726.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.9835
_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    -42.00  15.00   0.50    3.34    --  -46.48  38.00  90.00  114
  2  \w    -36.00 -11.00   0.50   13.36    --  -90.25  32.00 -40.00   50
  3  \w    -25.00  33.00   0.50    3.34    --  -46.48  32.00 -40.00  116
  4  \w     93.00 124.00   0.50    3.34    --   46.48  32.00 -40.00   62
  5  \w    144.00 169.00   0.50   13.36    --   97.33  32.00 -40.00   50
  6  \w    115.00 175.00   0.50   13.36    --   97.33 111.00 -90.00  120
  7  \w     96.00 142.00   0.50   13.36    --   97.33  32.00 -40.00   92
  8  \w     75.00 118.00   0.50    3.34    --   46.48  57.00  90.00   86
  9  \w     76.00 168.00   0.50   13.36    --   97.33  77.00  30.00  184
 10  \w     64.00 146.00   0.50   13.36    --   97.33 178.00 -60.00  164
 11  \w     33.00  69.00   0.50    3.34    --   46.48  57.00  90.00   72
 12  \w     22.00  49.00   0.50   13.36    --   97.33 -45.00 -60.00   54
 13  \w     25.00  50.00   0.50   13.36    --   97.33 -61.00 -30.00   50
 14  \w     33.00 102.00   0.50   13.36    --   97.33 -95.00  30.00  138
 15  \w     71.00 105.00   0.50   13.36    --   97.33 -95.00  90.00   68
 16  \w     73.00 100.00   0.50   13.36    --   97.33 -77.00  90.00   54
 17  \w     60.00 109.00   0.50   13.36    --   97.33-111.00  90.00   98
 18  \w     56.00 100.00   0.50   13.36    --   97.33-111.00 -30.00   88
 19  \w     79.00 109.00   0.50   13.36    --   97.33-111.00 -90.00   60
 20  \w     79.00 104.00   0.50   13.36    --   97.33 -77.00-180.00   50
 21  \w     79.00 109.00   0.50   13.36    --   97.33-111.00-180.00   60
 22  \w     60.00  94.00   0.50   13.36    --   97.33-111.00-150.00   68
 23  \w     56.00 102.00   0.50   13.36    --   97.33 -77.00-150.00   92
 24  \w     61.00 106.00   0.50   13.36    --   97.33-111.00 -60.00   90
 25  \w     44.00  71.00   0.50   13.36    --   97.33-111.00-180.00   54
 26  \w     27.00  62.00   0.50   13.36    --   97.33 -77.00-180.00   70
 27  \w     26.00  69.00   0.50   13.36    --   97.33 -61.00 -90.00   86
 28  \w     27.00  71.00   0.50   13.36    --   97.33 -61.00 -60.00   88
 29  \w     23.00 107.00   0.50   13.36    --   97.33-111.00  30.00  168
 30  \w     26.00  64.00   0.50   13.36    --   97.33 -61.00  90.00   76
 31  \w     23.00  61.00   0.50   13.36    --   97.33 -77.00  90.00   76
 32  \w     19.00  58.00   0.50   13.36    --   97.33 -95.00  90.00   78
 33  \w    -22.00  36.00   0.50    3.34    --   46.48 -32.00 159.00  116
 34  \w    -72.00  30.00   0.50    3.34    --  -46.48  77.00 -30.00  204
 35  \w    -50.00 -12.00   0.50   13.36    --  -90.25  45.00 150.00   76
 36  \w    -57.00 -31.00   0.50   13.36    --  -90.25 111.00  30.00   52
 37  \w    -96.00 -67.00   0.50   13.36    --  -90.25 -15.00-150.00   58
 38  \w   -128.00-100.00   0.50   13.36    --  -90.25 -15.00-150.00   56
 39  \w   -104.00 -76.00   0.50    3.34    --  -46.48-125.00 -30.00   56
 40  \w   -144.00 -84.00   0.50   13.36    --  -90.25 -95.00  60.00  120
 41  \w    -96.00 -56.00   0.50    3.34    --  -46.48 -32.00 159.00   80
 42  \w   -126.00 -99.00   0.50    3.34    --  -46.48 -32.00 159.00   54
 43  \w   -168.00 -74.00   0.50   13.36    --  -90.25 -32.00 159.00  188
 44  \w   -160.00-101.00   0.50   13.36    --  -90.25 -61.00 120.00  118
 45  \w   -172.00-139.00   0.50   13.36    --  -90.25 -15.00-150.00   66
 46  \w     23.00  70.00   0.50   13.36    --   97.33-111.00 -90.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0704068000
_diffrn_orient_matrix_UB_12      0.0136708000
_diffrn_orient_matrix_UB_13      0.0145278000
_diffrn_orient_matrix_UB_21      -0.0006320000
_diffrn_orient_matrix_UB_22      0.1544282000
_diffrn_orient_matrix_UB_23      0.0244582000
_diffrn_orient_matrix_UB_31      0.0138140000
_diffrn_orient_matrix_UB_32      -0.0625067000
_diffrn_orient_matrix_UB_33      0.0635712000
_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  0.0796
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.9991
_diffrn_reflns_Laue_measured_fraction_max 0.9835
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28202
_diffrn_reflns_point_group_measured_fraction_full 0.9991
_diffrn_reflns_point_group_measured_fraction_max 0.9835
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         72.12
_diffrn_reflns_theta_min         4.00
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.206
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       needle
_exptl_crystal_F_000             2220.128
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.2325
_refine_diff_density_min         -1.3503
_refine_diff_density_rms         0.1617
_refine_ls_d_res_high            0.8100
_refine_ls_d_res_low             11.0529
_refine_ls_extinction_coef       0.00027(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0630
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    44
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0630
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          -0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0891P)^2^+13.1518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1338
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              26
_reflns_limit_h_min              -28
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                4145
_reflns_number_total             4603
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt02733g2.cif
_cod_data_source_block           MCR25_2
_cod_depositor_comments
'Adding full bibliography for 7717543--7717550.cif.'
_cod_database_code               7717544
_chemical_oxdiff_formula         C42H41N2O2PRuS2
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 Ternary CH refined with riding coordinates:
 C31(H31)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C12(H12), C13(H13), C22(H22), C18(H18), C27(H27), C19(H19),
 C26(H26), C29(H29), C14(H14), C30(H30), C21(H21), C15(H15)
2.c Idealised Me refined as rotating group:
 C33(H33a,H33b,H33c), C32(H32a,H32b,H32c), C24(H24a,H24b,H24c), C23(H23a,H23b,
 H23c)
;
_olex2_exptl_crystal_mounting_method 'paratone oil and nylon cryoloop'
_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 3.312
_oxdiff_exptl_absorpt_empirical_full_min 0.273