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_7717549
_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         'C30 H40 Cl N5 O2 P Rh S2, 0.5(H2 O)'
_chemical_formula_sum            'C30 H41 Cl N5 O2.5 P Rh S2'
_chemical_formula_weight         745.156
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_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                 108.467(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.0707(3)
_cell_length_b                   8.9830(1)
_cell_length_c                   33.0254(3)
_cell_measurement_reflns_used    39564
_cell_measurement_temperature    99.9(5)
_cell_measurement_theta_max      74.1290
_cell_measurement_theta_min      2.8030
_cell_volume                     6491.88(13)
_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      99.9(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9996
_diffrn_measured_fraction_theta_max 0.9866
_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    -27.00  34.00   0.50    0.50    --  -47.23  19.00 -90.00  122
  2  \w    -38.00  31.00   0.50    0.50    --  -47.23  38.00 -30.00  138
  3  \w     -7.00  19.00   0.50    0.50    --  -47.23  38.00  90.00   52
  4  \w    -48.00 -13.00   0.50    1.00    --  -90.25  45.00 150.00   70
  5  \w    -51.00 -15.00   0.50    1.00    --  -90.25  45.00  90.00   72
  6  \w    -51.00 -19.00   0.50    1.00    --  -90.25  45.00  30.00   64
  7  \w    -50.00 -15.00   0.50    1.00    --  -90.25  45.00  60.00   70
  8  \w    -51.00 -12.00   0.50    1.00    --  -90.25  45.00 120.00   78
  9  \w    -43.00 -13.00   0.50    1.00    --  -90.25 111.00 120.00   60
 10  \w    -86.00 -61.00   0.50    0.50    --  -47.23 144.00 144.00   50
 11  \w    -75.00 -50.00   0.50    0.50    --  -47.23 127.00 -24.00   50
 12  \w    -51.00 -18.00   0.50    1.00    --  -90.25  45.00-150.00   66
 13  \w   -113.00 -27.00   0.50    0.50    --  -47.23 -57.00  30.00  172
 14  \w   -101.00 -75.00   0.50    1.00    --  -90.25 -45.00 150.00   52
 15  \w   -122.00 -74.00   0.50    0.50    --  -47.23-125.00  60.00   96
 16  \w   -111.00 -67.00   0.50    0.50    --  -47.23-144.00  90.00   88
 17  \w   -113.00 -60.00   0.50    1.00    --  -90.25-144.00  90.00  106
 18  \w   -114.00 -78.00   0.50    0.50    --  -47.23-127.00-100.00   72
 19  \w    -26.00  65.00   0.50    0.50    --   47.23 -57.00  90.00  182
 20  \w     61.00 108.00   0.50    1.00    --  100.91-111.00  60.00   94
 21  \w     94.00 122.00   0.50    1.00    --  100.91-144.00  90.00   56
 22  \w     82.00 108.00   0.50    1.00    --  100.91-111.00   0.00   52
 23  \w     73.00 105.00   0.50    1.00    --  100.91-111.00 -30.00   64
 24  \w     75.00 104.00   0.50    1.00    --  100.91 -95.00 -30.00   58
 25  \w     71.00 105.00   0.50    1.00    --  100.91 -77.00 -60.00   68
 26  \w     55.00  82.00   0.50    0.50    --   47.23-127.00-100.00   54
 27  \w     50.00  75.00   0.50    1.00    --  100.91-127.00-100.00   50
 28  \w     49.00  75.00   0.50    1.00    --  100.91 -77.00-120.00   52
 29  \w     38.00  64.00   0.50    1.00    --  100.91 -77.00 -60.00   52
 30  \w     23.00 106.00   0.50    1.00    --  100.91-111.00 -90.00  166
 31  \w     39.00  71.00   0.50    1.00    --  100.91 -61.00  30.00   64
 32  \w     29.00  71.00   0.50    1.00    --  100.91 -61.00   0.00   84
 33  \w     28.00  67.00   0.50    1.00    --  100.91 -61.00 -60.00   78
 34  \w     24.00  51.00   0.50    1.00    --  100.91 -45.00  30.00   54
 35  \w     23.00  48.00   0.50    1.00    --  100.91 -45.00  90.00   50
 36  \w     33.00  58.00   0.50    1.00    --  100.91 -77.00 150.00   50
 37  \w     60.00 106.00   0.50    1.00    --  100.91-111.00 150.00   92
 38  \w     58.00  83.00   0.50    0.50    --   47.23-144.00  90.00   50
 39  \w     26.00 104.00   0.50    1.00    --  100.91 -95.00 120.00  156
 40  \w     23.00  49.00   0.50    1.00    --  100.91-111.00  60.00   52
 41  \w     32.00 108.00   0.50    1.00    --  100.91-111.00 120.00  152
 42  \w     22.00  64.00   0.50    1.00    --  100.91 -95.00 -30.00   84
 43  \w     27.00  64.00   0.50    0.50    --   47.23 -57.00-150.00   74
 44  \w     25.00 101.00   0.50    1.00    --  100.91 -95.00-180.00  152
 45  \w     35.00 107.00   0.50    1.00    --  100.91-111.00-150.00  144
 46  \w     80.00 177.00   0.50    1.00    --  100.91  45.00  90.00  194
 47  \w    101.00 126.00   0.50    1.00    --  100.91 144.00 144.00   50
 48  \w    104.00 145.00   0.50    1.00    --  100.91 111.00 120.00   82
 49  \w    102.00 175.00   0.50    1.00    --  100.91 111.00  30.00  146
 50  \w    121.00 146.00   0.50    1.00    --  100.91 178.00   0.00   50
 51  \w    103.00 164.00   0.50    1.00    --  100.91 127.00 -24.00  122
 52  \w    104.00 132.00   0.50    1.00    --  100.91 111.00-180.00   56
 53  \w    108.00 137.00   0.50    1.00    --  100.91 178.00-180.00   58
 54  \w     62.00  87.00   0.50    1.00    --  100.91 178.00-180.00   50
 55  \w     64.00  98.00   0.50    1.00    --  100.91 178.00   0.00   68
 56  \w     78.00 146.00   0.50    1.00    --  100.91 178.00  30.00  136
 57  \w     23.00  48.00   0.50    1.00    --  100.91 -45.00 120.00   50
 58  \w   -143.00-118.00   0.50    1.00    --  -90.25-127.00-100.00   50
 59  \w   -155.00-129.00   0.50    1.00    --  -90.25-144.00  90.00   52
;
_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      0.0621223000
_diffrn_orient_matrix_UB_12      -0.0781301000
_diffrn_orient_matrix_UB_13      0.0082450000
_diffrn_orient_matrix_UB_21      0.0310924000
_diffrn_orient_matrix_UB_22      0.1523237000
_diffrn_orient_matrix_UB_23      0.0009753000
_diffrn_orient_matrix_UB_31      0.0114693000
_diffrn_orient_matrix_UB_32      0.0101363000
_diffrn_orient_matrix_UB_33      0.0484782000
_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  0.0661
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.9996
_diffrn_reflns_Laue_measured_fraction_max 0.9866
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            102852
_diffrn_reflns_point_group_measured_fraction_full 0.9996
_diffrn_reflns_point_group_measured_fraction_max 0.9866
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         74.35
_diffrn_reflns_theta_min         2.82
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.988
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77476
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       needle
_exptl_crystal_F_000             3100.151
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.2837
_refine_diff_density_min         -0.7796
_refine_diff_density_rms         0.0935
_refine_ls_d_res_high            0.8006
_refine_ls_d_res_low             15.6624
_refine_ls_goodness_of_fit_ref   1.0148
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    125
_refine_ls_number_parameters     787
_refine_ls_number_reflns         13075
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.0146
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+6.2315P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0674
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              27
_reflns_limit_h_min              -28
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              40
_reflns_limit_l_min              0
_reflns_number_gt                11249
_reflns_number_total             13075
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt02733g2.cif
_cod_data_source_block           MCR_14
_cod_depositor_comments
'Adding full bibliography for 7717543--7717550.cif.'
_cod_database_code               7717549
_chemical_oxdiff_formula         C30H55N5O2PRhS2
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O0aa-H0ac = O0aa-H0ad
 0.85 with sigma of 0.02
 H0ac-H0ad
 1.34 with sigma of 0.04
3.a Secondary CH2 refined with riding coordinates:
 C43a(H43a,H43b), C41a(H41a,H41b), C49(H49a,H49b), C45a(H45a,H45b), C41(H41c,
 H41d), C42(H42a,H42b), C43(H43c,H43d), C0aa(H0aa,H0ab), C44(H44c,H44d),
 C44a(H44a,H44b), C45(H45c,H45d), C46(H46a,H46b)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C26(H26), C22(H22), C23(H23), C26a(H26a), C25(H25), C16a(H16a),
 C22a(H22a), C25a(H25a), C12a(H12a), C23a(H23a), C12(H12), C13(H13), C16(H16),
 C15a(H15a), C14(H14), C14a(H14a), C13a(H13a), C15(H15)
3.c Idealised Me refined as rotating group:
 C36a(H36a,H36b,H36c), C27(H27d,H27e,H27f), C27a(H27a,H27b,H27c), C40a(H40a,
 H40b,H40c), C36(H36d,H36e,H36f), C39(H39d,H39e,H39f), C38(H38d,H38e,H38f),
 C40(H40d,H40e,H40f), C37a(H37a,H37b,H37c), C37(H37d,H37e,H37f), C39a(H39a,H39b,
 H39c), C38a(H38a,H38b,H38c)
;
_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 1.500
_oxdiff_exptl_absorpt_empirical_full_min 0.699