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_7717545
_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         'C32 H29 N2 O2 P Ru S2, C H2 Cl2'
_chemical_formula_sum            'C33 H31 Cl2 N2 O2 P Ru S2'
_chemical_formula_weight         754.702
_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             2024-10-25
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-10-25 deposited with the CCDC.	2024-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.1698(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.34223(8)
_cell_length_b                   20.4172(3)
_cell_length_c                   18.7826(2)
_cell_measurement_reflns_used    14693
_cell_measurement_temperature    99.9(5)
_cell_measurement_theta_max      73.8250
_cell_measurement_theta_min      4.3140
_cell_volume                     3166.68(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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                 'CCD plate'
_diffrn_detector_area_resol_mean 10.7110
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.9877
_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      4.00  81.00   1.00    6.41    --   40.55-125.00-120.00   77
  2  \w     17.00 109.00   1.00    6.41    --   40.55  77.00 -60.00   92
  3  \w    128.00 158.00   1.00   25.63    --  106.89  30.00  60.00   30
  4  \w     38.00 133.00   1.00   25.63    --  106.89 -30.00  90.00   95
  5  \w    110.00 152.00   1.00   25.63    --  106.89  77.00 150.00   42
  6  \w     76.00 156.00   1.00   25.63    --  106.89 125.00  60.00   80
  7  \w     37.00 136.00   1.00   25.63    --  106.89 -77.00   0.00   99
  8  \w     87.00 121.00   1.00   25.63    --  106.89  30.00  60.00   34
  9  \w      8.00 117.00   1.00    6.41    --   40.55  77.00 150.00  109
 10  \w     12.00 114.00   1.00    6.41    --   40.55  57.00  60.00  102
 11  \w     81.00 158.00   1.00   25.63    --  106.89  45.00-120.00   77
 12  \w     74.00 158.00   1.00   25.63    --  106.89  77.00 120.00   84
 13  \w     34.00 121.00   1.00   25.63    --  106.89-125.00 -60.00   87
 14  \w     79.00 158.00   1.00   25.63    --  106.89  30.00 -30.00   79
 15  \w    -32.00  69.00   1.00    6.41    --   40.55 -57.00  30.00  101
 16  \w    -32.00  69.00   1.00    6.41    --   40.55 -57.00 -90.00  101
 17  \w     74.00 158.00   1.00   25.63    --  106.89  77.00-180.00   84
 18  \w     78.00 158.00   1.00   25.63    --  106.89  61.00 -90.00   80
 19  \w     81.00 158.00   1.00   25.63    --  106.89  45.00  90.00   77
 20  \w     79.00 158.00   1.00   25.63    --  106.89  30.00  30.00   79
 21  \w      8.00  33.00   1.00    6.41    --   40.55  77.00-120.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0814429000
_diffrn_orient_matrix_UB_12      0.0484580000
_diffrn_orient_matrix_UB_13      0.0568204000
_diffrn_orient_matrix_UB_21      0.1524926000
_diffrn_orient_matrix_UB_22      0.0007222000
_diffrn_orient_matrix_UB_23      -0.0376358000
_diffrn_orient_matrix_UB_31      -0.0700911000
_diffrn_orient_matrix_UB_32      0.0578917000
_diffrn_orient_matrix_UB_33      -0.0470402000
_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  0.0604
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.9991
_diffrn_reflns_Laue_measured_fraction_max 0.9877
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29462
_diffrn_reflns_point_group_measured_fraction_full 0.9991
_diffrn_reflns_point_group_measured_fraction_max 0.9877
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         73.88
_diffrn_reflns_theta_min         4.33
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.547
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.583
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1547.055
_exptl_crystal_size_max          0.079
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.018
_refine_diff_density_max         0.8605
_refine_diff_density_min         -0.9816
_refine_diff_density_rms         0.1482
_refine_ls_d_res_high            0.8025
_refine_ls_d_res_low             10.2086
_refine_ls_goodness_of_fit_ref   1.0540
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    64
_refine_ls_number_parameters     395
_refine_ls_number_reflns         6346
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.0539
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+2.8337P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0905
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                5520
_reflns_number_total             6346
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt02733g2.cif
_cod_data_source_block           Crystal319-Copy
_cod_depositor_comments
'Adding full bibliography for 7717543--7717550.cif.'
_cod_original_cell_volume        3166.68(6)
_cod_database_code               7717545
_chemical_oxdiff_formula         C43H37N2S2RuPO2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl3S-C2S
 1.77 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N2) = Uanis(C1)
Uanis(C2S) = Uanis(C1S)
Ueq(N2), Ueq(C1): fixed at 0.05 with sigma of 0.1
4. Others
 Fixed Sof: C2S(0.25) H2Sa(0.25) H2Sb(0.25) C1S(0.75) H1Sa(0.75) H1Sb(0.75)
 Cl2S(0.75) Cl3S(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C2S(H2Sa,H2Sb), C1S(H1Sa,H1Sb)
5.b Aromatic/amide H refined with riding coordinates:
 C46(H46), C42(H42), C26(H26), C32(H32), C36(H36), C15(H15), C23(H23), C5(H5),
 C22(H22), C4(H4), C35(H35), C3(H3), C34(H34), C24(H24), C13(H13), C43(H43),
 C44(H44), C45(H45), C12(H12), C33(H33), C25(H25), C7(H7), C16(H16), C6(H6),
 C11(H11), C14(H14)
5.c Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c)
;
_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 8.377
_oxdiff_exptl_absorpt_empirical_full_min 0.258