Unconventional chalcogen-containing azolylidene metal complexes as potential anticancer therapeutics.
Romano-deGea, Jan; Sinenko, Irina L.; Pânzar, Peter M F; Neves Vieira, Adriana; Frederiksen, Lindsey E. K.; Glinkina, Kseniya; Fadaei-Tirani, Farzaneh; Scopelliti, Rosario; Kuttler, Fabien; Lau, Kelvin; Dyson, Paul J.; Chemical science 17 (2026) 4296–4306; doi:10.1039/d5sc05555e

data_1576704
_publ_section_title
;
 Unconventional chalcogen-containing azolylidene metal complexes as
 potential anticancer therapeutics.
;
_journal_issue                   8
_journal_name_full               'Chemical science'
_journal_page_first              4296
_journal_page_last               4306
_journal_paper_doi               10.1039/d5sc05555e
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         'C31 H32 Cl2 N2 Ru, C H2 Cl2'
_chemical_formula_sum            'C32 H34 Cl4 N2 Ru'
_chemical_formula_weight         689.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-11-02
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2023-06-16 deposited with the CCDC.	2025-12-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.216(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0757(5)
_cell_length_b                   12.3164(2)
_cell_length_c                   18.0889(7)
_cell_measurement_reflns_used    15416
_cell_measurement_temperature    139.99(10)
_cell_measurement_theta_max      71.1510
_cell_measurement_theta_min      3.1750
_cell_volume                     3063.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      139.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.968
_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     24.00  96.00   0.50    7.00    --   59.56-136.00  88.00  144
  2  \w     22.00  95.00   0.50    7.00    --   59.56-133.00 -93.00  146
  3  \w    -99.00 -20.00   0.50    7.00    --  -62.07 136.00 152.00  158
  4  \w    -97.00 -18.00   0.50    7.00    --  -62.07 133.00 -25.00  158
  5  \w   -115.00 -67.00   0.50    7.00    --  -71.26-136.00  88.00   96
  6  \w   -106.00 -26.00   0.50    7.00    --  -71.26 133.00 -25.00  160
  7  \w   -116.00 -69.00   0.50    7.00    --  -71.26-133.00 -93.00   94
  8  \w     28.00 109.00   0.50    7.00    --   71.88-136.00  88.00  162
  9  \w     29.00 108.00   0.50    7.00    --   73.45-133.00 -93.00  158
 10  \w     71.00 118.00   0.50    7.00    --   73.45 136.00 152.00   94
 11  \w   -113.00 -32.00   0.50    7.00    --  -75.95 136.00 152.00  162
 12  \w   -102.00 -70.00   0.50    7.00    --  -75.95 133.00 -25.00   64
 13  \w   -119.00 -94.00   0.50    7.00    --  -75.95-133.00 -93.00   50
 14  \w   -119.00 -89.00   0.50    7.00    --  -75.95-136.00  88.00   60
 15  \w     52.00  77.00   0.50    7.00    --   81.22-133.00 -93.00   50
 16  \w     74.00  99.00   0.50    7.00    --   81.22 136.00 152.00   50
 17  \w     38.00 118.00   0.50    7.00    --   81.22-136.00  88.00  160
 18  \w     79.00 104.00   0.50    7.00    --   81.22 133.00 -25.00   50
 19  \w     52.00  81.00   0.50    7.00    --   40.00  64.00 135.95   58
 20  \w     55.00  91.00   0.50    7.00    --   52.00  74.00-115.72   72
 21  \w     61.00  90.00   0.50    7.00    --   56.00  72.00 -61.66   58
 22  \w    -93.00 -59.00   0.50    7.00    --  -56.00 -74.00 168.56   68
 23  \w     10.00  36.00   0.50    7.00    --   59.56 -30.00  30.00   52
 24  \w     73.00 103.00   0.50    7.00    --   64.00  73.00 -18.13   60
 25  \w   -108.00 -74.00   0.50    7.00    --  -64.00 -58.00 -72.90   68
 26  \w   -103.00 -71.00   0.50    7.00    --  -64.00 -58.00 -30.42   64
 27  \w     32.00  82.00   0.50    7.00    --   71.88 -95.00  90.00  100
 28  \w   -115.00 -80.00   0.50    7.00    --  -72.00 -63.00 140.44   70
 29  \w   -105.00 -75.00   0.50    7.00    --  -72.00 -74.00 -36.83   60
 30  \w     35.00  83.00   0.50    7.00    --   73.45 -95.00 -60.00   96
 31  \w     34.00  82.00   0.50    7.00    --   73.45 -95.00 150.00   96
 32  \w   -117.00 -87.00   0.50    7.00    --  -75.95-125.00   0.00   60
 33  \w   -120.00 -88.00   0.50    7.00    --  -75.95-125.00  30.00   64
 34  \w   -118.00 -83.00   0.50    7.00    --  -76.55 -64.00-101.53   70
 35  \w   -121.00 -86.00   0.50    7.00    --  -76.55 -55.00-173.73   70
 36  \w   -110.00 -84.00   0.50    7.00    --  -76.55 -62.00  -2.21   52
 37  \w   -122.00 -86.00   0.50    7.00    --  -76.55 -48.00-132.36   72
 38  \w   -120.00 -85.00   0.50    7.00    --  -76.55 -48.00  92.65   70
 39  \w     36.00 112.00   0.50    7.00    --   81.22-125.00 -90.00  152
 40  \w     40.00 112.00   0.50    7.00    --   81.22-125.00-150.00  144
 41  \w     79.00 112.00   0.50    7.00    --   81.22-125.00-180.00   66
 42  \w     85.00 112.00   0.50    7.00    --   81.22-125.00   0.00   54
 43  \w     42.00  68.00   0.50    7.00    --   81.22-125.00   0.00   52
 44  \w     80.00 126.00   0.50    7.00    --   81.22 125.00-180.00   92
 45  \w     82.00 126.00   0.50    7.00    --   81.22 125.00  30.00   88
 46  \w     82.00 108.00   0.50    7.00    --   81.22 125.00-120.00   52
 47  \w     81.00 127.00   0.50    7.00    --   81.22 125.00 120.00   92
 48  \w     57.00 112.00   0.50    7.00    --   81.22-125.00 -30.00  110
 49  \w     44.00  92.00   0.50    7.00    --   81.22 -95.00 -30.00   96
 50  \w     87.00 112.00   0.50    7.00    --   81.22-125.00 120.00   50
 51  \w     35.00  75.00   0.50    7.00    --   81.22-125.00 120.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0645776000
_diffrn_orient_matrix_UB_12      -0.0027711000
_diffrn_orient_matrix_UB_13      -0.0475227000
_diffrn_orient_matrix_UB_21      0.0915365000
_diffrn_orient_matrix_UB_22      0.0004802000
_diffrn_orient_matrix_UB_23      0.0804093000
_diffrn_orient_matrix_UB_31      -0.0012068000
_diffrn_orient_matrix_UB_32      -0.1250150000
_diffrn_orient_matrix_UB_33      0.0013836000
_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  0.1118
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            57987
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.607
_diffrn_reflns_theta_min         3.232
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.535
_exptl_absorpt_correction_T_max  0.770
_exptl_absorpt_correction_T_min  0.357
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.495
_exptl_crystal_description       needle
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.281
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.048
_refine_diff_density_max         2.240
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         6163
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0673
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0911P)^2^+15.0500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1694
_refine_ls_wR_factor_ref         0.1899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4515
_reflns_number_total             6163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05555e2.cif
_cod_data_source_block           pp41
_cod_depositor_comments
'Adding full bibliography for 1576700--1576709.cif.'
_cod_database_code               1576704
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C32 H34 N2 Cl4 Ru1'
_shelx_estimated_absorpt_t_max   0.714
_shelx_estimated_absorpt_t_min   0.226
_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.a Ternary CH refined with riding coordinates:
 C29(H29)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C15(H15A,H15B), C32(H32A,H32B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C13(H13),
 C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24),
  C26(H26), C27(H27)
2.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              43167
_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 2.015
_oxdiff_exptl_absorpt_empirical_full_min 0.247