Diacylthioureas - an overlooked class of ligands; the coordination chemistry of diacylated thiourea with platinum(II), palladium(II) and gold(III).
Risi, Matthew C.; Atiga, Simeon; Christopher, Timothy D.; Henderson, William; Saunders, Graham C.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 4977–4989; doi:10.1039/d4dt03390f

data_7718106
_publ_section_title
;
 Diacylthioureas - an overlooked class of ligands; the coordination
 chemistry of diacylated thiourea with platinum(II), palladium(II) and
 gold(III).
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4977
_journal_page_last               4989
_journal_paper_doi               10.1039/d4dt03390f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C25 H26 Cl N2 O2 P Pd S'
_chemical_formula_sum            'C25 H26 Cl N2 O2 P Pd S'
_chemical_formula_weight         591.41
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-02-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-02-12 deposited with the CCDC.	2025-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                68.297(2)
_cell_angle_beta                 85.0358(17)
_cell_angle_gamma                81.1443(18)
_cell_formula_units_Z            2
_cell_length_a                   9.70784(19)
_cell_length_b                   10.9768(3)
_cell_length_c                   12.7313(3)
_cell_measurement_reflns_used    22163
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.0060
_cell_measurement_theta_min      3.7320
_cell_volume                     1244.82(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9653
_diffrn_measured_fraction_theta_max 0.9653
_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    -79.00   8.00   0.50    0.15    --  -46.98  94.00  80.00  174
  2  \w     -2.00  66.00   0.50    0.15    --   46.98 -94.00 -30.00  136
  3  \w    -72.00 -45.00   0.50    0.59    --  -90.25  94.00  80.00   54
  4  \w   -150.00-125.00   0.50    0.59    --  -90.25 -94.00 -30.00   50
  5  \w     63.00  99.00   0.50    0.59    --   97.33 -94.00 -30.00   72
  6  \w    105.00 175.00   0.50    0.59    --   97.33  94.00  80.00  140
  7  \w    -16.00   9.00   0.50    0.15    --   22.00 102.00  60.81   50
  8  \w     15.00  40.00   0.50    0.15    --   46.00  89.00  -6.13   50
  9  \w     14.00  39.00   0.50    0.15    --   46.00  89.00-124.93   50
 10  \w     14.00  39.00   0.50    0.15    --   46.00  89.00 108.45   50
 11  \w    -68.00 -26.00   0.50    0.15    --  -46.98 -57.00 -30.00   84
 12  \w   -119.00 -61.00   0.50    0.15    --  -46.98 -57.00  60.00  116
 13  \w    -53.00 -26.00   0.50    0.15    --  -46.98 -57.00  60.00   54
 14  \w   -120.00 -82.00   0.50    0.15    --  -46.98 -57.00 -30.00   76
 15  \w     83.00 124.00   0.50    0.15    --   46.98  38.00-180.00   82
 16  \w     85.00 114.00   0.50    0.15    --   46.98  38.00  60.00   58
 17  \w     28.00  72.00   0.50    0.15    --   46.98  38.00 -90.00   88
 18  \w     88.00 119.00   0.50    0.15    --   46.98  38.00 -90.00   62
 19  \w     28.00  75.00   0.50    0.15    --   46.98  38.00-180.00   94
 20  \w     28.00  75.00   0.50    0.15    --   46.98  38.00  60.00   94
 21  \w     17.00  42.00   0.50    0.15    --   50.00  90.00  53.64   50
 22  \w     17.00  42.00   0.50    0.15    --   50.00  90.00 -27.95   50
 23  \w     16.00  41.00   0.50    0.15    --   50.00  92.00 157.60   50
 24  \w     16.00  41.00   0.50    0.15    --   50.00  92.00-149.58   50
 25  \w     32.00  61.00   0.50    0.15    --   54.00  77.00  95.57   58
 26  \w     88.00 114.00   0.50    0.15    --   54.00  77.00  95.57   52
 27  \w     33.00  59.00   0.50    0.15    --   58.00  77.00 -79.38   52
 28  \w    -72.00 -35.00   0.50    0.15    --  -62.00 -77.00 118.81   74
 29  \w     36.00  62.00   0.50    0.15    --   62.00  74.00-155.31   52
 30  \w    -68.00 -42.00   0.50    0.15    --  -66.00 -73.00  10.02   52
 31  \w    -68.00 -42.00   0.50    0.15    --  -66.00 -74.00 -72.29   52
 32  \w    -65.00 -40.00   0.50    0.15    --  -66.00 -76.00  42.30   50
 33  \w   -145.00 -98.00   0.50    0.15    --  -70.00 -71.00 -97.98   94
 34  \w    -78.00 -46.00   0.50    0.15    --  -70.00 -72.00  61.31   64
 35  \w    -73.00 -47.00   0.50    0.15    --  -70.00 -70.00  90.82   52
 36  \w    -71.00 -45.00   0.50    0.15    --  -70.00 -71.00 -97.98   52
 37  \w    -72.00 -46.00   0.50    0.15    --  -70.00 -72.00  -9.98   52
 38  \w    -74.00 -48.00   0.50    0.15    --  -70.00 -69.00 -38.25   52
 39  \w    -71.00 -45.00   0.50    0.15    --  -70.00 -71.00-155.44   52
 40  \w    -69.00 -44.00   0.50    0.15    --  -70.00 -74.00 -44.90   50
 41  \w   -148.00-113.00   0.50    0.59    --  -74.00 -70.00-136.48   70
 42  \w    -80.00 -50.00   0.50    0.59    --  -74.00 -70.00-136.48   60
 43  \w    -82.00 -50.00   0.50    0.59    --  -74.00 -76.00 -94.71   64
 44  \w    -73.00 -47.00   0.50    0.59    --  -74.00 -76.00 165.01   52
 45  \w    -81.00 -55.00   0.50    0.59    --  -78.00 -66.00 173.09   52
 46  \w    -88.00 -55.00   0.50    0.59    --  -78.00 -75.00  50.82   66
 47  \w    -78.00 -52.00   0.50    0.59    --  -78.00 -74.00 139.42   52
 48  \w    -78.00 -53.00   0.50    0.59    --  -78.00 -71.00-157.91   50
 49  \w    -95.00 -55.00   0.50    0.59    --  -78.00 -70.00 -65.13   80
 50  \w    -84.00 -59.00   0.50    0.59    --  -82.00 -68.00  22.02   50
 51  \w   -140.00-114.00   0.50    0.59    --  -82.00 -68.00  22.02   52
 52  \w   -111.00 -55.00   0.50    0.59    --  -82.00 -77.00 128.82  112
 53  \w    -81.00 -56.00   0.50    0.59    --  -82.00 -77.00 149.03   50
 54  \w    -92.00 -60.00   0.50    0.59    --  -82.00 -68.00 177.04   64
 55  \w    -84.00 -56.00   0.50    0.59    --  -82.00 -75.00  98.44   56
 56  \w   -141.00-115.00   0.50    0.59    --  -82.00 -75.00  98.44   52
 57  \w    -96.00 -59.00   0.50    0.59    --  -86.00 -77.00  79.70   74
 58  \w   -161.00 -91.00   0.50    0.59    --  -90.25 -66.00  58.47  140
 59  \w   -163.00 -71.00   0.50    0.59    --  -90.25 -60.00 128.88  184
 60  \w   -154.00 -72.00   0.50    0.59    --  -90.25 -71.00-114.06  164
 61  \w   -108.00 -65.00   0.50    0.59    --  -90.25 -72.00 -88.08   86
 62  \w   -154.00-106.00   0.50    0.59    --  -90.25 -75.00-146.16   96
 63  \w   -136.00 -92.00   0.50    0.59    --  -90.25 -77.00-150.00   88
 64  \w   -144.00-117.00   0.50    0.59    --  -90.25 -72.00 -88.08   54
 65  \w   -118.00 -66.00   0.50    0.59    --  -90.25 -76.00 172.59  104
 66  \w   -118.00 -65.00   0.50    0.59    --  -90.25 -75.00 106.35  106
 67  \w    -89.00 -64.00   0.50    0.59    --  -90.25 -75.00-146.16   50
 68  \w   -165.00-140.00   0.50    0.59    --  -90.25 -77.00-150.00   50
 69  \w    -61.00 -25.00   0.50    0.59    --  -90.25  61.00  30.00   72
 70  \w   -148.00-122.00   0.50    0.59    --  -90.25 -76.00 172.59   52
 71  \w   -162.00-131.00   0.50    0.59    --  -90.25 -75.00 106.35   62
 72  \w    -98.00 -64.00   0.50    0.59    --  -90.25 -75.00-118.11   68
 73  \w   -163.00 -87.00   0.50    0.59    --  -90.25 -45.00 -60.00  152
 74  \w   -165.00 -64.00   0.50    0.59    --  -90.25 -77.00  30.00  202
 75  \w   -102.00 -65.00   0.50    0.59    --  -90.25 -75.00 -11.72   74
 76  \w   -159.00 -79.00   0.50    0.59    --  -90.25 -45.00  60.00  160
 77  \w   -126.00-101.00   0.50    0.59    --  -90.25 -75.00-118.11   50
 78  \w   -165.00 -64.00   0.50    0.59    --  -90.25 -76.00  10.91  202
 79  \w   -138.00 -64.00   0.50    0.59    --  -90.25 -77.00 -35.01  148
 80  \w    -88.00 -63.00   0.50    0.59    --  -90.25 -77.00-180.00   50
 81  \w    -88.00 -63.00   0.50    0.59    --  -90.25 -77.00-150.00   50
 82  \w   -142.00-102.00   0.50    0.59    --  -90.25 -77.00-180.00   80
 83  \w    -51.00 -25.00   0.50    0.59    --  -90.25  45.00 120.00   52
 84  \w   -111.00 -63.00   0.50    0.59    --  -90.25 -77.00 -90.00   96
 85  \w   -163.00-128.00   0.50    0.59    --  -90.25 -77.00 -90.00   70
 86  \w     26.00  51.00   0.50    0.59    --   97.33 -45.00-120.00   50
 87  \w     42.00 109.00   0.50    0.59    --   97.33-111.00 150.00  134
 88  \w     31.00 109.00   0.50    0.59    --   97.33-111.00 -30.00  156
 89  \w     46.00  71.00   0.50    0.59    --   97.33 -61.00 -60.00   50
 90  \w     66.00  92.00   0.50    0.59    --   97.33 178.00   0.00   52
 91  \w     69.00 100.00   0.50    0.59    --   97.33 -95.00-120.00   62
 92  \w     37.00  63.00   0.50    0.59    --   97.33 -95.00-120.00   52
 93  \w     26.00 106.00   0.50    0.59    --   97.33-111.00  60.00  160
 94  \w    117.00 146.00   0.50    0.59    --   97.33  77.00 -60.00   58
 95  \w     24.00 105.00   0.50    0.59    --   97.33 -95.00 150.00  162
 96  \w     31.00  70.00   0.50    0.59    --   97.33 -61.00   0.00   78
 97  \w     71.00 102.00   0.50    0.59    --   97.33  77.00 -60.00   62
 98  \w     71.00  97.00   0.50    0.59    --   97.33  77.00  60.00   52
 99  \w     35.00 109.00   0.50    0.59    --   97.33-111.00-120.00  148
100  \w     47.00 104.00   0.50    0.59    --   97.33-111.00  90.00  114
101  \w     26.00  65.00   0.50    0.59    --   97.33 -95.00-150.00   78
102  \w     20.00  46.00   0.50    0.59    --   97.33 -45.00  60.00   52
103  \w    102.00 128.00   0.50    0.59    --   97.33 178.00   0.00   52
104  \w     25.00  50.00   0.50    0.59    --   97.33 -45.00-150.00   50
;
_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      -0.0856125000
_diffrn_orient_matrix_UB_12      -0.0600533000
_diffrn_orient_matrix_UB_13      0.1100846000
_diffrn_orient_matrix_UB_21      0.0562113000
_diffrn_orient_matrix_UB_22      0.0891239000
_diffrn_orient_matrix_UB_23      0.0510527000
_diffrn_orient_matrix_UB_31      -0.1238236000
_diffrn_orient_matrix_UB_32      0.1080332000
_diffrn_orient_matrix_UB_33      -0.0474845000
_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  0.0675
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            33325
_diffrn_reflns_theta_full        72.1346
_diffrn_reflns_theta_max         72.13
_diffrn_reflns_theta_min         3.74
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.597
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.98a (Rigaku Oxford Diffraction, 2023)
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    1.5777
_exptl_crystal_description       irregular
_exptl_crystal_F_000             603.7182
_exptl_crystal_recrystallization_method DCM/Ether
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.4868
_refine_diff_density_min         -1.3957
_refine_diff_density_rms         0.1262
_refine_ls_d_res_high            0.8100
_refine_ls_d_res_low             11.8226
_refine_ls_goodness_of_fit_ref   1.0281
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    46
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0281
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+0.4496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0922
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              13
_reflns_limit_k_min              -12
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                4487
_reflns_number_total             4736
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt03390f2.cif
_cod_data_source_block           MCR105_auto
_cod_depositor_comments
'Adding full bibliography for 7718104--7718109.cif.'
_cod_original_cell_volume        1244.81(5)
_cod_database_code               7718106
_chemical_oxdiff_formula         C30H30N3O2PPdS
_diffrn_oxdiff_digest_frames
;
016313af684aba6b5909d246719d6375e300109b407
;
_diffrn_oxdiff_digest_hkl
;
0155f9fdc313068fa65bfeaf910415456e3b62
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2.a Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C6(H6a,H6b)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C23(H23), C32(H32), C22(H22), C35(H35), C25(H25), C14(H14),
 C15(H15), C36(H36), C16(H16), C13(H13), C26(H26), C24(H24), C33(H33), C34(H34),
  N2(H2)
2.c Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C7(H7a,H7b,H7c)
;
_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 1.556
_oxdiff_exptl_absorpt_empirical_full_min 0.665