A revised understanding of the speciation of gold(III) dithiocarbamate complexes in solution.
Brown, Ryan K.; Bunyan, Joseph N.; Agrawal, Ashi; Li, Guoyu; Dautoras, Dominykas; Sarker, Jagodish C.; Keat, Terng Tor; Hicks, Thomas; Hogarth, Graeme; Pugh, David; Dalton transactions (Cambridge, England : 2003) 54 (2025) 7627–7640; doi:10.1039/d5dt00240k

data_7718363
_publ_section_title
;
 A revised understanding of the speciation of gold(III) dithiocarbamate
 complexes in solution.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7627
_journal_page_last               7640
_journal_paper_doi               10.1039/d5dt00240k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C30 H28 Au N2 S4, Au Cl2, C H2 Cl2'
_chemical_formula_sum            'C31 H30 Au2 Cl4 N2 S4'
_chemical_formula_weight         1094.54
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-03-06
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-03-07 deposited with the CCDC.	2025-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                100.096(2)
_cell_angle_beta                 92.0640(10)
_cell_angle_gamma                96.601(2)
_cell_formula_units_Z            2
_cell_length_a                   9.42310(10)
_cell_length_b                   13.6971(3)
_cell_length_c                   14.0103(3)
_cell_measurement_reflns_used    27976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.7240
_cell_measurement_theta_min      1.4910
_cell_volume                     1765.58(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     -4.00 106.00   0.50    0.50    --   23.85  37.00  17.00  220
  2  \w    -60.00  20.00   0.50    0.50    --   23.85 -37.00-138.00  160
  3  \w   -108.00   4.00   0.50    0.50    --  -24.16 -37.00-138.00  224
  4  \w    -14.00  58.00   0.50    0.50    --  -24.16  37.00  17.00  144
  5  \w     22.00 106.00   0.50    0.50    --   23.85  19.00 120.00  168
  6  \w    -11.00  19.00   0.50    0.50    --   23.85  82.00   8.27   60
  7  \w    -64.00 -16.00   0.50    0.50    --   23.85 -19.00 -60.00   96
  8  \w    -17.00  10.00   0.50    0.50    --   23.85  94.00-142.15   54
  9  \w    -18.00  57.00   0.50    0.50    --   23.85 -77.00 -60.00  150
 10  \w    -18.00  57.00   0.50    0.50    --   23.85 -77.00-150.00  150
 11  \w      0.00  67.00   0.50    0.50    --   23.85 -99.00 150.00  134
 12  \w    -56.00   3.00   0.50    0.50    --  -24.16 -57.00 -30.00  118
 13  \w     22.00  58.00   0.50    0.50    --  -24.16  19.00  90.00   72
 14  \w     22.00  58.00   0.50    0.50    --  -24.16  19.00 120.00   72
 15  \w     22.00  58.00   0.50    0.50    --  -24.16  19.00-180.00   72
 16  \w    -56.00   3.00   0.50    0.50    --  -24.16 -57.00 120.00  118
 17  \w    -56.00   3.00   0.50    0.50    --  -24.16 -57.00-180.00  118
 18  \w     22.00  58.00   0.50    0.50    --  -24.16  19.00 150.00   72
 19  \w    -57.00  24.00   0.50    0.50    --  -24.16  77.00  30.00  162
 20  \w    -56.00   3.00   0.50    0.50    --  -24.16 -57.00  60.00  118
 21  \w    -21.00   5.00   0.50    0.50    --   23.85 101.00 127.53   52
 22  \w    -19.00   7.00   0.50    0.50    --   23.85  98.00-117.44   52
 23  \w    -18.00   8.00   0.50    0.50    --   23.85  96.00  83.55   52
 24  \w      0.00  67.00   0.50    0.50    --   23.85 -99.00 -60.00  134
 25  \w    -64.00 -16.00   0.50    0.50    --   23.85 -19.00  30.00   96
 26  \w    -20.00   6.00   0.50    0.50    --   23.85 100.00 175.04   52
 27  \w   -107.00   4.00   0.50    0.50    --  -24.16 -38.00-180.00  222
 28  \w   -108.00   4.00   0.50    0.50    --  -24.16 -37.00-138.00  224
 29  \w    -57.00  24.00   0.50    0.50    --  -24.16  77.00 -30.00  162
 30  \w    -85.00 -14.00   0.50    0.50    --  -24.16 131.00-120.71  142
 31  \w     22.00  58.00   0.50    0.50    --  -24.16  19.00 -30.00   72
 32  \w   -108.00   4.00   0.50    0.50    --  -24.16 -37.00-138.00  224
 33  \w   -107.00   4.00   0.50    0.50    --  -24.16 -38.00-120.00  222
 34  \w   -107.00   4.00   0.50    0.50    --  -24.16 -38.00-150.00  222
 35  \w     22.00  58.00   0.50    0.50    --  -24.16  19.00 -60.00   72
 36  \w    -83.00 -12.00   0.50    0.50    --  -24.16 128.00  33.70  142
 37  \w     -4.00 106.00   0.50    0.50    --   23.85  38.00-180.00  220
 38  \w     -4.00 106.00   0.50    0.50    --   23.85  38.00 -90.00  220
 39  \w     -4.00 106.00   0.50    0.50    --   23.85  38.00-120.00  220
 40  \w     -4.00 106.00   0.50    0.50    --   23.85  38.00-150.00  220
 41  \w     -4.00 106.00   0.50    0.50    --   23.85  37.00  17.00  220
 42  \w     -4.00 106.00   0.50    0.50    --   23.85  37.00  17.00  220
 43  \w     -4.00 106.00   0.50    0.50    --   23.85  38.00 -60.00  220
 44  \w   -107.00   4.00   0.50    0.50    --  -24.16 -38.00  90.00  222
 45  \w   -107.00   4.00   0.50    0.50    --  -24.16 -38.00  60.00  222
 46  \w   -107.00   4.00   0.50    0.50    --  -24.16 -38.00 -30.00  222
 47  \w   -107.00   4.00   0.50    0.50    --  -24.16 -38.00  30.00  222
 48  \w   -107.00   4.00   0.50    0.50    --  -24.16 -38.00 150.00  222
 49  \w   -107.00   4.00   0.50    0.50    --  -24.16 -38.00 120.00  222
 50  \w   -107.00   4.00   0.50    0.50    --  -24.16 -38.00   0.00  222
 51  \w   -107.00   4.00   0.50    0.50    --  -24.16 -38.00 -60.00  222
 52  \w   -107.00   4.00   0.50    0.50    --  -24.16 -38.00 -90.00  222
 53  \w     -4.00 106.00   0.50    0.50    --   23.85  38.00   0.00  220
 54  \w     -4.00 106.00   0.50    0.50    --   23.85  38.00  30.00  220
 55  \w     -4.00 106.00   0.50    0.50    --   23.85  38.00  60.00  220
 56  \w     -4.00 106.00   0.50    0.50    --   23.85  38.00  90.00  220
 57  \w     -4.00 106.00   0.50    0.50    --   23.85  38.00 120.00  220
 58  \w     -4.00 106.00   0.50    0.50    --   23.85  38.00 150.00  220
 59  \w    -53.00  41.00   0.50    0.50    --   23.85 -57.00-180.00  188
 60  \w     -4.00 106.00   0.50    0.50    --   23.85  38.00 -30.00  220
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0727906000
_diffrn_orient_matrix_UB_12      0.0042168000
_diffrn_orient_matrix_UB_13      -0.0117205000
_diffrn_orient_matrix_UB_21      0.0081883000
_diffrn_orient_matrix_UB_22      0.0515195000
_diffrn_orient_matrix_UB_23      0.0209067000
_diffrn_orient_matrix_UB_31      0.0198819000
_diffrn_orient_matrix_UB_32      -0.0117172000
_diffrn_orient_matrix_UB_33      0.0455921000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            141649
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.958
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.864
_exptl_absorpt_correction_T_max  0.758
_exptl_absorpt_correction_T_min  0.110
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.059
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.357
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.038
_refine_diff_density_max         3.734
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         6227
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0191
_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^)+(0.0198P)^2^+5.5388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0461
_refine_ls_wR_factor_ref         0.0466
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5958
_reflns_number_total             6227
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00240k2.cif
_cod_data_source_block           '[Au(p-tolyl2dtc)2][AuCl2]'
_cod_depositor_comments
'Adding full bibliography for 7718352--7718363.cif.'
_cod_database_code               7718363
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Au C H2 Cl2 Cl2 Au S2 N2 C30 H28'
_chemical_oxdiff_usercomment     'yellow rod JCS_100'
_shelx_estimated_absorpt_t_max   0.729
_shelx_estimated_absorpt_t_min   0.144
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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 Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C10(H10), C11(H11), C13(H13), C14(H14),
 C18(H18), C19(H19), C21(H21), C22(H22), C25(H25), C26(H26), C28(H28), C29(H29)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              23257
_shelx_hkl_checksum              78605
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.435
_oxdiff_exptl_absorpt_empirical_full_min 0.319