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_7718362
_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         'C18 H36 Au N2 S4, Au Cl2'
_chemical_formula_sum            'C18 H36 Au2 Cl2 N2 S4'
_chemical_formula_weight         873.56
_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             2025-02-28
_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                76.596(2)
_cell_angle_beta                 77.724(2)
_cell_angle_gamma                84.299(2)
_cell_formula_units_Z            2
_cell_length_a                   8.1079(2)
_cell_length_b                   13.3585(2)
_cell_length_c                   13.5963(3)
_cell_measurement_reflns_used    11522
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.5480
_cell_measurement_theta_min      1.5590
_cell_volume                     1397.80(5)
_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 1.000
_diffrn_measured_fraction_theta_max 0.919
_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     -8.00 103.00   0.50    0.15    --   20.24  40.00  50.00  222
  2  \w     -8.00 103.00   0.50    0.15    --   20.24  40.00  50.00  222
  3  \w     -8.00 103.00   0.50    0.15    --   20.24  40.00  50.00  222
  4  \w     22.00 103.00   0.50    0.15    --   20.24  19.00 -90.00  162
  5  \w     -8.00  69.00   0.50    0.15    --   20.24  38.00-150.00  154
  6  \w     -8.00 103.00   0.50    0.15    --   20.24  38.00-180.00  222
  7  \w    -62.00  25.00   0.50    0.15    --   20.24 -40.00-103.00  174
  8  \w      0.00  64.00   0.50    0.15    --   20.24 -99.00-120.00  128
  9  \w      0.00  64.00   0.50    0.15    --   20.24 -99.00   0.00  128
 10  \w    -18.00  53.00   0.50    0.15    --   20.24 -77.00  30.00  142
 11  \w      0.00  64.00   0.50    0.15    --   20.24 -99.00  90.00  128
 12  \w      0.00  64.00   0.50    0.15    --   20.24 -99.00 150.00  128
 13  \w   -109.00 -16.00   0.50    0.15    --  -20.71 -19.00  90.00  186
 14  \w    -56.00   7.00   0.50    0.15    --  -20.71 -57.00  90.00  126
 15  \w    -56.00   7.00   0.50    0.15    --  -20.71 -57.00  60.00  126
 16  \w   -103.00   7.00   0.50    0.15    --  -20.71 -40.00-103.00  220
 17  \w    -56.00   7.00   0.50    0.15    --  -20.71 -57.00-180.00  126
 18  \w    -65.00   5.00   0.50    0.15    --  -20.71 101.00-107.24  140
 19  \w    -71.00  -1.00   0.50    0.15    --  -20.71 110.00 168.14  140
 20  \w    -19.00  62.00   0.50    0.15    --  -20.71  40.00  50.00  162
 21  \w     22.00  62.00   0.50    0.15    --  -20.71  19.00 120.00   80
 22  \w     22.00  62.00   0.50    0.15    --  -20.71  19.00 150.00   80
 23  \w    -16.00  62.00   0.50    0.15    --  -20.71  38.00 150.00  156
 24  \w    -16.00  62.00   0.50    0.15    --  -20.71  38.00   0.00  156
 25  \w     22.00  62.00   0.50    0.15    --  -20.71  19.00  30.00   80
 26  \w     22.00  62.00   0.50    0.15    --  -20.71  19.00  90.00   80
 27  \w     22.00  62.00   0.50    0.15    --  -20.71  19.00 -90.00   80
 28  \w     22.00  62.00   0.50    0.15    --  -20.71  19.00-120.00   80
 29  \w     22.00  62.00   0.50    0.15    --  -20.71  19.00-150.00   80
 30  \w     22.00  62.00   0.50    0.15    --  -20.71  19.00-180.00   80
 31  \w    -41.00 -15.00   0.50    0.15    --   20.24 132.00  56.21   52
 32  \w    -37.00 -10.00   0.50    0.15    --   20.24 125.00 117.14   54
 33  \w    -39.00 -12.00   0.50    0.15    --   20.24 128.00 176.00   54
 34  \w    -34.00  -6.00   0.50    0.15    --   20.24 118.00 127.21   56
 35  \w    -27.00   2.00   0.50    0.15    --   20.24 106.00  97.39   58
 36  \w    -27.00   2.00   0.50    0.15    --   20.24 106.00-127.69   58
 37  \w    -25.00   4.00   0.50    0.15    --   20.24 102.00-166.32   58
;
_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      -0.0674565000
_diffrn_orient_matrix_UB_12      0.0248574000
_diffrn_orient_matrix_UB_13      -0.0237632000
_diffrn_orient_matrix_UB_21      0.0423794000
_diffrn_orient_matrix_UB_22      -0.0122457000
_diffrn_orient_matrix_UB_23      -0.0473638000
_diffrn_orient_matrix_UB_31      -0.0411283000
_diffrn_orient_matrix_UB_32      -0.0471152000
_diffrn_orient_matrix_UB_33      0.0135213000
_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  0.0480
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            74105
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.606
_diffrn_reflns_theta_min         1.569
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.982
_exptl_absorpt_correction_T_max  0.557
_exptl_absorpt_correction_T_min  0.056
_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    2.076
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.349
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.071
_refine_diff_density_max         1.285
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       0.00149(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         8622
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0187
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0163P)^2^+1.2290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0395
_refine_ls_wR_factor_ref         0.0403
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7946
_reflns_number_total             8622
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00240k2.cif
_cod_data_source_block           '[Au(iBu2dtc)2][AuCl2]'
_cod_depositor_comments
'Adding full bibliography for 7718352--7718363.cif.'
_cod_database_code               7718362
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C18 H36 N2 Au2 Cl2 S4'
_chemical_oxdiff_usercomment     'yellow rod JCS_103'
_shelx_estimated_absorpt_t_max   0.509
_shelx_estimated_absorpt_t_min   0.114
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_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:
 C3(H3), C7(H7), C12(H12), C16(H16)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C6(H6A,H6B), C11(H11A,H11B), C15(H15A,H15B)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              55921
_shelx_hkl_checksum              55246
_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 2.053
_oxdiff_exptl_absorpt_empirical_full_min 0.358