Identification of Au-hydrides as key intermediates in the reduction of Au(iii) prodrugs to active Au(i) species under protic conditions.
Ochs, Jasmine; Metzler-Nolte, Nils; Chemical science 17 (2026) 4183–4190; doi:10.1039/d5sc06212h

data_1576654
_publ_section_title
;
 Identification of Au-hydrides as key intermediates in the reduction of
 Au(iii) prodrugs to active Au(i) species under protic conditions.
;
_journal_issue                   8
_journal_name_full               'Chemical science'
_journal_page_first              4183
_journal_page_last               4190
_journal_paper_doi               10.1039/d5sc06212h
_journal_volume                  17
_journal_year                    2026
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C17 H18 Au Cl N2 O3 S'
_chemical_formula_sum            'C17 H18 Au Cl N2 O3 S'
_chemical_formula_weight         562.829
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_Int_Tables_number      19
_atom_sites_solution_primary     dual
_audit_creation_date             2025-02-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-02-17 deposited with the CCDC.	2025-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.8602(1)
_cell_length_b                   14.2036(2)
_cell_length_c                   25.7174(4)
_cell_measurement_reflns_used    4860
_cell_measurement_temperature    106(1)
_cell_measurement_theta_max      76.2490
_cell_measurement_theta_min      3.4480
_cell_volume                     1775.33(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      106(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9926
_diffrn_measured_fraction_theta_max 0.9369
_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    138.00 164.00   0.50    0.29    --  105.91 125.00  60.00   52
  2  \w     97.00 137.00   0.50    0.29    --  105.91 125.00  60.00   80
  3  \w    103.00 175.00   0.50    0.29    --  105.91 114.00  99.00  144
  4  \w     43.00  74.00   0.50    0.29    --  105.91 -61.00-120.00   62
  5  \w   -119.00 -74.00   0.50    0.07    --  -47.28-125.00  60.00   90
  6  \w   -161.00-124.00   0.50    0.29    --  -91.75 -42.00  84.00   74
  7  \w   -116.00 -85.00   0.50    0.29    --  -91.75 -42.00  84.00   62
  8  \w   -116.00 -81.00   0.50    0.07    --  -47.28-125.00  30.00   70
  9  \w   -117.00 -75.00   0.50    0.07    --  -47.28-125.00-150.00   84
 10  \w    -48.00 -23.00   0.50    0.29    --  -91.75  45.00  30.00   50
 11  \w    -48.00 -22.00   0.50    0.29    --  -91.75  45.00  90.00   52
 12  \w    -73.00 -25.00   0.50    0.29    --  -91.75 114.00  99.00   96
 13  \w    -59.00 -22.00   0.50    0.07    --  -47.28  82.00  19.00   74
 14  \w    -48.00 -23.00   0.50    0.29    --  -91.75  45.00 -90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1820132000
_diffrn_orient_matrix_UB_12      0.0703639000
_diffrn_orient_matrix_UB_13      -0.0299558000
_diffrn_orient_matrix_UB_21      0.2535250000
_diffrn_orient_matrix_UB_22      -0.0623179000
_diffrn_orient_matrix_UB_23      0.0103440000
_diffrn_orient_matrix_UB_31      -0.0556205000
_diffrn_orient_matrix_UB_32      -0.0540283000
_diffrn_orient_matrix_UB_33      -0.0508567000
_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  0.0643
_diffrn_reflns_av_unetI/netI     0.0736
_diffrn_reflns_Laue_measured_fraction_full 0.9926
_diffrn_reflns_Laue_measured_fraction_max 0.9369
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            6668
_diffrn_reflns_point_group_measured_fraction_full 0.9183
_diffrn_reflns_point_group_measured_fraction_max 0.8449
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.66
_diffrn_reflns_theta_min         3.44
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.227
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.106
_exptl_crystal_description       needle
_exptl_crystal_F_000             1070.649
_exptl_crystal_recrystallization_method
'grown by slow evaporation of DCM/methanol'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.5880
_refine_diff_density_min         -1.7114
_refine_diff_density_rms         0.2322
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   -0.002(14)
_refine_ls_d_res_high            0.7923
_refine_ls_d_res_low             12.8587
_refine_ls_goodness_of_fit_ref   1.0205
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    31
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3154
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.0184
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          -0.0006
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0684P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1055
_reflns_Friedel_coverage         0.713
_reflns_limit_h_max              5
_reflns_limit_h_min              -5
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              32
_reflns_limit_l_min              -31
_reflns_number_gt                3013
_reflns_number_total             3154
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5sc06212h2.cif
_cod_data_source_block           JO_MA_08_2_auto_a
_cod_original_sg_symbol_Hall     ' P 2ac 2ab'
_cod_database_code               1576654
_chemical_oxdiff_formula         CHNOSAu
_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. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C13(H13)
3.b Secondary CH2 refined with riding coordinates:
 C12(H12a,H12b)
3.c Me refined with riding coordinates:
 C15(H15a,H15b,H15c), C17(H17a,H17b,H17c)
3.d Aromatic/amide H refined with riding coordinates:
 N2(H2), C2(H2a), C11(H11), C3(H3), C10(H10), C4(H4), C9(H9), C5(H5), C8(H8)
;
_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 1.417
_oxdiff_exptl_absorpt_empirical_full_min 0.557