Gold-catalyzed amination of <i>in situ</i> formed alkyl gold species with <i>p</i>-quinonediimines as a N source.
Pan, Xinyu; Abdulla, Yusuf; Bao, Ming; Xu, Xinfang; Organic & biomolecular chemistry 24 (2026) 670–674; doi:10.1039/d5ob01823d

data_7161039
_publ_section_title
;
 Gold-catalyzed amination of <i>in situ</i> formed alkyl gold species with
 <i>p</i>-quinonediimines as a N source.
;
_journal_issue                   3
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              670
_journal_page_last               674
_journal_paper_doi               10.1039/d5ob01823d
_journal_volume                  24
_journal_year                    2026
_chemical_formula_moiety         'C31 H29 N3 O5 S2'
_chemical_formula_sum            'C31 H29 N3 O5 S2'
_chemical_formula_weight         587.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2plck7
_audit_creation_date             2025-09-19
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-09-22 deposited with the CCDC.	2025-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.322(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9606(11)
_cell_length_b                   10.2207(10)
_cell_length_c                   18.4680(13)
_cell_measurement_reflns_used    4624
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.0780
_cell_measurement_theta_min      3.4650
_cell_volume                     3007.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.929
_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    -81.00 -16.00   0.50    0.20    --  -39.95 110.00  41.00  130
  2  \w     32.00  82.00   0.50    0.20    --   39.95-110.00 -53.00  100
  3  \w    -69.00 -43.00   0.50    0.20    --  -94.50 110.00  41.00   52
  4  \w   -127.00 -97.00   0.50    0.20    --  -94.50-110.00 -53.00   60
  5  \w    107.00 132.00   0.50    0.20    --  108.87 110.00  41.00   50
  6  \w     33.00 107.00   0.50    0.20    --  108.87-110.00 -53.00  148
  7  \w    -25.00  45.00   0.50    0.20    --  -39.95  19.00 150.00  140
  8  \w    -44.00  14.00   0.50    0.20    --   39.95 -19.00 -30.00  116
  9  \w    -32.00  19.00   0.50    0.20    --   39.95 -19.00 -90.00  102
 10  \w    -44.00  21.00   0.50    0.20    --   39.95 -19.00-150.00  130
 11  \w    -40.00 -15.00   0.50    0.20    --  -94.50  45.00 -90.00   50
 12  \w    -43.00 -16.00   0.50    0.20    --  -94.50  45.00-150.00   54
 13  \w    -71.00 -20.00   0.50    0.20    --  -94.50 125.00 120.00  102
 14  \w    -43.00 -15.00   0.50    0.20    --  -94.50  45.00   0.00   56
 15  \w    -50.00 -17.00   0.50    0.20    --  -94.50  45.00 150.00   66
 16  \w    -48.00 -22.00   0.50    0.20    --  -94.50  45.00-180.00   52
 17  \w    -43.00 -15.00   0.50    0.20    --  -94.50  45.00-120.00   56
 18  \w    -71.00 -46.00   0.50    0.20    --  -94.50  61.00   0.00   50
 19  \w     35.00 105.00   0.50    0.20    --  108.87 -77.00   0.00  140
 20  \w     99.00 143.00   0.50    0.20    --  108.87  45.00-150.00   88
 21  \w     45.00  71.00   0.50    0.20    --  108.87 -61.00 120.00   52
 22  \w     34.00  60.00   0.50    0.20    --  108.87 -61.00 -60.00   52
 23  \w     73.00 102.00   0.50    0.20    --  108.87 -94.00  30.00   58
 24  \w     29.00 105.00   0.50    0.20    --  108.87 -94.00 -30.00  152
 25  \w     38.00  71.00   0.50    0.20    --  108.87 -61.00   0.00   66
 26  \w     80.00 171.00   0.50    0.20    --  108.87  45.00  90.00  182
 27  \w     41.00 107.00   0.50    0.20    --  108.87-125.00  30.00  132
 28  \w     34.00  71.00   0.50    0.20    --  108.87 -61.00  90.00   74
;
_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      -0.0073053000
_diffrn_orient_matrix_UB_12      0.1476033000
_diffrn_orient_matrix_UB_13      0.0148977000
_diffrn_orient_matrix_UB_21      -0.0851175000
_diffrn_orient_matrix_UB_22      -0.0229272000
_diffrn_orient_matrix_UB_23      0.0332556000
_diffrn_orient_matrix_UB_31      0.0453264000
_diffrn_orient_matrix_UB_32      -0.0195817000
_diffrn_orient_matrix_UB_33      0.0752195000
_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  0.1138
_diffrn_reflns_av_unetI/netI     0.0876
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15838
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.019
_diffrn_reflns_theta_min         2.773
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.966
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.49a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5680
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1689
_refine_ls_R_factor_gt           0.0890
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2470
_refine_ls_wR_factor_ref         0.3396
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2490
_reflns_number_total             5680
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ob01823d2.cif
_cod_data_source_block           lf-167
_cod_database_code               7161039
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N S'
_cell_oxdiff_angle_alpha         89.837(6)
_cell_oxdiff_angle_beta          93.333(5)
_cell_oxdiff_angle_gamma         89.953(8)
_cell_oxdiff_length_a            15.9567(12)
_cell_oxdiff_length_b            10.2261(12)
_cell_oxdiff_length_c            18.4632(8)
_cell_oxdiff_measurement_reflns_used 4624
_cell_oxdiff_volume              3007.6(4)
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.943
_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. Rigid bond restraints
 C00M, C00K
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3.a Ternary CH refined with riding coordinates:
 C00N(H00N)
3.b Aromatic/amide H refined with riding coordinates:
 N009(H009), C00D(H00D), C00F(H00F), C00H(H00H), C00I(H00I), C00L(H00L),
 C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V),
 C00X(H00X), C00Z(H00Z), C010(H010), C011(H011), C012(H012)
3.c X=CH2 refined with riding coordinates:
 C00M(H00A,H00B)
3.d Idealised Me refined as rotating group:
 C013(H01A,H01B,H01C), C014(H01D,H01E,H01F), C015(H01G,H01H,H01I)
;
_shelx_res_checksum              91982
_shelx_hkl_checksum              87640
_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 4.773
_oxdiff_exptl_absorpt_empirical_full_min 0.357