Thiophenyl and benzothiophenyl gold isocyanide complexes: synthesis, structures, and aurophilic and gold-involving chalcogen bonding interactions
Pavlov, Kirill G.; Grudova, Mariya R.; Kubasov, Alexey S.; Khrustalev, Victor N.; Kritchenkov, Ilia S.; Gomila, Rosa M.; Frontera, Antonio; Tskhovrebov, Alexander G.; CrystEngComm 27 (2025) 7021–7031; doi:10.1039/D5CE00724K

data_7250888
_publ_section_title
;
 Thiophenyl and benzothiophenyl gold isocyanide complexes: synthesis,
 structures, and aurophilic and gold-involving chalcogen bonding
 interactions
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              7021
_journal_page_last               7031
_journal_paper_doi               10.1039/D5CE00724K
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C51 H42 Au3 N3 S3'
_chemical_formula_sum            'C51 H42 Au3 N3 S3'
_chemical_formula_weight         1383.95
_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
_audit_creation_date             2025-04-22
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7205)
;
_audit_update_record
;
2025-04-22 deposited with the CCDC.	2025-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                64.989(9)
_cell_angle_beta                 80.550(9)
_cell_angle_gamma                79.057(8)
_cell_formula_units_Z            2
_cell_length_a                   11.0862(13)
_cell_length_b                   14.950(3)
_cell_length_c                   15.372(3)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.110
_cell_measurement_theta_min      2.255
_cell_volume                     2256.7(7)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 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 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13709
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.214
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    9.906
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.2853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1366 before and 0.0496 after correction.
The Ratio of minimum to maximum transmission is 0.3824.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.037
_exptl_crystal_description       block
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.594
_refine_diff_density_min         -2.527
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         7800
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0630
_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^)+70.5839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1505
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7123
_reflns_number_total             7800
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00724k2.cif
_cod_data_source_block           mo_22kub38_0m_a
_cod_depositor_comments
'Adding full bibliography for 7250880--7250889.cif.'
_cod_original_cell_volume        2256.6(7)
_cod_database_code               7250888
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.437
_shelx_estimated_absorpt_t_min   0.066
_olex2_refinement_description
;
1. Restrained distances
 S3B-C36B
 1.74 with sigma of 0.01
 C35B-Au3B
 2.03 with sigma of 0.01
 C35B-C42B
 1.41 with sigma of 0.01
 S3B-C37B
 1.74 with sigma of 0.01
 C36B-C42B
 2.28 with sigma of 0.02
 C36B-C35B
 1.36 with sigma of 0.01
 N3A-C44A
 1.42 with sigma of 0.01
 C43A-N3A
 1.14 with sigma of 0.01
 N3A-C43A
 1.13 with sigma of 0.01
 C43A-Au3A
 1.99 with sigma of 0.01
 N3B-C43B
 1.13 with sigma of 0.01
 C43B-Au3B
 1.99 with sigma of 0.01
 C49B-C51B
 1.52 with sigma of 0.02
 C45B-C50B
 1.52 with sigma of 0.02
 N3A-Au3A
 3.12 with sigma of 0.01
 N3B-Au3B
 3.12 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
Uanis(C43A) = Uanis(N3A) = Uanis(C44A)
Uanis(C35B) = Uanis(C36B) = Uanis(C42B) = Uanis(C37B)
Uanis(C43B) = Uanis(N3B) = Uanis(C44B) = Uanis(C49B) = Uanis(C45B)
Uanis(C38A) = Uanis(C39A) = Uanis(C40A) = Uanis(C41A) = Uanis(C42A) =
Uanis(C37A) = Uanis(C35A) = Uanis(C36A)
Uanis(C46A) = Uanis(C44A) = Uanis(C45A) = Uanis(C51A) = Uanis(C48A) =
Uanis(C49A) = Uanis(C47A) = Uanis(C50A)
Uanis(C41B) = Uanis(C42B) = Uanis(C38B) = Uanis(C39B) = Uanis(C40B) =
Uanis(C37B)
Uanis(C44B) = Uanis(C49B) = Uanis(C48B) = Uanis(C47B) = Uanis(C46B) =
Uanis(C51B) = Uanis(C45B) = Uanis(C50B)
3. Others
 Fixed Sof: Au3B(0.5) S3B(0.5) N3B(0.5) C35B(0.5) C36B(0.5) H36B(0.5)
 C41B(0.5) H41B(0.5) C42B(0.5) C37B(0.5) C38B(0.5) H38B(0.5) C39B(0.5)
 H39B(0.5) C40B(0.5) H40B(0.5) C43B(0.5) C45B(0.5) C44B(0.5) C49B(0.5)
 C48B(0.5) H48B(0.5) C47B(0.5) H47B(0.5) C46B(0.5) H46B(0.5) C50B(0.5)
 H50A(0.5) H50B(0.5) H50C(0.5) C51B(0.5) H51A(0.5) H51B(0.5) H51C(0.5)
 Au3A(0.5) S3A(0.5) N3A(0.5) C35A(0.5) C36A(0.5) H36A(0.5) C38A(0.5) H38A(0.5)
 C39A(0.5) H39A(0.5) C40A(0.5) H40A(0.5) C41A(0.5) H41A(0.5) C42A(0.5)
 C37A(0.5) C43A(0.5) C44A(0.5) C45A(0.5) C46A(0.5) H46A(0.5) C47A(0.5)
 H47A(0.5) C48A(0.5) H48A(0.5) C49A(0.5) C50A(0.5) H50D(0.5) H50E(0.5)
 H50F(0.5) C51A(0.5) H51D(0.5) H51E(0.5) H51F(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14),
 C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C29(H29), C30(H30), C31(H31),
  C36B(H36B), C41B(H41B), C38B(H38B), C39B(H39B), C40B(H40B), C48B(H48B),
 C47B(H47B), C46B(H46B), C36A(H36A), C38A(H38A), C39A(H39A), C40A(H40A),
 C41A(H41A), C46A(H46A), C47A(H47A), C48A(H48A)
4.b Fitted hexagon refined as free rotating group:
 C41B(C42B,C37B,C38B,C39B,C40B), C45B(C44B,C49B,C48B,C47B,C46B), C38A(C39A,
 C40A,C41A,C42A,C37A)
4.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C50B(H50A,H50B,H50C), C51B(H51A,H51B,H51C), C50A(H50D,H50E,H50F),
 C51A(H51D,H51E,H51F)
;
_shelx_res_checksum              13700
_olex2_submission_special_instructions 'No special instructions were received'