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_7250886
_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         'C39 H36 Au3 N3 S3'
_chemical_formula_sum            'C39 H36 Au3 N3 S3'
_chemical_formula_weight         1233.81
_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     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-04-21
_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                100.3410(10)
_cell_angle_beta                 97.3260(10)
_cell_angle_gamma                103.9530(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9569(2)
_cell_length_b                   11.6078(3)
_cell_length_c                   17.3895(4)
_cell_measurement_reflns_used    9809
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.57
_cell_measurement_theta_min      2.42
_cell_volume                     1887.90(8)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX3 (Bruker, 2018)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON-III CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            43955
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.598
_diffrn_reflns_theta_min         2.142
_exptl_absorpt_coefficient_mu    11.825
_exptl_absorpt_correction_T_max  0.149
_exptl_absorpt_correction_T_min  0.095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.170
_exptl_crystal_description       prism
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.095
_refine_diff_density_min         -1.200
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       0.00075(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         13735
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0233
_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^)+(0.0076P)^2^+1.8655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0432
_refine_ls_wR_factor_ref         0.0452
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12127
_reflns_number_total             13735
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00724k2.cif
_cod_data_source_block           MG7
_cod_depositor_comments
'Adding full bibliography for 7250880--7250889.cif.'
_cod_database_code               7250886
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.270
_shelx_estimated_absorpt_t_min   0.201
_olex2_refinement_description
;
1. Restrained distances
 S1-C11 = S1-C12 = S1'-C11' = S1'-C12'
 1.7 with sigma of 0.003
 S2-C24 = S2-C25 = S2'-C24' = S2'-C25'
 1.7 with sigma of 0.003
 S3-C37 = S3-C38 = S3'-C37' = S3'-C38'
 1.7 with sigma of 0.003
 C10-C13 = C10-C13'
 1.45 with sigma of 0.003
 C23-C26 = C23-C26'
 1.45 with sigma of 0.003
 C36-C39 = C36-C39'
 1.45 with sigma of 0.003
 C10-C11 = C12-C13 = C10-C11' = C12'-C13'
 1.36 with sigma of 0.003
 C23-C24 = C25-C26 = C23-C24' = C25'-C26'
 1.36 with sigma of 0.003
 C36-C37 = C38-C39 = C36-C37' = C38'-C39'
 1.36 with sigma of 0.003
2. Restrained planarity
 C10, S1, C11, C12, C13
 with sigma of 0.003
 C10, S1', C11', C12', C13'
 with sigma of 0.003
 C23, S2, C24, C25, C26
 with sigma of 0.003
 C23, S2', C24', C25', C26'
 with sigma of 0.003
 C36, S3, C37, C38, C39
 with sigma of 0.003
 C36, S3', C37', C38', C39'
 with sigma of 0.003
3. Uiso/Uaniso restraints and constraints
Uanis(S1) = Uanis(C12')
Uanis(S1') = Uanis(C12)
Uanis(C11) = Uanis(C13')
Uanis(C11') = Uanis(C13)
Uanis(S2) = Uanis(C25')
Uanis(S2') = Uanis(C25)
Uanis(C24) = Uanis(C26')
Uanis(C24') = Uanis(C26)
Uanis(S3) = Uanis(C38')
Uanis(S3') = Uanis(C38)
Uanis(C37) = Uanis(C39')
Uanis(C37') = Uanis(C39)
4. Others
 Fixed Sof: S1(0.75) C11(0.75) H11A(0.75) C12(0.75) H12A(0.75) C13(0.75)
 H13A(0.75) S1'(0.25) C11'(0.25) H11B(0.25) C12'(0.25) H12B(0.25) C13'(0.25)
 H13B(0.25) S2(0.75) C24(0.75) H24A(0.75) C25(0.75) H25A(0.75) C26(0.75)
 H26A(0.75) S2'(0.25) C24'(0.25) H24B(0.25) C25'(0.25) H25B(0.25) C26'(0.25)
 H26B(0.25) S3(0.5) C37(0.5) H37A(0.5) C38(0.5) H38A(0.5) C39(0.5) H39A(0.5)
 S3'(0.5) C37'(0.5) H37B(0.5) C38'(0.5) H38B(0.5) C39'(0.5) H39B(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C11(H11A), C12(H12A), C13(H13A), C11'(H11B),
 C12'(H12B), C13'(H13B), C17(H17), C18(H18), C19(H19), C24(H24A), C25(H25A),
 C26(H26A), C24'(H24B), C25'(H25B), C26'(H26B), C30(H30), C31(H31), C32(H32),
 C37(H37A), C38(H38A), C39(H39A), C37'(H37B), C38'(H38B), C39'(H39B)
5.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C),
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              15441
_olex2_submission_special_instructions 'No special instructions were received'