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_7250885
_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         '0.333(C39 H36 Au3 N3 S3)'
_chemical_formula_sum            'C13 H12 Au N S'
_chemical_formula_weight         411.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-04-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2025-04-22 deposited with the CCDC.	2025-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.929(2)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   11.8718(6)
_cell_length_b                   20.3094(10)
_cell_length_c                   15.8840(8)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.042
_cell_measurement_theta_min      2.347
_cell_volume                     3772.4(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11810
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.986
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.836
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.2950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1287 before and 0.0613 after correction.
The Ratio of minimum to maximum transmission is 0.3954.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.172
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.677
_refine_diff_density_min         -3.998
_refine_diff_density_rms         0.313
_refine_ls_extinction_coef       0.00031(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         6440
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0832P)^2^+31.5862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1403
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5520
_reflns_number_total             6440
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00724k2.cif
_cod_data_source_block           mo_21kub51_1_0m_a
_cod_depositor_comments
'Adding full bibliography for 7250880--7250889.cif.'
_cod_database_code               7250885
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.201
_shelx_estimated_absorpt_t_min   0.044
_olex2_refinement_description
;
1. Restrained distances
 S3A-C27
 1.71 with sigma of 0.02
 C27-C28A
 1.38 with sigma of 0.02
 C30-C29
 1.38 with sigma of 0.02
 C27-S3B
 1.71 with sigma of 0.02
 C29-C28A
 1.42 with sigma of 0.02
 C30-C28B
 1.42 with sigma of 0.02
 C28B-C27
 1.38 with sigma of 0.02
 C29-S3B
 1.71 with sigma of 0.02
 S1A-C1
 1.71 with sigma of 0.02
 C3-S1B
 1.71 with sigma of 0.02
 C27-S3A
 1.71 with sigma of 0.02
 S1A-C4
 1.71 with sigma of 0.02
 S1B-C1
 1.71 with sigma of 0.02
 C2B-C4
 1.42 with sigma of 0.02
 C2A-C1
 1.38 with sigma of 0.02
 S3B-C27
 1.71 with sigma of 0.02
 C2A-C3
 1.42 with sigma of 0.02
 C30-S3A
 1.71 with sigma of 0.02
 C3-C4
 1.38 with sigma of 0.02
 C2B-C1
 1.38 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(C28B) = Uanis(C28A)
Uanis(C2B) = Uanis(C2A)
Uanis(C28A) = Uanis(C30)
Uanis(C2B) = Uanis(C3)
Uanis(C15) = Uanis(C14)
3. Others
 Fixed Sof: C28B(0.3) H28B(0.3) C2B(0.4) H2B(0.4) S1B(0.4) C28A(0.7) H28A(0.7)
 H3A(0.6) H3B(0.4) H30A(0.3) H30(0.7) H4B(0.4) H4A(0.6) H29(0.7) H29A(0.3)
 S3A(0.7) S3B(0.3) S1A(0.6) C2A(0.6) H2A(0.6)
4.a Aromatic/amide H refined with riding coordinates:
 C28B(H28B), C2B(H2B), C28A(H28A), C15(H15), C22(H22), C16(H16), C34(H34),
 C3(H3A), C3(H3B), C36(H36), C30(H30A), C30(H30), C21(H21), C35(H35), C8(H8),
 C4(H4B), C4(H4A), C17(H17), C29(H29), C29(H29A), C10(H10), C23(H23), C9(H9),
 C2A(H2A)
4.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C38(H38A,H38B,H38C), C13(H13A,H13B,H13C), C12(H12A,H12B,
 H12C), C39(H39A,H39B,H39C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              77944
_olex2_submission_special_instructions 'No special instructions were received'