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_7250880
_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         'C52 H48 Au4 N4 S4'
_chemical_formula_sum            'C52 H48 Au4 N4 S4'
_chemical_formula_weight         1645.05
_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
_audit_creation_date             2025-04-15
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-04-22 deposited with the CCDC.	2025-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.548(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.5871(11)
_cell_length_b                   12.3929(7)
_cell_length_c                   21.3684(14)
_cell_measurement_reflns_used    9798
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.04
_cell_measurement_theta_min      2.40
_cell_volume                     5035.1(5)
_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)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0358
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            41666
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.926
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.824
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.4978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1085 before and 0.0551 after correction.
The Ratio of minimum to maximum transmission is 0.6673.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.170
_exptl_crystal_description       block
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.026
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         11555
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0077P)^2^+7.6350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0440
_refine_ls_wR_factor_ref         0.0460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10132
_reflns_number_total             11555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00724k2.cif
_cod_data_source_block           mg-6_tetr_a
_cod_depositor_comments
'Adding full bibliography for 7250880--7250889.cif.'
_cod_database_code               7250880
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.201
_shelx_estimated_absorpt_t_min   0.088
_olex2_refinement_description
;
1. Restrained distances
 S4B-C40
 1.712 with sigma of 0.02
 C41A-C40
 1.455 with sigma of 0.02
 C41B-C42B
 1.455 with sigma of 0.02
 C41A-C42A
 1.471 with sigma of 0.02
 C42A-C43A
 1.455 with sigma of 0.02
 C40-S4A
 1.712 with sigma of 0.02
 S4A-C43A
 1.712 with sigma of 0.02
 C43B-C42B
 1.455 with sigma of 0.02
 S4B-C43B
 1.712 with sigma of 0.02
 C41B-C40
 1.455 with sigma of 0.02
 C40-S4B
 1.712 with sigma of 0.02
 C28B-C27
 1.455 with sigma of 0.02
 S3A-C27
 1.712 with sigma of 0.02
 S3A-C30
 1.712 with sigma of 0.02
 S3B-C29
 1.712 with sigma of 0.02
 S3B-C27
 1.712 with sigma of 0.02
 C29-C28A
 1.471 with sigma of 0.02
 C30-C28B
 1.471 with sigma of 0.02
 C28A-C27
 1.455 with sigma of 0.02
 C15A-C16
 1.471 with sigma of 0.02
 C15A-C14
 1.455 with sigma of 0.02
 C15B-C14
 1.455 with sigma of 0.02
 C16-C17
 1.455 with sigma of 0.02
 S2A-C17
 1.712 with sigma of 0.02
 C16-S2B
 1.712 with sigma of 0.02
 C16-C15A
 1.471 with sigma of 0.02
 C15B-C17
 1.471 with sigma of 0.02
 S2A-C14
 1.712 with sigma of 0.02
 C17-C16
 1.455 with sigma of 0.02
 C2A-C4
 1.471 with sigma of 0.02
 S1A-C3
 1.712 with sigma of 0.02
 C4-S1B
 1.712 with sigma of 0.02
 C4-C3
 1.455 with sigma of 0.02
 S1B-C1
 1.712 with sigma of 0.02
 S1A-C1
 1.712 with sigma of 0.02
 C3-C2B
 1.471 with sigma of 0.02
 C1-C2B
 1.455 with sigma of 0.02
2. Restrained planarity
 S4A, C41A, C42A, C43A
 with sigma of 0.1
 S4B, C41B, C42B, C43B
 with sigma of 0.1
 S4B, C40, C41B, C42B, C43B
 with sigma of 0.1
 S4A, C40, C41A, C42A, C43A
 with sigma of 0.1
 S3A, C27, C28A, C29, C30
 with sigma of 0.1
 S3B, C27, C28B, C29, C30
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(C42B) = Uanis(C43A)
Uanis(C41A) = Uanis(C41B)
Uanis(S4B) = Uanis(S4A)
Uanis(C15A) = Uanis(C15B)
Uanis(S1A) = Uanis(S1B)
Uanis(C2B) = Uanis(C2A)
Uanis(C28B) = Uanis(C28A)
Uanis(S3A) = Uanis(S3B)
Uanis(C43B) = Uanis(C42A)
Uanis(C43A) = Uanis(C42B)
Uanis(C41A) = Uanis(C42A)
Uanis(C43A) = Uanis(C41B)
4. Others
 Fixed Sof: S1A(0.8) S1B(0.2) S2A(0.55) S2B(0.45) S3A(0.8) S3B(0.2) S4A(0.5)
 S4B(0.5) C2A(0.8) H2A(0.8) C2B(0.2) H2B(0.2) H3A(0.8) H3B(0.2) H4B(0.2)
 H4A(0.8) C15A(0.55) H15A(0.55) C15B(0.45) H15B(0.45) H16A(0.45) H16(0.55)
 H17(0.55) H17A(0.45) C28A(0.8) H28A(0.8) C28B(0.2) H28B(0.2) H29A(0.2)
 H29(0.8) H30(0.8) H30A(0.2) C41A(0.5) H41A(0.5) C41B(0.5) H41B(0.5) C42A(0.5)
 H42A(0.5) C42B(0.5) H42B(0.5) C43A(0.5) H43A(0.5) C43B(0.5) H43B(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C2B(H2B), C3(H3A), C3(H3B), C4(H4B), C4(H4A), C8(H8), C9(H9),
 C10(H10), C15A(H15A), C15B(H15B), C16(H16A), C16(H16), C17(H17), C17(H17A),
 C21(H21), C22(H22), C23(H23), C28A(H28A), C28B(H28B), C29(H29A), C29(H29),
 C30(H30), C30(H30A), C34(H34), C35(H35), C36(H36), C41A(H41A), C41B(H41B),
 C42A(H42A), C42B(H42B), C43A(H43A), C43B(H43B), C47(H47), C48(H48), C49(H49)
5.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C51(H51A,H51B,H51C), C52(H52A,
 H52B,H52C)
;
_shelx_res_checksum              83347
_olex2_submission_special_instructions 'No special instructions were received'