Abstract The cleavage of bis (1, 2, 3-thiadiazole) s in the presence of strong bases in situ gives bis (alkynethiolate) s, which provide bis (alkynethiolate) gold (I) derivatives with the general formula [Au 2 (S–C≡ C–spacer–C≡ C–S) L 2](L= monophosphanes; spacer= none, 1, 4-C 6 H 4, 1, 3-C 6 H 4, 2, 7-C 15 H 12 and 3, 5-C 7 H 7 N). The dinuclear structure was confirmed by X-ray diffraction studies of the complexes (PPN) 2 [Au 2 (S–C≡ C–C≡ ...