A series of triarylantimony (V) dithiocyanates has been prepared by oxidising the appropriate antimony (III) compound with thiocyanogen. IR and 14N NMR spectroscopy indicate the presence of terminally N-bonded thiocyanate groups and this has been confirmed by a crystal structure determination for the SbPh3 (NCS) 2. The asymmetric unit contains three independent trigonal bipyramidal molecules, which differ in the orientations ...