Abstract Copper (I) pentafluorothiophenolate, CuSC 6 F 5 reacted with a number of acyl and alkyl halides in either n-hexane or DMF. The products RCH 2 SC 6 F 5 (R= Me, Ph, C 6 F 5 S, C 6 F 5 SCH 2), Ph 2 CHSC 6 F 5, R 3 CSC 6 F 5 (R= Me, Ph) and RCOSC 6 F 5 (R= Me, C 6 F 5) have been characterized and their spectra, particularly NMR spectra (H 1, C 13, F 19) have been examined.