Abstract The zinc coupling reaction of 1, 2-dichloroiodotrifluoroethane (I) in acetic anhydride- methylene chloride has been reinvestigated in more detail than its original disclosure. The expected coupling product C 4 F 6 Cl 4 was shown to be an isomeric mixture of three components, CF 2 ClCFClCFClCF 2 Cl (II, 80%), CFCl 2 CF 2 CF 2 CFCl 2 (IIa, 15%) and CF 2 ClCFClCF 2 CFCl 2 (IIb, 5%). In addition, other products eg CF 2 CFCl, C 6 F 9 Cl 5 ...