Abstract To clear some confusion in the literature, the “direct syntheses “of As 2 (C 6 F 4) 3 and of Sb 2 (C 6 F 4) 3 have been repeated and the identities of the compounds confirmed by analytical data and spectroscopic methods. Mixtures of As and Sb, when heated with 1, 2- I 2 C 6 F 4, give As 2 (C 6 F 4) 3, Sb 2 (C 6 F 4) 3 and AsSb-(C 6 F 4) 3. When Sb is heated with 1, 2-I 2 C 6 H 4 and 1, 2-I 2 C 6 F 4, three compounds are formed: Sb 2 (C 6 F 4) 3, Sb ...