Pentafluorophenylantimony(V) di- and tetracarboxylates of the molecular formula C6F5SbX2L2 (when X = L = OCOR (R = -CH3, CH2Cl, -CHCl2, -CCl3, -CF3, -CH2OC6H3Cl2-2,4, -CH2OC6H2Cl3-2,4,5) and when X = Cl; L = -OCOCH3, -OCOCHCl2) have been synthesized by the metathetical reaction of pentafluorophenylantimony(V) tetrachloride and (dibromide)dichloride with corresponding sodium salt of carboxylic acids in appropriate molar ratio using 15-crown-5 as phase transfer catalyst. The van't Hoff factor 'i' and molar conductance data of the compounds revealed them to be monomeric and non-conducting in nature. Elemental analysis, UV, IR and NMR (H-1, F-19 and C-13) were used to characterize the derivatives. Compounds are tentatively assigned as a pentacoordinated square pyramidal structure in which carboxylate ligand behaving as a monodentate ligand. (C) 2002 Elsevier Science B.V. All rights reserved.