A series of new triarylantimony(V) dicarboxylates of the general formula Ar3SbL2 (where Ar = C6H5and L = C6H5CONHCH2COO–, C6H2(OH)3COO–, C6H5COO–, C6H5C2H2COO–, C6H4(OH)COO–, (C6H5)2(OH)C.COO–) have been prepared by the reaction of triarylantimony(V) dichloride and a carboxylic acid in the presence of triethylamine as well as the metathesis of sodium or silver salt of the carboxylic acid andtriarylantimony(V) dichloride. The newly synthesized compounds have been characterized by conventional methods. A tentative trigonalbipyramidal structure is suggested in which (OCOR) group occupy axial position and the three organic groups are situated at the equatorial position. The melting points of compounds did not change even after prolong stirring with water at room temperature for several hours indicating their hydrolytic stability.