Abstract Tetrachloroantimony(V) carboxilates and tetrachloroantimony(V) alkoxides, resp., react with carboxilic acids and alkohols or water, resp., to yield d,h-μ-carboxilato-e-μ-hydroxo-f-μ-oxo-bis[trichloroantimony(V)] (1, R = H, CH3), a new type of cyclic antimony(V) compounds. The crystal and molecular structure of 1 (R = CH3) is determined by X-ray analysis. Units of 1 (R - CH3) are associated by strong hydrogen bonds. The vibrational spectra of 1 (R = H, CH3) are discussed.