The transition metal carboxylates M (O2CR) n (M= Cr, R= C2H5, C6H5, n= 3; M= Mn, Fe, Ni, R= CH3, C2H5, C6H5, n-C7H15, n= 2, not all combinations) have been prepared by oxidising suitable metal anodes electrochemically in solutions of RCOOH in acetonitrile. With Co and Cu, a wide range of carboxylic acids (R= C2H5, c-C3H5, c-C5H9, C6H5, n- C4H9, n-C7H15, 2-ethylhexanoic, oleic, linoleic) has been used successfully to give M ( ...