The synthesis and properties of bimetallic complexes [Cl(2)M(LL)MCl(2)] (M = Pt, Pd) are reported (LL are two 1,2,4-triaminobutane units linked by nitrogens in position 4 as alpha,omega-dicarboxylic acid bis(amides) H2NCH2CHNH2CH2CH2NHCO(CH2)(n)CONHCH2CH2CHNH2CH(2)NH(2), n = 3-6, 8). In these complexes two cis-PtCl2 fragments are bridged by a spacer. Their solvolysis in Me(2)SO was studied by multinuclear (H-1, C-13 and Pt-195) NMR spectroscopy. The ionic compounds [(DMSO)(Cl)Pt(LL)Pt(Cl)(DMSO)]Cl-2 were isolated and characterized as mixtures of cis/trans isomers. The ligands containing two vicinal diamino units were prepared from N-1,N-2-bis(tert-butoxycarbonyl)-N-4-(trifluoroacetyl)-1,2,4-triaminobutane, by basic removal of the trifluoroacetyl group and acylation of free amine with dicarboxylic acid dichlorides of variable chains. Subsequent splitting of Boc protecting groups and reaction with K2PtCl4 or Na2PdCl4 under controlled-pH conditions afforded the title compounds.