The crystal structures of benzyl triphenyl phosphonium tri-chloro cupprate (1) and tetra-chloroferrate (2) have been determined by X-ray crystallography. The structures contain completely isolated elongated tetrahedral [CuCl 3 ] -as dimmers with two bridging and four terminal chlorines (1), and tetrahedral [FeCl 4 ] -(2). In designing a metal containing surfactant system, salts (1) and (2) were refluxed with dodecyl amine to form the corresponding metallosurfactants (1a) and (2a) or to hexadecyl pyridinium chloride to form the corresponding cationic metallosurfactants (1b) and (2b), respectively. The critical micelle concentration (CMC) values of these surfactant metal complexes in aqueous solution were recorded from surface tension measurements. They showed antibacterial activity against the growth of Gram positive and Gram negative bacteria.