The interaction of a linearly linked tris-cyclam derivative incorporating p-xylyl linkages between nitrogen donor atoms on adjacent rings with nickel(II), copper(II), zinc(II), cadmium(II), and palladium(II) is reported. All five metals yield solid complexes in which the metal-ligand stoichiometry is 3:1. In the case of Cu(II), a spectrophotometric titration confirmed the formation of a complex of this stoichiometry in acetonitrile. Where appropriate, visible spectral, electrochemical, magnetic moment, ESR, and NMR studies have been performed to probe the nature of the respective complexes in both the solid state and in solution. Cyclic voltamograms of both the Ni(II) (low spin) and Cu(II) complexes both yield evidence for M(II)/M(III) as well as M(I)/M(II) couples in acetonitrile.