The crystal structure of the precursor [Pd(PPh3)(2)(Hatu)][CF3SO3](2) (1) and the anion-templated syntheses of the nickel/palladium metalla-macrocycles [Pd2Ni2(atu)(4)(PPh2R)(4)X](3+) (R = Ph, X = I, 2; R = Py, X = Cl, 3; atu = deprotonated amidinothiourea) are herein reported. The three new compounds have been structurally characterised and, for 1 and 3, interesting intermolecular interactions leading to dimers and extended structures in the solid state, respectively, have been observed. (C) 2003 Elsevier Ltd. All rights reserved.