New nonsymmetric metallo(II)-salphen complexes 1-6 [salphen = N,NЈ-bis(salicylidene)-1,2-diaminobenzene, M = Zn, Ni] have been prepared in high yield by a templated, one-pot two-step procedure starting from substituted orthophenylenediamines, salicylaldehydes and metal acetates in MeOH under mild conditions. The procedure allows the introduction of functional groups in the bridging phenyl fragment, whereas the use of the substituted monoimine intermediates 7-10 results in complexes with two structurally dif-