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Four new heterobimetallic complexes [CuL 1 ][MnCl 4 ] ( 1 ), [CuL 2 ][MnCl 4 ] ( 2 ), [NiL 1 ][MnCl 4 ] ( 3 ), [NiL 2 ][MnCl 4 ] ( 4 ) (L 1 = 4,6,6-trimethyl-1,9-diamino-3,7-di-aza-nona-3-ene; L 2 = 1,15-dihydroxy-7,9,9-trimethyl-3,6,10,13-tetra-aza-pentadeca-6-ene) have been prepared from elemental metals, ethylenediamine dihydrochloride or its N-(2-hydroxyethyl) derivative and acetone by the template condensation reaction. All complexes have been characterized by elemental analysis, IR and UV-Visible spectroscopy. The structures of 2 and 3 have been determined by X-ray crystallography ( 2 : Orthorhombic, Pna2 1, a = 20.136(4), b = 11.185(2), c = 10.251(2)Å, Z = 4; 3 : Orthorhombic, Pca2 1, a = 14.335(2), b = 11.405(2), c = 11.154(2)Å, Z = 4 ). Both crystals consist of alternating complex cations [ML] 2+ and anions [MnCl 4 ] 2- linked together by N-H···Cl-Mn and O-H···Cl-Mn hydrogen bonds forming 2D corrugated sheets in ( 2 ) and 1D helical chains in ( 3 ). Complex 2 represents the first single crystal structure elucidation of the complex containing L 2 . [ABSTRACT FROM AUTHOR]