Metal complexes of divalent copper (1-2), cobalt (3), and nickel (4) with mixed ligands acetylacetone (acac) and adenine were prepared and characterized by IR, mass spectra, elemental and thermal analysis. The X-ray crystal structures of {[Cu(acac)(2)(adenine)]center dot EtOH} complex (1) and {[Cu(acac)(2)(adenine)]center dot DMF center dot H2O} (2) were determined. Compound (1) crystallizes in the triclinic space group P - 1 with a = 7.547(3) angstrom, b = 7.828(3) angstrom, c = 17.791(6) angstrom, alpha = 79.538(6)degrees, beta = 82.240(7)degrees, gamma = 86.010 (6)degrees, V = 1023.1(6) angstrom(3), and Z = 2. Complex (1) forms a hydrogen bonded 2: 2 complex {[Cu(acac)(2)(adenine)](2): [EtOH](2)} arranged in bilayers. Complex (2) crystallizes in the triclinic space group P - 1 with a = 7.828(2) angstrom, b = 8.095(2) angstrom, c = 16.995(5) angstrom, alpha = 78.508(5)degrees, b = 84.949(5)degrees, gamma = 89.285(5)degrees, V = 1051.2(5)angstrom(3), and Z = 2. Complex (2) also forms bilayers with H-bonded DMF. Thermal analysis TG and DSC of the compounds (25-800 degrees C, under N-2) reveals the disproportionation of ligands with the associated heat.