A novel trinuclear nickel (II) cluster {[NiL(EtOH)]2(OAc)2Ni} · 2EtOH has been synthsized and characterized by elemental analyses, TG-DTA, IR and 1H-NMR etc. The X-ray crystallography of the cluster indicates that the ligand moieties of the cluster provide the N2O2 donors set to Ni2, while one oxygen atom of the μ-acetato and one oxygen atom of the ethanol molecule coordinate to Ni2, consequently forming a slightly distorted octahedral geometry. The double μ-acetato bridges adopt the more familiar μ O-C-O form which connect the Ni2-Ni1 and Ni1-Ni2#, respectively, so quadruple µ-phenoxo oxygens from 2 ligand moieties and double oxygen atoms from µ-acetato constitute another octahedral geometry. It is worthy noting that the distance from the Ni1 to Ni2 (3.089Å) is significantly longer than other coordination bond, shows a weaker interaction. In addition, the HOMO and LUMO levels of the cluster were deduced. [ABSTRACT FROM AUTHOR]