Department of Chemistry, The University of Burdwan, Burdwan-713 104, West Bengal, India E-mail : barin_l@yahoo.co.uk Fax : 91-342-2530452 Manuscript received online 23 July 2012, accepted 30 July 2012. One hexacoordinated mononuclear compound of the type [Ni(L)(CH3COO)PF6 (1) [L = N,N'-(bis(pyridine-2-yl)benzylidine)-1,4-butanediamine] has been synthesized and characterized by physico-chemical and spectroscopic methods. Single crystal X-ray structural analysis shows that nickel(ll) center in 1 adopts a disto1��ted octahedral geometry bound by four N atoms of L and two 0 atoms of an acetate in chelating fashions. In crystalline state, mononuclear units in 1 are engaged in weak cooperative intermolecular C...H...O hydrogen bonds and ��...�� interactions afl'o1��ding to a 2D sheet structure. Compound 1 is thermally stable up to 251 ��C and displays 1(��-��*) fluorescence at room temperature in DMF solution.