. Can. J. Chem. 68, 507 (1990). WOF4.bipy was prepared from the reaction of WOF4 with 2,2'-bipyridyl (bipy) in the melt or in solution in CHzCll or CHXN.The adduct, which is not moisture-sensitive at room temperature, was characterized by elemental analysis, X-ray powder data, and vibrational spectroscopy. WOF4. bipy is almost insoluble in the usual organic solvents, and the species which were observed in CH2C12 or CH3CN by 'H NMR and Rarnan spectroscopy resulted from the dismutation of WOF4. bipy into W02F2. bipy and WF6. bipy .This transformation in solution was revealed by the slow growing of crystals identified as W02F2. bipy and by the 'H NMR spectrum which displayed lines assigned to the independently synthesized and characterized species WF6.bipy. Unlike the WOF4 adduct, the tungstyl adduct is moisture-sensitive, its crystal structure showed that the tungsten atom is surrounded by a very distorted octahedron of ligands with each nitrogen of the bipy ligand trans to one oxygen atom and the two fluorine atoms trans to each other. The space group, unit cell parameters, and R factor for CIOH8F2N202W are as follows: monoclinic, P2',, (No. 14) (alternate setting of the standard space group P2,/,), a = 8.637(1) A, b = 13.823(2) .A, c = 9.526(2) .A, P = 109.98(2)", V = 1068.8(6) .A3, Z = 4, and R = 0.044 for 806 (1 > 3u(1)) of 1471 total reflections and 94 parameters.