The new MoVI complex [Mo(O) (μ-O) (SAE)]2 was prepared and characterized by means of spectroscopic (i.r.,1Hn.m.r.) and crystallographic measurements. Crystals of the [Mo(C9H8NO2)(H2O)]2, M=582.3, orthorhombic, space group Pbca,a=13.108(4),b=8.982(2),c=16.842(4) A, v=1982.9 A3, z=4, Dm=1.93(2), Dc=1.95 g cm−3, MoKα γ=0.71069 A, μ=1.3 mm−1, F(000)=1152, T=295K, R=0.035 for 2413 reflections. The crystal structure consists of [Mo(O)(μ-O)(L)]2, in dimeric units. The coordination geometry around each molybdenum atom is distorted octahedral with Mo−O (terminal) and Mo−O (bridge) distances of 1.694(3) and 1.760(3) A, respectively, and with the angle O(1)−Mo−O(2) of 105.6(1)o, typical for manycis-dioxocomplexes of MoVI. The asymmetric bridge is characterized by the following parameters: Mo−O(2)i and Mo−Moi distances equal 2.408(3) and 3.319(3) A, respectively, and the Mo−O(2)−Moi and O(2)−Mo−O(2)i angles equal 104.5(1)o and 75.5(1)o, respectively. The i. r. and Raman spectra of molybdenum complexes with an asymmetric double oxygen bridge display a strong absorption the 800–850 cm−1 range.