Crystals of Li 2 [(UO 2 )(MoO 4 ) 2 ] have been synthesized by solid-state reaction of Li 2 CO 3 , UO 3 and MoO 3 . The crystal structure of the compound (triclinic, P1, a=5.3455(4), b=5.8297(4), c=8.2652(6) Å, α=108.267(2), β=100.566(2), γ=104.121(2) o , V=227.56(3) Å 3 , Z=1) has been solved by direct methods and refined to R 1 =0.027 (wR 2 =0.047). The structure is based upon chains of composition [(UO 2 )(MoO 4 ) 2 ] 2 - composed of UrO 4 square bipyramids that share corners with MoO 4 tetrahedra. The chains are parallel to the a axis and are linked into a three-dimensional framework by Li + cations in trigonal bipyramidal coordination. The LiO 5 trigonal bipyramids form edge-sharing chains parallel to the a axis.