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LiYbF4 is Zircon-like structured and crystallizes in the tetragonal I4_1/a space group. The structure is three-dimensional. Li1+ is bonded in a 4-coordinate geometry to four equivalent F1- atoms. All Li–F bond lengths are 1.94 Å. Yb3+ is bonded in a 8-coordinate geometry to eight equivalent F1- atoms. All Yb–F bond lengths are 2.30 Å. F1- is bonded in a 3-coordinate geometry to one Li1+ and two equivalent Yb3+ atoms.
LiYbF2 crystallizes in the tetragonal I4_1/amd space group. The structure is three-dimensional. Li is bonded in a square co-planar geometry to four equivalent F atoms. All Li–F bond lengths are 2.47 Å. Yb is bonded to six equivalent F atoms to form distorted edge-sharing YbF6 octahedra. There are four shorter (2.29 Å) and two longer (2.33 Å) Yb–F bond lengths. F is bonded to two equivalent Li and three equivalent Yb atoms to form a mixture of distorted edge and corner-sharing FLi2Yb3 trigonal bipyramids.