The crystal structure and dielectric properties of wet-chemically prepared Ca2YbNbO6 ceramics have been investigated. It is difficult to obtain a single phase of Ca2YbNbO6 by conventional solid state reaction with the appropriate oxides or carbonates. In this work, it was prepared by the wet-chemical method with Ca- and Yb-nitrates, Nb-chloride and citric acid. We obtained a single phase powder by heat treatment at 1000 degrees C for 10 hrs. X-ray diffraction results show that Ca2YbNbO6 has an orthorhombic structure (a(0) = 0.556 nm, b(0) = 0.575 nm, c(0) = 0.800 nm), which is based on the B-site ordered perovskite structure. Investigation of the crystal structure and dielectric properties as a function of temperature showed no structural phase change.