Single crystals of CuTa 2O 6 have been synthesized in a CuOCu 2O flux. X-ray investigations show that this compound has an orthorhombic pseudocubic symmetry and crystallizes with 4 molecules per unit cell in the space group Pmmm. The cell parameters are: a = 7.5228(9) Å, b = 7.5248(9) Å, and c = 7.5199(9) Å. The structure as determined from single crystal X-ray diffraction data is a defective perovskite-like structure. The Ta 5+ cations occupy the octahedral B sites of the ideal perovskite structure (the mean TaO distance is 1.985 Å), while the Cu 2+ cations partially occupy the A sites. Three Cu 2+ cations are located in the middle of the cubic edges while the fourth is statistically distributed over the three face centers. The twelve oxygen atoms around the copper cations are arranged as three mutually perpendicular squares of different size. The three sets of the CuO distances are 2.027, 2.763, and 3.293 Å. Electronic scattering chemical analysis and cation charge calculations according Zachariasen's method reveal the presence of Cu + cations over all the Cu sites. This reduction gives rise to a stoichiometric range for this compound. The structure refinement shows that the chemical formula of the studied crystal is about Cu 1.03Ta 2O 6.