The compound Th₁₃Te₂₄O₇₄ was prepared by three independent methods, namely, thermal decomposition of ThTe₂O₆ in oxygen and argon and direct solid-state reaction of ThO₂ and TeO₂.The X-ray powder diffraction patterns of the three products, by and large, are similar, except for some differences in intensities and extra diffraction lines. The thermal decomposition of ThTe₂O₆ was carried out in the streams of oxygen and argon by thermogravimetry at a heating rate of 5 K/min in the temperature range of 725– 840^° C. The solid-state reaction of ThO₂ and TeO₂(13:24)!was carried out in a sealed ampoule at 700^° C. The measured density of this compound is 8.23 g/cm 3.An orthorhombic lattice with unit cell parameters, a=11.310± 0.005 Å , b= 14.064±0.006 Å , c=9.056±0.004 Å ,and volume of 1440.419±1.088 ( Å )³ was determined for this compound