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The crystal structure of three compositions of matter has been determined to be iso-structural with FeB ortho-rhombic (space group Pnma). The crystalline structures are: Ti0.5Ta0.5B, Zr0.5Ta0.5B and Hf0.5Ta0.5B. A process for preparing ceramics is disclosed. Molded ceramics including the compositions of matter are useful for applications such as rocket nozzles, leading edges on hypersonic missiles, engine parts and other applications requiring a structural component to operate at temperatures of 1600° C. to 2400° C.