A new lithium copper bismuth oxide, LiCuBiO4 was prepared by hydrothermal reaction using NaBiO30.1*4H2O. The crystal structural model of this compound was refined by using synchrotron X-ray powder diffraction data. This bismuthate has the LiCuSbO4 related structure with the orthorhombic cell (Space group: Pnma) of a=10.9096(9), b=5.8113(5) and c=5.0073(4) Å, and the final R-factors were Rwp=4.84 and Rp=3.58%. This compound is the first example of a lithium copper bismuthate containing Bi5+. An antiferromagnetic ordering of Cu2+ moment was observed at 6 K.
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