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A new compound K6Ti0.67Nb15.33O42 was prepared for the first time by solid state reaction in K2O-Ni2O3-Nb2O5 ternary system. The new compound was characterized by electron probe, X-ray powder diffraction and DTA. The result of X-ray powder diffraction shows that K6Ti0.67Nb15.33O42 crystallizes the hexagonal system with unit cell parameters a = 9. 1341(5) A ,c=12. 090(1)A . and space group P62/mcm(193 ).