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New intercalation compounds with Cu2+ ions in the interlayer of layered perovskite oxides, OA1-xCa2-xLaxNb3O10 (OA = n-octylammonium ion, 0 ≤ x < 1), have been prepared by ion-exchange reaction, and characterized by means of XRD and XAS. For the detail elucidation of the fine structure of the Cu K-edge XANES spectra, polarized XAS was applied for the [Cu(en)2]2+ and Cu2+ ions intercalated to the single crystal. According to the XANES and EXAFS spectra measured at Cu K-edge, copper ions are four-coordinated. In addition, XANES spectra have shown that the charge transfer from host layer to intercalated ions influences on the chemical state of copper ion.

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