NaFeMnO ( = 1 and 2/3) layered oxides were prepared by an improved solid-state synthesis method. The XRD analysis confirmed the high purity of these samples. The Rietveld refinement of the crystalline structure illustrated that the prepared materials crystallize in a hexagonal system in the space group with the P3 structure for = 1 and in a rhombohedral system with the 6/ space group and P2 structure type for = 2/3.
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