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MCM-48 mesoporous molecular sieves containing iron(III) were obtained using a direct sol−gel route followed by removal of the cetyltrimethylammonium hydroxide template before calcination. UV−visible, ESR, and XANES spectroscopies show that iron mostly occupies tetrahedral sites of the siliceous walls. The formation of oxide nanoclusters in the channels is favored in the presence of the organic template molecules during calcination.

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