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A strategy for in situ fabrication of nanoscale-thin layers of anatase TiO2 coated on the metal-organic framework (MOF) material, MIL-53(AI), is developed. The preparation conditions for crystallized TiO2 are normally incompatible with the thermal and chemical stability of MOFs. Based on our strategy, we found that the redundant organic ligands (1,4-benzenedicarboxylic acid, H2BDC) within the pores of the as-synthesized MOF play a key function in the protection and support of the framework during hydrother- mal loading of the TiO, precursor, as well as in preventing the infiltration of the precursor into the pores. After annealing, a nanoscale-thin layer of highly crystalline anatase Ti02, with a thickness of 6-10 nm, was successfully attached to the external surface of the MIL-53(AI) crystals, while the porous framework remains intact. The core-shell structure of the MOF@TiO2 nanocomposite endows the resulting materials with additional optical response and enhanced moisture and chemical stability.