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Polyoxoanions have enormous potential as drug delivery hosts, as catalysts, as agents for sequestering nuclear waste heavy metals, and as luminescent materials for laser and optical devices applications. We report the encapsulation of the polyoxoanion [Eu(H₂O)₃(α-1- P₂W₁₇O₆₁)]^7- within Mobil crystalline material (MCM)-41. For proper host−guest interaction, it was necessary to functionalize the surface walls of MCM-41 through use of a silylation reagent, specifically, (aminopropyl)triethoxysilane. A stable and integrated [Eu(H₂O)₃(α-1-P₂W₁₇O₆₁)]^7- polyoxoanion was shown to be formed inside the channels of modified MCM-41. X-ray diffraction, ²⁹Si magic angle spinning (MAS) NMR, UV−vis absorption, emission and excitation spectra, and Raman scattering measurements have been used to structurally characterize the various products. Cross-polarization ²⁹Si MAS NMR has been shown to better reveal …