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Park, Sohyun; Liu, H.; Kleinsorge, M.; Grey, Clare P.; Toby, Brian H.; Parise, John B. (2004): [Li-Si-O]-MFI: A new microporous lithosilicate with the MFI topology. In: Chemistry of Materials, Vol. 16, No. 13: pp. 2605-2614
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We report the synthesis and structure solution of [Li-Si-O]-MFI (a = 19.793(4) Å, b = 19.766(4) Å, c = 13.266(3) Å, space group P2 12 12 1), a framework zeolite related to ZSM-5 (silicalite) with a Li/Si ratio of 4:92. Single-crystal synchrotron X-ray diffraction data, 29Si NMR, and infrared spectroscopy indicate that the Li is randomly distributed over the framework sites. In addition, Li occupies ordered positions on extraframework sites that are occluded in voids outlined by the double five- or six-membered rings. The strong interaction between the extraframework Li cations and the negatively charged framework may be responsible for the distortion of the lattice from Pnma, the usual symmetry associated with as-synthesized members of the MFI-family, to its subgroup symmetry P2 12 12 1. Variable-temperature 7Li and 1H MAS NMR experiments show that the extraframework Li cations are not directly accessible to gas molecules, but that the protons formed on calcination are accessible.