Order-disorder in the super-sodalite Zn3Al6(PO4)12, 4tren, 17H2O (MIL-74): a combined XRD-NMR assessment

Journal of the American Chemical Society
Lionel BeitoneGérard Férey

Abstract

A new mixed zinc-aluminum phosphate Zn(3)Al(6)(PO(4))(12), 4tren, 17H(2)O (MIL-74) has been hydrothermally synthesized with the tris(2-aminoethyl)amine (tren) as a structure-directing agent (453 K, 36 h, autogenous pressure). The solid was characterized by a nonclassical method combining single-crystal X-ray diffraction and several solid-state NMR experiments, RFDR, C7 double quantum ((31)P), and 3QMAS ((27)Al). Its crystal structure is cubic, a = 16.7942(1) A, but the choice of the space group does not follow usual routes of structure determination, due to some "disorder" between Zn and Al. It can be assigned as well to I-43m or to P-43n. The open-framework is built up from an enneameric unit (T = Zn, Al) containing five TO(4) and four PO(4) tetrahedra (one of the P-O bonds is terminal). A central TO(4) tetrahedral unit shares all of the corners with four phosphates groups. Two phosphate groups are connected to two other peripheral TO(4) units. It results in the formation of a "pseudo" planar building block T(5)P(4) consisting of four square 4-rings. The connection of the T(5)P(4) units generates a three-dimensional framework, which defines a super-sodalite topology. The resulting cavities (diameter of 10 A) are bound by 12-ri...Continue Reading

References

Jan 1, 1995·Acta Crystallographica. Section A, Foundations of Crystallography·R H Blessing
Dec 14, 2001·Journal of the American Chemical Society·J PlévertM O'Keeffe
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Citations

Sep 10, 2013·Solid State Nuclear Magnetic Resonance·Charlotte MartineauFrancis Taulelle
Apr 11, 2012·Dalton Transactions : an International Journal of Inorganic Chemistry·Charlotte MartineauKarim Adil
Apr 3, 2020·Chemical Society Reviews·Eric BreynaertJohan A Martens
Jan 17, 2008·Chemical Society Reviews·Gérard Férey
Jun 2, 2016·Progress in Nuclear Magnetic Resonance Spectroscopy·Mohamed HaouasCharlotte Martineau
Oct 9, 2014·Journal of the American Chemical Society·Sharon E Ashbrook, Scott Sneddon
Jan 18, 2005·Inorganic Chemistry·Chia-Her Lin, Sue-Lein Wang
Sep 15, 2005·Journal of the American Chemical Society·Yueh-Chun LiaoSue-Lein Wang

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