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Updated: May 29, 2026

Experimental Approaches for the Synthesis of Low-Valent Metal-Organic Frameworks from Multitopic Phosphine Linkers
Published on: May 12, 2023
Facile synthesis of zero-, one-, and two-dimensional vanadyl pyrophosphates
Diego Solis-Ibarra1, Jared S Silvia, Vojtech Jancik
1Department of Chemistry, Massachusetts Institute of Technology, 77 Massachusetts Avenue, Cambridge, Massachusetts 02139, USA.
Abstract:
Crystallization of Na(2)VOP(2)O(7) from its aqueous solution results in formation of a one-dimensional inorganic polymer {Na(2)VO(H(2)O)P(2)O(7)·7H(2)O}(n) (1). When this polymer is dehydrated at elevated temperatures this polymer undergoes a phase transition to form the two-dimensional framework β-Na(2)VOP(2)O(7), which although previously reported had been difficult to access. Exchanging lithium for sodium via ion-exchange chromatography results in formation of a discrete, cyclic, tetramer species, Li(8)[VOP(2)O(7)(H(2)O)·4H(2)O](4) (2). Isolation of crystalline β-Li(2)VOP(2)O(7) using a dehydration procedure analogous to the one employed for the sodium derivative was unsuccessful. In contrast, we show that β-K(2)VOP(2)O(7) can be obtained from the amorphous phase K(2)VOP(2)O(7)·nH(2)O (n = 0-7) upon thermal dehydration.
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