Abstract
Three original hexavanadate-based materials (DIEA)2[V6O13{(OCH2)3CNHCOC6H4X−p)}2] (X=Cl, Br, I) have been synthesized via the amidation of H2[V6O13{(OCH2)3CNH2}2] and p-halogenated benzoic acid. The components and structures of the products were determined by FT-IR, 1H NMR, ESI-MS, XPS and single-crystal X-ray diffraction. The molecular structures of three compounds are similar: a Lindqvist-type cluster {V6O19} covalently links to two halogenated benzoyl trialkoxyl ligands. However, they exhibit diverse packing manners because of their difference in hydrogen-bonding interactions. The anions [V6O13{(OCH2)3CNHCOC6H4Cl−p)}2]2- are arranged in a 1D chain structure by intermolecular hydrogen-bonding interactions, while the other two compounds show a 2D “sandwich biscuit” layered packing structure without hydrogen bonds between the anions. Moreover, when choosing a condensing agent to increase the yield, PyBOP has an overwhelming advantage over common EDCI/HOBt. This article also discusses the reaction mechanism in detail, and provides experimental guidance for the rational design of POM-based organic-inorganic hybrids.
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