The reaction of (NH4)2HPO4 with (NH4)2Na2K2V10O28, followed by addition of Me3NHCl, yields dark crystals of the phosphovanadate cluster (Me3NH)4(NH4)[H4PV14O42]. The structure consists of an α-Keggin framework capped by two [VO] subunits. The protonation sites were identified as the doubly-bridging oxygens, O10. Crystal data: orthorhombic space group Fddd, a=10.706(2), b=23.581(4), c=37.271(8) Å, V=9409.3(22) Å3, Z=8. X-ray data were collected on a Siemens R3m/V diffractometer using a θ/2θ scan technique with graphite monochromated MoKα radiation. A total of 2733 reflections was collected (to 2θ=55°), of which 1850 were used in subsequent structure solution and refinement (I>3σ(I)). The structure was solved by direct methods, and least-squares refinement converged at R=0.033.
ASJC Scopus subject areas
- Physical and Theoretical Chemistry
- Inorganic Chemistry
- Materials Chemistry