Journal
INORGANIC CHEMISTRY
Volume 55, Issue 21, Pages 11583-11592Publisher
AMER CHEMICAL SOC
DOI: 10.1021/acs.inorgchem.6b02116
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Funding
- Ministry of Education, Culture, Sports, and Science, Japan [26420787]
- Spanish Ministry of Science and Innovation (MICINN) [CTQ2014-52774-P]
- DGR of the Generalitat de Catalunya [2014SGR199]
- XRQTC
- JSPS KAKENHI [JP16K06863]
- A-STEP program of the Japanese Science and Technology Agency (JST)
- Furukawa Foundation for Promotion of Technology
- Grants-in-Aid for Scientific Research [26420787, 16K06863, 15H06425] Funding Source: KAKEN
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Dipotassium cation (K+)-encapsulated Preyssler-type phosphotungstate, [P5W30O110K2](13-), was prepared by heating monobismuth (Bi3+)-encapsulated Preyssler-type phosphotungstate, [P5W30O110Bi-(H2O)](12-), in acetate buffer in the presence of an excess amount of potassium cations. Characterization of the isolated potassium salt, K-13[P5W30O110K2] (1a), and its acid form, H-13[P5W30O110K2] (1b), by single crystal X-ray structure analysis, P-31 and W-183 nuclear magnetic resonance (NMR), Fourier transform infrared (FT-IR) spectroscopy, cyclic voltammetry (CV), high-resolution electrospray ionization mass spectroscopy (HR-ESI-MS), and elemental analysis revealed that two potassium cations are encapsulated in the Preyssler-type phosphotungstate molecule with formal D-5h symmetry, which is the first example of a Preyssler-type compound with two encapsulated cations. Incorporation of two potassium cations enhances the thermal stability of the potassium salt, and the acid form shows catalytic activity for hydration of ethyl acetate. Packing of the Preyssler-type molecules was observed by high resolution high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM).
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