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Preparation of Preyssler-type Phosphotungstate with One Central Potassium Cation and Potassium Cation Migration into the Preyssler Molecule to form Di-Potassium-Encapsulated Derivative.


ABSTRACT: A mono-potassium cation-encapsulated Preyssler-type phosphotungstate, [P5W30O110K]14- (1), was prepared as a potassium salt, K14[P5W30O110K] (1a), by heating mono-bismuth- or mono-calcium-encapsulated Preyssler-type phosphotungstates (K12[P5W30O110Bi(H2O)] or K13[P5W30O110Ca(H2O)]) in acetate buffer. Characterization of the potassium salt 1a by single-crystal X-ray structure analysis, 31P and 183W nuclear magnetic resonance (NMR) spectroscopy, Fourier transform infrared spectroscopy, high-resolution electrospray ionization mass spectroscopy, and elemental analysis revealed that one potassium cation is encapsulated in the central cavity of the Preyssler-type phosphotungstate molecule with a formal D 5h symmetry. Density functional theory calculations have confirmed that the potassium cation prefers the central position of the cavity over a side position, in which no water molecules are coordinated to the encapsulated potassium cation. 31P NMR and cyclic voltammetry analyses revealed the rapid protonation-deprotonation of the oxygens in the cavity compared to that of other Preyssler-type compounds. Heating of 1a in the solid state afforded a di-K+-encapsulated compound, K13[P5W30O110K2] (2a), indicating that a potassium counter-cation is introduced in one of the side cavities, concomitantly displacing the internal potassium ion from the center to a second side cavity, thus providing a new method to encapsulate an additional cation in Preyssler compounds.

SUBMITTER: Hayashi A 

PROVIDER: S-EPMC6641389 | biostudies-literature | 2018 Feb

REPOSITORIES: biostudies-literature

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Preparation of Preyssler-type Phosphotungstate with One Central Potassium Cation and Potassium Cation Migration into the Preyssler Molecule to form Di-Potassium-Encapsulated Derivative.

Hayashi Akio A   Wihadi Muh Nur Khoiru MNK   Ota Hiromi H   López Xavier X   Ichihashi Katsuya K   Nishihara Sadafumi S   Inoue Katsuya K   Tsunoji Nao N   Sano Tsuneji T   Sadakane Masahiro M  

ACS omega 20180227 2


A mono-potassium cation-encapsulated Preyssler-type phosphotungstate, [P<sub>5</sub>W<sub>30</sub>O<sub>110</sub>K]<sup>14-</sup> (<b>1</b>), was prepared as a potassium salt, K<sub>14</sub>[P<sub>5</sub>W<sub>30</sub>O<sub>110</sub>K] (<b>1a</b>), by heating mono-bismuth- or mono-calcium-encapsulated Preyssler-type phosphotungstates (K<sub>12</sub>[P<sub>5</sub>W<sub>30</sub>O<sub>110</sub>Bi(H<sub>2</sub>O)] or K<sub>13</sub>[P<sub>5</sub>W<sub>30</sub>O<sub>110</sub>Ca(H<sub>2</sub>O)]) in ac  ...[more]

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