Osmium Osmium I 8100 Functionalized Heteropolyanions: High-Valent Metal Nitrido Fragments Incorporated into a Keggin Polyoxometalate Structure. -Three new nitrido-functionalized polyoxotungstates are synthesized which feature the incorporation of [Os VI ≡N] 3+ (III), [Re VI ≡N] 3+ (V), and [Re VII ≡N] 4+ fragments into the framework of a Keggin-type heteropolyanion. Compound (III) is characterized by 15 N, 31 P, and 183 W NMR and for (V) results obtained by EPR spectroscopy (confirming the paramagnetic character), cyclic voltammetry, and single crystal XRD (cubic, space group Im3m) are briefly reported. -(KWEN, H.; TOMLINSON, S.; MAATTA*, E. A.; DABLEMONT, C.; THOUVENOT, R.; PROUST, A.; GOUZERH, P.; Chem.
The solubility of the corn protein zein is measured gravimetrically from 30 to 60 °C in seven imidazolium-based ionic liquids and three conventional solvents, acetic acid, 70 vol % aqueous ethanol, and 1-methylimidazole. At elevated temperatures the solubility of zein in six of the ionic liquids exceeds that of the current industry standard, 70 vol % aqueous ethanol. The ionic liquids 1-methylimidazolium acetate and 1-ethyl-3-methylimidazolium dicyanamide can dissolve 2.5 times more zein at 60 °C than 70 vol % aqueous ethanol. Single and multivariate regressions are used to model zein's solubility as a function of common solvent properties. Solvents able to dissolve more zein have small molecular volumes, low polarities, and act as a weak hydrogen bond acceptors.
Three examples of nitrido-functionalized polyoxometalate species are reported, namely (n-Bu4N)4[PW11O39(OsN)] (1), (n-Bu4N)4[PW11O39(ReN)] (2), and (n-Bu4N)3[PW11O39(ReN)] (3), which feature the incorporation of [OsVI identical to N]3+, [ReVI identical to N]3+ and [ReVII identical to N]4+ fragments, respectively, into the framework of a Keggin-type heteropolyanion.
Infrared spectroscopy is known to be a useful tool for identifying local structure changes in zeolites. Infrared spectroscopy is often employed to complement X-ray diffraction data. Local structure changes in zeolite CIT-6 and its zeolite beta (*BEA) analogs caused by calcination, altering framework composition, and ion exchange have been identified with mid- and far-infrared spectroscopy. Differences in the local structures of the samples were observed in mid- and far-infrared spectra, including changes in the intratetrahedral asymmetric stretch, the double-ring mode, and the intratetrahedral bending mode regions. The infrared spectra indicate that calcination or acetic acid extraction changed the structure of CIT-6 to that of zeolite beta (*BEA). Zinc ion exchange or the substitution of aluminum into the framework structure of acetic acid extracted samples retained the CIT-6 structure.
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