Journal
EUROPEAN JOURNAL OF INORGANIC CHEMISTRY
Volume -, Issue 17, Pages 2455-2458Publisher
WILEY-V C H VERLAG GMBH
DOI: 10.1002/ejic.200801073
Keywords
Clathrates; Cage compounds; Zintl anions; Oxidation; Ionic liquids
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Funding
- National Science Foundation [CHE-0616805]
- Robert A. Welch Foundation
- Max-Planck-Gesellschaft
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The new clathrate-II K8.6(4)Ge136 has been synthesized by mild oxidation of K4Ge9 in the ionic liquid n-dodecyltrimethylammonium chloride (DTAC)/AlCl3 at 300 degrees C and subsequent annealing at 370 degrees C. Refinement of the crystal structure from X-ray powder diffraction data revealed the composition K8.6(4)Ge136 [space group Fd (3) over barm, a = 15.302(1) angstrom], which was also confirmed by energy-dispersive X-ray spectrometry (EDXS), transmission electron microscopy, and scanning electron microscopy on the bulk material. K, atoms preferably occupy the larger Ge-28 cages rather than the Ge-20 cages in the clathrate-II structure. K8.6(4)Ge136 is metastable and was found to decompose exothermically at 471 degrees C. ((C) Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2009)
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