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DOI: 10.1039/A902530H (Paper) Reference Section for: J. Chem. Soc., Dalton Trans., 1999, 1531-1532

Synthesis and characterization of K3Cu11Te16 from supercritical ethylenediamine

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Mehtap Emirdag, George L. Schimek and Joseph W. Kolis

Abstract

Reaction of copper with potassium polytelluride, K2Te5, in supercritical ethylenediamine (305 °C, 2370 psi) led to a new compound with building blocks formed from Cu8Te12 pentagonal dodecahedral cages made with Cu2Te3 pentagons; the dodecahedrons are connected by copper atoms and tritelluride fragments to generate tunnels filled with potassium.

References

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  11. The synthesis of K3Cu11Te16 was achieved by combining 30 mg Cu powder (0.47 mmol), 52 mg K2Te5(0.072 mmol), and 44 mg Te powder (0.34 mmol) in 0.7 ml of ethylenediamine (en) in a ¼ inch quartz tube. The tube was sealed under vacuum and placed in a high-pressure autoclave. The autoclave was counter-pressured to 2370 psi, placed in a furnace, and heated at 305 °C for one day. Tubes were opened under argon and washed with ethylenediamine and tetrahydrofuran using standard Schlenk techniques. After the crystals were dried under vacuum, they were placed in mineral oil. Shiny black column crystals were recovered with over 90% yield. They are extremely air sensitive.
  12. Crystal data for K3Cu11Te16. The single crystal X-ray diffraction data for the title compound were collected at room temperature on a four circle Rigaku AFC7R diffractometer (Mo-Kα= 0.71073 Å, graphite monochromator). The unit cell was based on the indexing of 25 reflections with a 2θ range of 36.89–44.32°. Three standard reflections were measured every 100 reflections with decay =–1.6%. 2θmax= 50°, M= 2857.90, gray column, 0.064 × 0.064 × 0.034 mm. Orthorhombic Imma, Z= 4, a= 23.642(3), b= 19.577(2), c= 6.958(2)Å, V= 3220.5(9)Å3, Dc= 5.89 g cm–3, µ(Mo-Kα)= 21.701 mm–1. Refinement on F, 1255 observed reflections [I > 3σ(I)], 80 parameters (all atoms anisotropic), R= 0.031, Rw= 0.037, S= 2.59, maximum and minimum residual electron density: 1.28 and –1.01 e Å–3. The structure was solved with direct methods and refinned by full matrix least-square techniques explained as in previous work.1 CCDC reference number 186/1408.
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