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DOI: 10.1039/A806729E (Paper) Reference Section for: J. Mater. Chem., 1998, 8, 2587-2589

Rb2Cu3CeTe5: a quaternary semiconducting compound with a two-dimensional polytelluride framework

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Rhonda Patschke, Paul Brazis, Carl R. Kannewurf and Mercouri Kanatzidis

Abstract

Rb2Cu3CeTe5 has been synthesized from the reaction of Cu and Ce in a molten alkali metal/polytelluride flux. The compound crystallizes in the monoclinic space group, C2/m (no. 12) with a=18.6884(1) Å, b=6.2384(2) Å, c=12.5264(3) Å, β=112.795(1)°, V=1346.34(5) Å3[hair space], and Z=4. Rb2Cu3CeTe5 is two-dimensional with 1/∞[Cu3CeTe5[hair space]]2– layers built from one-dimensional 1/∞ [Cu2CeTe5[hair space]]3– chains that are ‘stitched’ together by distorted tetrahedral Cu atoms; the compound is paramagnetic and a narrow-gap p-type semiconductor.

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  16. (a) Rb2Cu3CeTe5 was synthesized from a mixture of 0.448 g Rb2Te ( 3.0 mmol), 0.095 g Cu (3.0 mmol), 0.070 g Ce ( 1.0 mmol) and 0.447 g Te (7.0 mmol) which was sealed under vacuum in a carbon coated quartz tube and heated to 850 °C for 10 days. The tube was then cooled to 400 °C at 3 °C h–1, and then quenched to room temperature. The excess RbxTey flux was removed, under nitrogen atmosphere, with dimethylformamide to reveal black needle-shaped crystals in 45% yield (based on Cu). The crystals are air and water stable. Phase homogeneity was confirmed by comparing the power X-ray diffraction pattern of the product against that calculated using the crystallographically determined atomic coordinates. Microprobe analysis carried out on randomly selected crystals gave an average composition of Rb2.46Cu3.29Ce1.0Te5.55. A Siemens SMART Platform CCD diffractometer was used to collect data from a crystal of 0.160 × 0.035 ×0 .010 mm dimensions using Mo-Kα(λ= 0.71073 Å) radiation. SMART16b software was used for data acquisition and SAINT16c for data extraction and reduction. An absorption correction was performed using SADABS.16d; Crystal data at 173 K: a= 18.6884(1), b= 6.2384( 2), c= 12.5264(3)Å, β= 112.795(1)°, V= 1346.34(5)Å3, Z = 4, Dc= 5.623 g cm–3, monoclinic, space group C2/m(no. 12), µ= 25.741 mm–1, index ranges 22≤h≤20, 0≤k≤7, 0≤l≤14, 2θmax= 50°, total data 3427, unique data 1307 (Rint= 0.044), data with Fo2 >2σ(Fo2) 1087, no. of variables 60, final R/wR2 = 0.0461/0.1182, GOF 1.041. The structure was solved and refined using the SHELXTL-5 package of crystallographic programs;16e SHELXTL refines on F2. (b) SMART: 1994, Siemens Analytical Xray Systems, Inc., Madison, WI 53719 USA; (c) SAINT: Version 4, 1994–1996, Siemens Analytical Xray Systems, Inc., Madison, WI 53719 USA; (d) SADABS: G. M. Sheldrick, University of Göttingen, Germany, to be published. (e) SHELXTL: Version 5, 1994, G. M. Sheldrick, Siemens Analytical X-ray Instruments, Inc. Madison, WI 53719. Full crystallographic details, excluding structure factors, have been deposited at the Cambridge Crystallographic Data Centre (CCDC). Any request to the CCDC for this material should quote the full literature citation and the reference number 1145/124.
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