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• W2054821607 abstract "Cs4SeeSi2, monoclinic, C12/ml (no. 12), a = 15.148(3) A, b = 7.599(1) k,c= 10.057(2) k,s= 121.833(2)°, V= 983.5 A, Ζ = 2, AgtfFJ = 0.028, wRretfF) = 0.068, T= 298 K. Source of material Crystals of Cs4Si2Seg were serendipitously formed in a molten chalcogenide reaction of 51.5 mg U, 21.8 mg Si, 94.0 mg Se, and 40.6 mg Cs2Se2. The reactants were combined in a fused silica ampoule in an inert atmosphere glovebox, sealed under vacuum, and heated to 725 °C at a rate of 35 K/hour. After 200 hours of heating, the ampoule was cooled at 3 K/hour to room temperature. Dimethylformamide was added to dissolve remaining cesium selenide flux, resulting in well-formed clear block-like crystals of Cs4Si2Ses together with CsU2Se6 [1]. The same reaction without lead to Cs4Si2See as identified by unit cell. Discussion This compound is isostnictural to Cs4Ge2Ses [2], The structure consists two tetrahedra of SiSe4 bound by two Se-Se bonds to form a ring complex anion [Si2Seg] surrounded by Cs cations. Table 1. Data collection and handling. Crystal: transparent colorless block, size 0.10x0.15x0.15 mm Wavelength: Mo Ka radiation (0.71073 A) 147.78 cm -1 Diffractometer, scan mode: Bruker SMART CCD, φ/ω 2l?niax: 46.5° Nfhldhnosma, N(hkl)umque· 3106,772 Criterion for / 0 N ( h k l ) p . /obs>2cr(/obs), 720 N(param)nftati'· 40 Program: SHELXTL [3] Table 2. Atomic coordinates and displacement parameters (in A). Atom Site χ y ζ U U22 i/33 U12 Un Un Cs(l) 4i 0.41163(5) 0 0.14620(8) 0.0321(4) 0.0352(4) 0.0277(4) 0 0.0150(3) 0 Cs(2) 4i 0.15960(5) 0 0.28145(8) 0.0325(4) 0.0347(4) 0.0330(4) 0 0.0201(3) 0 Se(l) 4/ 0.31214(8) 0 -0.2684(1) 0.0237(6) 0.0399(7) 0.0328(7) 0 0.0160(5) 0 Se(2) 4/ 0.12580(8) 0 -0.1108(1) 0.0296(6) 0.0365(6) 0.0247(6) 0 0.0169(5) 0 Se(3) 8; 0.08779(6) 0.24308(8) -0.46476(9) 0.0267(4) 0.0229(5) 0.0281(5) -0.0026(3) 0.0150(4) 0.0008(3) Si(l) 4i 0.1553(2) 0 -0.3018(3) 0.023(1) 0.022(1) 0.022(2) 0 0.012(1) 0 Acknowledgments. This research was funded by the Department of Energy (grant no. DE-FG03-OZER15351). The authors acknowledge S. M. Miller for assistance in crystallographic topics. References 1. Chan, B. C.; Hulvey, Z.; Abney, K. D.; Dorhout, P. K.: Synthesis and Characterization of AlhSe« (A = Cs, K). Inorg. Chem. 43 (2004) 2453- 2455. 2. Sheldrick, W. S.; Schaaf, B.: Preparation and crystal structure of the ce- sium selenidogermanates(IV) Cs4Ge4Seio · 2CH3OH and Cs4Ge2See· Z. Naturforsch. 49b (1994) 655-659. 3. Sheldrick, G. M.: SHELXTL. Structure Determination Software Suite. V. 6.10. Bruker AXS, Madison, Wisconsin, USA 2000. * Correspondence author (e-mail: pkd@lamar.colostate.edu ) Unauthenticated Download Date | 3/9/16 9:59 AM" @default.
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• W2054821607 date "2005-04-01" @default.
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• W2054821607 title "Crystal structure of tetracesium octaselenidodisilicate, Cs4Si2Se8" @default.
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