Zeitschrift fiir Kristallographie - New Crystal Structures 213
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© by R. Oldenbourg Verlag, München 1998
Crystal structure of potassium selenìdoantìmonate(III), K2Sb4Se8
W . S. Sheldrick and M . W a c h h o l d
Ruhr-Universität Bochum. Lehrstuhl für Analytische Chemie, Universitätsslraße 150, D-44780 Bochum. Germany
Received March .3. 1997. transferred to 1st update of database ICSD in 1998. CSD-No. 402886
It is isostructural with Cs2Sb4Se8 and Cs2Sb4S8 (see refs. 2, 3).
The structure is built up of condensed SbSes^-pyramids to form a one dimensional [Sb4Se6]-chain with 3- and 4-fold coordinated Sb-atoins. These chains are linked by Se2^~ bridging ligands to form sheets with large SbeSes 14-membered rings parallel to the (101) crystallographic plane. Due to long Sb•••Se interactions between the sheets, each Sb atom possesses a distorted square pyramidal (ψ-octahedral) coordination. The К ions between the sheets exhibit an irregular 10-fold coordination sphere.
Table 1. Parameters used for the X-ray data collection
Source of material: The title compound (see ref. 1) was prepared by reaction of K2CO3 ( 145 mg, 1.05 nmiol) with SbaSes (386 mg, 0.80 mmol) and Se (91 mg, 1.15 mmol) in 0.55 m! methanol in a closed glass tube at 4 7 3 К for 30 h.
K2Sb4Se8, tricUnic, PT (No. 2), a =6.373(1) Л, b =7.046(1) Â, с =^9.554(2) К OL =81.54(3)°, β =85.03(3)°, γ =74.02(3)°, V=407.5 Â^, Z=l,R(F) =0.044,Λν/Ο =0.078.
Table 2. Final atomic coordinates and displacement parameters (in Â^)
Crystal: shiny black, rectangular blocks.
size 0.40 X 0.46 χ 0.55 mm Wavelength: Mo Ka radiation (0.71073 À)
μ: 249.00 cm-'
Diffiractometer: Siemens P4
Scan mode: ω
Tmeasurenuru'· 294 К 50°
ЩНкОипцие: 1427
Criterion for /0: /ο>2σ(/ο) N(param)r^„td·. 65
Programs: SHELXS-86. SHELXL-93
Atom Site X У г í/ll U22 Un t/12 Uli Un
Sb(l) 2/ 0.1612(2) 0.1818(2) 0.0515(1) 0.0241(6) 0.0219(5) 0.0262(5) -0.0086(5) 0.0009(4) -0.0013(4) Sb{2) 2/ 0.4464(2) 0.5962(1) 0.1709(1) 0.0218(6) 0.0221(5) 0.0202(5) -0.0074(5) 0.0020(4) -0.0044(4) Se(l) 2/ 0.0869(3) 0.4910(2) 0.2177(2) 0.024(1) 0.0241(8) 0.0276(8) -0.0083(7) 0.0000(7) -0.0068(6) Se(2) 2Í 0.6111(3) 0.4012(2) 0.4155(2) 0.024(1) 0.0313(9) 0.0221(8) -0.0009(8) -0.0018(7) -0.0001(6) Se(3) 2i 0.6817(3) 0.0693(2) 0.7208(2) 0.029(1) 0.0209(8) 0.0242(8) -0.0035(7) -0.0073(7) -0.0051(6) Se(4) 2i 0.7755(3) 0.1472(2) 0.1206(2) 0.0212(9) 0.0238(8) 0.0249(8) -0.0049(7) -0.0012(7) -0.0061(6) K(l) 2i 0.1779(7) 0.1866(6) 0.5631(4) 0.036(3) 0.042(2) 0.036(2) -0.009(2) -0.001(2) -0.013(2)
References
1. Wachhold, M.: Methanolothermale Darstellung und Strukturchemie von (Poly-)Chalkogenidometallaten der Gruppen IS und 16. Dissertation, Ruhr-Universität Bochum, Germany 1997.
2. Sheldrick, W. S.; Kaub, J.: Darstellung und Kristallstruktur von CsSb2Se4.
Z. Anorg. Allg. Cham. 536 (1986) 114-118.
4.
5.
3. McCarthy, T. J.; Kanatzidis M. G.: Polysulfide Ligands in Solid-Stale Antimony Compounds. Isolation and Structural Characterization of Cs2Sb4S8 and CsSbSô. Inorg. Chem. 33 (1994) 1205-1211.
Sheldrick, G. M.: Phase AnneaUng in SHELX-90: Direct Methods for Large Structures. Acta CrystaUogr. A4Í (1990) 467-473.
Sheldrick, G. M.: SHELXL-93, a program for refining crystal structures.
University of Göttingen, Germany 1993.
