24
Zeitschrift für Kristallographie - New Crystal Structures 213© by R. Oldenbourg Verlag, München 1998
Crystal structure of rubidium selenìdoantimonate(III), Rb2Sb4Seg
W. S. Sheldrick and M. Wachhold
Ruhr-Universität Bochum, Lehrstuhl für Analytische Chemie, Universitatssu-aße 150, D-44780 Bochum, Germany Received March 3, 1997, u^sferred to 1st update of database ICSD in 1998, CSD-No. 402887
Source of material: The title compotmd (see ref. 1) was prepared by reaction of КЬгСОз (278 mg, 1.20 mmol) with ЗЬгЗез (393 mg, 0.82 mmol) and Se (136 mg, 1.72 mmol) in 0.55 ml methanol in a closed glass tube at 468 К for 24h.
Rb2Sb4Se8, triclinic, PT (No. 2), a =6.443(1 ) Â, b =7.075(1) Â, с =9.677(2) Â, α =81.02(3)°, β =85.73(3)°, γ=74.47(3)°, V=419.6 Â^
Ζ=1, ЩР) =0.065, Л =0.167.
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-atoms. These chains are linked by Se2^" bridging ligands to fomi sheets with large SbeSeg 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-octa- hedral) coordination. The Rb ions between the sheets exhibit an irregular 10-fold coordination sphere.
Table 1. Parameters used for the X-ray data collection Crystal: shiny black, rectangular blocks.
size 0.28 X 0.40 χ 0.42 mm Wavelength: Mo Ka radiation (0.71073 Â)
μ: 294.50 cm-'
Dif&actometer: Siemens P4
Scan mode: ω
'^measuremem- 294 К
гОтах: 50°
ЩМсОипщи^·. 1439
Criterion for lo. /ο>2σ(/ο)
N(param)r^«rf: 65
Programs: SHELXS-86, SHELXL-93
Table 2. Final atomic coordinates and displacement parameters (in A^)
Atom Site χ У ζ ί/π Un ί/зз Un Un Uli
Rb(l) 2/ 0.1741(3) 0.1821(3) 0.5619(2) 0.0275(9) 0.035(1) 0.028(1) -0.0095(7) 0.0003(7) -0.0063(7) Sb(l) 2Í 0.1612(2) 0.1820(2) 0.0461(1) 0.0220(7) 0.0223(7) 0.0231(7) -0.0093(5) 0.0006(4) 0.0010(4) Sb(2) li 0.4421(2) 0.5958(2) 0.1693(1) 0.0210(6) 0.0206(6) 0.0191(6) -0.0072(4) 0.0016(4) -0.0018(4) Se(l) 2i 0.0899(2) 0.4861(2) 0.2138(2) 0.0223(9) 0.0226(9) 0.0227(9) -0.0094(6) -0.0003(6) -0.0032(6) Se(2) li 0.6091(2) 0.4053(2) 0.4160(2) 0.0197(8) 0.0280(9) 0.0204(9) -0.0025(6) -0.0013(6) 0.0029(6) Se(3) li 0.6760(2) 0.0701(2) 0.7292(2) 0.0236(9) 0.0189(8) 0.0246(9) -0.0040(6) -0.0062(6) -0.0015(6) Se(4) li 0.7805(2) 0.1494(2) 0.1156(2) 0.0178(8) 0.0217(8) 0.0219(8) -0.0052(6) -0.0022(6) -0.0014(6)
Rrferences
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.: DarsteUung und Kristallstruktur von CsSb2Se4.
Z. Anorg. Allg.Chem. 536 (1986) 114-118.
3. McCarthy, T. J.; Kanatzidis M. G.: Polysulfide Ligands in Solid-State Anümony Compounds. Isolation and Structural Characterization of Cs2Sb4S8 and CsSbSe. Inorg. Chem. 33 (1994) 1205-1211.
4. Sheldrick, G. M.: Phase Annealing in SHELX-90: Direct Methods for Large Structures. Acta Crystallogr. A46 (1990) 467^73.
5. Sheldrick, G. M.: SHELXL-93, a program for refining crystal structures.
University of Göttingen, Germany 1993.
