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Synthesis and Crystal Structures of Cs5Nb2S4X9 – Double Salts Containing New Cluster Anions [Nb2(μ-S2)2X8]4– (X = Cl, Br)

✍ Scribed by Maxim Sokolov; Hideo Imoto; Taro Saito; Vladimir Fedorov

Publisher
John Wiley and Sons
Year
1999
Tongue
German
Weight
197 KB
Volume
625
Category
Article
ISSN
0372-7874

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✦ Synopsis

Bis(disulfide)

bridged Nb(+4) cluster halide complexes [Nb 2 S 4 X 8 ] 4± (X = Cl, Br) were prepared by acid hydrolysis of [Nb 2 S 4 (NCS) 8 ] 4± in concentrated aqueous HCl or HBr, solution from which they can be isolated as double salts Cs 5 [Nb 2 S 4 X 8 ]X (X = Cl, 1; X = Br, 2). The crystal structures of 1 and 2 were determined. The isolation and Xray structure of oxonium salt (H 3 O) 5 [Nb 2 S 4 Cl 8 ]Cl (3) is also reported. 1±3 contain new [Nb 2 S 4 X 8 ] 4± anions which can also be viewed as excised building blocks of polymeric solids NbS 2 X 2 . The extra halogen resides in the center of octahedron formed by six Cs + or H 3 O + ions. All the three salts are isostructural and crystallize in tetragonal space group Immm with the following parameters: a = 10.269(2), b = 16.343(2), c = 7.220(1) A Ê for 1, a = 10.934(1), b = 16.613(2), c = 7.470(1) A Ê for 2, a = 9.639(1), b = 16.031(1), c = 7.071(1) A Ê for 3. The parameters of the Nb 2 S 4 core are only slightly affected by the change from Cl to Br.

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Compounds with Cluster Cations together
Compounds with Cluster Cations together with Cluster Anions [(M6X12)(EtOH)6]2+ besides [(Mo6Cl8)Cl4X2]2– (M = Nb, Ta; X = Cl, Br) – Synthesis and Crystal Structures
✍ I. Bašic; N. Brničević; U. Beck; A. Simon; R. E. McCarley 📂 Article 📅 1998 🏛 John Wiley and Sons 🌐 German ⚖ 179 KB 👁 1 views

Compounds consisting of both cluster cations and cluster anions of the composition [(M 6 X 12 )(EtOH) 6 ][(Mo 6 Cl 8 )Cl 4 X 2 ] ´n EtOH ´m Et 2 O (M = Nb, Ta; X = Cl, Br) have been prepared by the reaction of (M 6 X 12 )X 2 ´6 EtOH with (Mo 6 Cl 8 )Cl 4 . IR data are given for three compounds. The