Coordination Chemistry of [Nb2(S2)2]4+ Clusters: Preparation and Crystal Structures of K4[Nb2(S2)2(C2O4)4] · 6 H2O and (NH4)6[Nb2(S2)2(C2O4)4](C2O4)

✍ Scribed by M. Sokolov; A. Virovets; W. Clegg

• Publisher: John Wiley and Sons
• Year: 2001
• Tongue: German
• Weight: 151 KB
• Volume: 627
• Category: Article
• ISSN: 0372-7874
• DOI: 10.1002/1521-3749(200101)627:1<119::aid-zaac119>3.0.co;2-e

✦ Synopsis

Bis(disulfido)

bridged Nb IV cluster oxalate complexes [Nb 2 (S 2 ) 2 (C 2 O 4 ) 4 ] 4± were prepared by ligand substitution reaction from the aqua ion [Nb 2 (l-S 2 ) 2 (H 2 O) 8 ] 4+ and isolated as K 4

(3). The crystal structures of 1 and 2 were determined. The crystals of 1 belong to the space group P1, a = 720.94( ) pm, b = 983.64(10) pm, c = 1071.45(10) pm, a = 109.812(1)°, b = 91.586(2)°, c = 105.257(2)°. The crystals of 2 are monoclinic, space group C2/c, a = 1567.9(2) pm, b = 1906.6(3) pm, c = 3000.9(4) pm, b = 95.502(2)°. The packing in 2 shows alternating layers of cluster anions and of ammonium/uncoordinated oxalates perpendicular to the [1 0 1] direction.

Vibration spectra, electrochemistry and thermogravimetric properties of the complexes are also discussed.