Abstract The thioarsenate(III) Cs2As8S13 has been prepared by the reaction of Cs2CO3 with As2S3 in aqueous solution under pressure at 180 °C. Its structure has been established by X-ray structural analysis. The polymeric anion (As8S132-)n is composed of individual As4S4 -rings, which are each connected to three further eight-membered rings via As-S-As bridges, so giving rise to an infinite layer structure.

[(μ-NtC4H9)2V2Cp2(OtC4H9)2] (2) and [(μ-Cl)2V2Cp2(NtC4H9)2] (6) have been prepared by reac­tion of LitC4H9 with tC4H9N=VCp(OtC4H9)Cl and tC4H9N=VCpCl2, respectively. The molecular structure has been investigated by X-ray diffraction analysis. NMR and ESR Spectra indicate two types of tert-butyliminovanadium(IV) complexes: 2 (diamagnetic) and 6 (paramagnetic).

CsSb2Se4 wurde durch hydrothermale Reaktion von Cs2CO3 mit Sb2Se3 bei einer Temperatur von 115°C dargestellt. Eine Röntgenstrukturanalyse ergab, daß die Verbindung Polyselenoantimonat(III)‐Anionen (Sb2Se4 ‐)n beinhaltet, die sowohl (Sb)SeSb‐ als auch (Sb)SeSe(Sb)‐Brücken aufweisen. Für eines der beiden unabhängigen Sb‐Atome wird eine ψ‐tetraedrische Koordination, für das andere eine ψ‐trigonalbipyramidale Koordination gefunden. Die SbSe‐Polyeder sind über gemeinsame Ecken und Kanten sowie über direkte SeSe‐Bindungen zu Schichten vernetzt.

The title phase is obtainable by hydrothermal reaction of Cs2CO3 with Sb2Se3 in a H2O suspension at 1 15°C within 10d. The structure of the novel compound (PT, Z=2) consists of (Sb2Se; )" anions, containing (Sb)Se‐Sb and (Sb)Se‐Se(Sb) bridges, and of Cs cations.