The solid-state structures of unsolvated potassium, rubidium, and cesium carbazolates were determined
using laboratory X-ray powder diffraction data. Potassium and rubidium carbazolates adopt a polymeric
helical arrangement, whereas cesium carbazolate forms a polymeric twisted column structure.
The synthesis of six alkali metal carbazolide crown ether complexes is reported: Potassium-carbazolide(18-crown-6) (1), rubidium-carbazolide(18-crown-6) (2), rubidium-carbazolide(15crown-5) (3), cesium-carbazolide(18-crown-6) (4), cesium-carbazolide-bis(15-crown-5) (5), and cesium-carbazolide-bis(benzo-15crown-5) (6). The complexes 1 to 6 were synthesized from the alkali metal carbazolide (obtained in solution by metalation of carbazole with KH or Rb-and Cs-hexamethyldisilazide) and the corresponding crown ether. The structures of 1, 3, 4, and 5 could be determi-
Einleitung 1)Im Rahmen unserer systematischen Untersuchungen zur Struktur der Alkalimetallsalze heterocyclischer Amide berichteten wir kürzlich über die Synthese und Struktur von Kronenether-Komplexen der Alkalimetall-Pyrrolide und -Indolide [1,2]. In der vorliegenden Arbeit leisten wir nun einen Beitrag zur Synthese und Struktur der Alkalimetall-Carbazolide. Das Carbazolid-Anion (Abb. 1, rechts) ist verwandt mit dem Pyrrolid-und dem Indolid-Anion (Abb. 1, links, und 1, Mitte) und lässt sich wie letztere leicht durch Deprotonierung des neutralen NH-sauren Amins (hier: Carbazol) herstellen. Wie Pyrrolid und Indolid ist auch Carbazolid fähig, über das freie Elektronenpaar am Stickstoffatom eine dative N-Metall-σ-Bindung zu bilden. Dane-1581 ned by X-ray diffraction. Complex 1 is mononuclear, the carbazolide anion shows an η 1 (N)-coordination to the metal cation. The complexes 3 and 4 are dinuclear with a central metal 2 N 2 -ring. Compound 5 has a salt-like structure with a sandwich-like [Cs(15crown-5) 2 ] ϩ cation and an uncoordinated carbazolide anion.
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