ISSN:
0044-2313
Keywords:
Chemistry
;
Inorganic Chemistry
Source:
Wiley InterScience Backfile Collection 1832-2000
Topics:
Chemistry and Pharmacology
Description / Table of Contents:
Contributions to the Chemistry of Organo Transition Metal Compounds. 55. Preparation and Properties of Niobocenium and Tantalocenium Salts - Crystal and Molecular Structure of [(C5H5)2NbCl2][BF4] · CH3CNNiobocenium and tantalocenium compounds of the type [(C5H5)2MCl2]X (X = BF4, PBh4, PF6) were synthesized from the metallocene dichlorides and ferricenium salts, [(C5H5)2Fe]X, in methylene dichloride or tetrahydrofuran. With acetonitrile as solvent [(C5H5)2MCl2]X · CH3CN complexes are formed. Stable methyl compounds of the type [(C5H5)2M(CH3)2]X were obtained, when (C5H5)2Ta(CH3)2 is oxidized by means of ferricenium salts. The new complexes were characterized by elemental analysis, i. r., and 1H n.m.r. spectra. The structure of [(C5H5)2NbCl2][BF4] · CH3CN has been determined by X-ray structure analysis. The compound crystallizes in the orthorhombic space group Cmcm with a = 8.324(12), b = 19.581(13), c = 9,563(8) Å and Z = 4. The coordination geometry of the Nb atom is tetrahedrally.
Notes:
Niobocenium- und Tantalocenium-Verbindungen des Typs [(C5H5)2MCl2]X (X = BF4, PF6, BPh4) wurden aus den Metallocendichloriden und Ferricenium-Salzen, [(C5H5)2Fe]X, in Methylenchlorid bzw. Tetrahydrofuran als Reaktionsmedium erhalten. Bei Verwendung von Acetonitril entstanden Verbindungen des Typs [(C5H5)2MCl2]X · CH3CN (X = BF4, PF6). Durch Oxydation von (C5H5)2Ta(CH3)2 mit Ferricenium-Salzen waren stabile Komplexe der Zusammensetzung [(C5H5)2Ta(CH3)2]X zugängig. - Die dargestellten Verbindungen wurden charakterisiert durch Elementaranalysen sowie IR- und 1H-NMR-Spektren. Die Struktur der Verbindung [(C5H5)2NbCl2][BF4] · CH3CN wurde durch Röntgenkristallstrukturanalyse bestimmt. Die Verbindung kristallisiert orthorhombisch in der Raumgruppe Cmcm mit den Gitterkonstanten a = 8,324(12), b = 19,581(13), c = 9,563(8) Å und Z = 4. Die Koordinationsgeometrie des Nb-Atoms ist tetraedrisch.
Additional Material:
3 Ill.
Type of Medium:
Electronic Resource
URL:
http://dx.doi.org/10.1002/zaac.19905870110
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