Volume 25, Issue 13
Preparative Inorganic Chemistry
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ChemInform Abstract: Preparation of Mononitropentahydrohexaborate(2-) and Crystal Structure of M2(B6H5(NO2)), M: K (I), Cs (II).

A. FRANKEN

A. FRANKEN

Inst. Anorg. Chem., Christian-Albrechts-Univ., D-24098 Kiel, Germany

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W. PREETZ

W. PREETZ

Inst. Anorg. Chem., Christian-Albrechts-Univ., D-24098 Kiel, Germany

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M. RATH

M. RATH

Inst. Anorg. Chem., Christian-Albrechts-Univ., D-24098 Kiel, Germany

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K.-F. HESSE

K.-F. HESSE

Inst. Anorg. Chem., Christian-Albrechts-Univ., D-24098 Kiel, Germany

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First published: March 29, 1994

Abstract

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ChemInform Abstract

Yellow single crystals of the title compounds (I) and (II) are prepared in 8% yield by electrolysis of (NBu4)(B6H7) and (NBu4)NO2 in CH2Cl2 in the presence of an organic base (DBU) and addition of KOH or CsOH, resp., and isolated by ion exchange chromatography on DEAE- cellulose. As revealed from single crystal XRD, compounds (I) and (II) crystallize in the monoclinic space groups P21/m with Z = 2 and P21/a with Z = 4, respectively. The structure of (II) is closely related to that of the recently prepared Cs2(B6H5(CN)). In all three compounds the B6 octahedron of the anion is compressed in the direction to the substituent. The substituted cluster ions are arranged in layers parallel to the crystallograpic axes with an angle of inclination of 19° of the NO2 substituent towards the (110) plane.

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