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By reaction of Cs 2 [B 6 H 6 ] with in situ generated dicyanogen in aqueous alkaline solution the monocyanohydrohexaborate Cs 2 [B 6 H 5 (CN)] and the dicyanohydrohexaborate cis-Cs 2 [B 6 H 4 (CN)2] are formed. The compounds have been separated by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structure of Cs 2 [B 6 H 5 (CN)] was determined from single crystal X-ray diffraction analysis; monoclinic, space group P2 1 /a with a = 9.540(8), b = 9.977(3), c = 10.578(2)Å, β = 105.06(2)°. The B 6  octahedron is compressed in the direction of the nearly linear B—CN bond by about 5%, with bond lengths between 1.71 and 1.76Å. The "B NMR spectra of the two compounds reveal the features of substituted B 6  cages with C 4v  and C 2v  point symmetry. In the  13 C NMR spectrum of Cs 2 [B 6 H 5 (CN)] a quartet at -139 ppm with  1 J(C,B) 92 Hz is observed. The IR and Raman spectra exhibit very strong CN stretching bands for Cs 2 [B 6 H 5 (CN)] at 2149, and for cis-Cs 2 [B 6 H 4 (CN) 2 ] at 2170 cm -1 .

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Darstellung,  11 B-,  13 C-NMR- und Schwingungsspektren der closo-Hexaborate [B 6 H 5 (CN)1 2 - und cis-[B 6 H 4 (CN) 2 ] 2−  sowie Kristallstruktur von Cs 2 [B 6 H 5 (CN)] / Preparation,  11 B, 13 C NMR and Vibrational Spectra of the closo-Hexaborates [B 6 H 5 (CN)] 2-  and cis-[B 6 H 4 (CN) 2 ] 2 -, and the Crystal Structure of Cs 2 [B 6 H 5 (CN)]