Darstellung, 11B-, 13C-NMR-und Schwingungsspektren von Cyanomethylhexahydro-closo-Hexaborat(Hexaborat(1-), [B6H6(CH2CN)]– sowie Kristallstruktur von [P(C6H5)4][B6H6(CH2CN)] / Preparation, 11B, 13C NMR and Vibrational Spectra of Cyanomethylhexahydro-closohexaborate(1-), [B6H6(CH2CN)]- and the Crystal Structure of [P(C6H5)4][B6H6(CH2CN)]
Abstract
By reaction of [B 6 H 6 ] 2- with chloroacetonitrile in dichloromethane the cyanomethylhexahy-dro-closo-hexaborate(1-), [B 6 H 6 (CH 2 CN)] - is formed. The com pound has been separated from excess [B 6 H 6 ] 2- by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structure of [P(C 6 H 5 ) 4 ][B 6 H 6 (CH 2 CN)] has been determined by single crystal X-ray diffraction analysis; triclinic, space group P1 with a = 7.503(3), b = 12.0949(8), c = 14.6572(11) Å α = 79.399(6)°, β = 79.19(2)°, γ = 89.2(2)°. The 11 B NMR spectrum is consistent with a mono hetero substituted octahedral B6 cage. In the 13 C NMR spectrum of Cs 2 [B 6 H 5 (CH 2 CN)] a singlet at 131.9 ppm (CN) and a quartet at 2.97 ppm with 1 J(C,B) = 54.7 Hz (CH 2 ) are observed. The IR and Raman spectra exhibit a very strong CN stretching band at 2218 cm -1 .
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