ISSN:
0044-2313
Keywords:
1,10-Dinitro-octahydro-closo-decaborate(2-)
;
Crystal Structure
;
11B NMR Spectrum
;
Vibrational Spectra
;
Chemistry
;
Inorganic Chemistry
Source:
Wiley InterScience Backfile Collection 1832-2000
Topics:
Chemistry and Pharmacology
Description / Table of Contents:
Preparation, 11B NMR, Vibrational Spectra and Crystal Structure of [P(C6H5)4]2 [1,10-(O2N)2B10H8]By reaction of [N(C4H9)4]2[B10H10] in aqueous acetonitrile with NO2 a reaction mixture is formed from which [1,10-(O2N)2B10H8]2- has been isolated by ion exchange chromatography on diethylaminoethyl(DEAE) cellulose. The X-ray structure determination of [P(C6H5)4]2 [1,10-(O2N)2B10H8] (triclinic, space group P1, a = 10.831(3), b = 13.059(3), c = 18.496(5) Å, α = 82.13(2), β = 75.87(2), γ = 71.08(2)°, Z = 2) reveals the coordination of both nitro groups via N in the apical positions of the B10 cluster with B1-N1 = 1.526(3) and B10-N2 = 1.537(3) Å and ONO angles of 119.3(2) and 120.1(2)°. The 11B NMR spectrum exhibits the characteristic feature (2:8) of a in 1,10 position disubstituted B10 cluster with a strong downfield shift of the ipso-B atoms at + 17.3 ppm. The IR and Raman spectra show strong NO stretching vibrations at 1384 und 1425 cm-1.
Notes:
Beim Einleiten von NO2 in eine wäßrige Acetonitrillösung von [N(C4H9)4]2 [B10H10] entsteht ein Produktgemisch, aus dem [1,10-(O2N)2B10H8]2- durch Ionenaustauschchromatographie an Diethylaminoethyl(DEAE)-Cellulose isoliert worden ist. Die Röntgenstrukturanalyse an [P(C6H5)4]2 [1,10-(O2N)2B10H8] (triklin, Raumgruppe P1, a = 10,831(3), b = 13,059(3), c = 18,496(5) Å, α = 82,13(2), β = 75,87(2), γ = 71,08(2)°, Z = 2) beweist die Bindung der beiden Nitro-Gruppen über die N-Atome in apikaler Position des B10-Clusters mit den Abständen von B1-N1 = 1,526(3) und B10-N2 = 1,537(3) Å und den ONO-Winkeln 119,3(2) und 120.1(2)°. Im 11B-NMR-Spektrum beobachtet man das charakteristische Signalmuster (2:8) eines in 1,10-Position disubstituierten B10-Clusters mit starkem Tieffeldshift der ipso-B-Kerne bei + 17,3 ppm. Im IR- und Raman-Spektrum treten intensive NO-Valenzschwingungen bei 1384 und 1425 cm-1 auf.
Additional Material:
3 Ill.
Type of Medium:
Electronic Resource
URL:
http://dx.doi.org/10.1002/zaac.199762301108
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