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  • 1
    ISSN: 0044-2313
    Keywords: Tris(tri-tert-butylsilyl)heptaphosphonortricyclane P7(t-Bu3Si)3 ; synthesis ; 31P{1H} NMR data ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Characterization, and Structure of P7(t-Bu3Si)3 („Tris(supersilyl)heptaphosphane(3)“Tris(tri-tert-butylsilyl)heptaphosphanortricyclane P7(t-Bu3Si)3 1 is obtained from the reaction of (t-Bu)3Si—Si(t-Bu)3 with white phosphorus and forms colorless to pale yellow thermostable crystals. 1 is identified by the complete analysis of its 31P{1H} NMR spectrum (A[MX]3 spin system) as well as by a single crystal structure determination (space group Pca21, a = 170.76(2)pm, b = 131.14(3)pm, c = 426.61(5)pm, α = β = γ= 90°, Z = 8 formula units in the elementary cell). The steric demand of the (t-Bu)3Si-Groups causes an increase of the exocyclic bond angles at the equatorial phosphorus atoms Pe, while it does not particularly influence the P7-skeleton. Chlorine (r.t.) and bromine (70°C) degrade the P7-cage of 1 with formation of PX3 and (t-Bu)3SiX (X = Cl, Br).
    Notes: Tris(tri-tert-butylsilyl)-heptaphosphanortricyclan P7(t-Bu3Si)3 1 entsteht durch Umsetzung von (t-Bu)3Si—Si(t-Bu)3 mit weißem Phosphor und bildet farblose bis blaßgelbe thermostabile Kristalle. Die Identität von 1 wird durch die vollständige Analyse des 31P{1H}-NMR-Spektrums (A[MX]3-Spinsystem) sowie durch eine Kristallstrukturbestimmung belegt. 1 kristallisiert in der Raumgruppe Pca21 mit Z = 8 Formeleinheiten; a = 170,76(2)pm, b = 131,14(3)pm, c = 426,61(5)pm, α = β = γ= 90°. Der erhöhte Raumbedarf der (t-Bu)3Si-Gruppen führt zu einer Aufweitung der exocyclischen Bindungswinkel an den äquatorialen Phosphoratomen Pe ohne das P7-Gerüst besonders zu beeinflußen. Chlor (Raumtemperatur) und Brom (70°C) bauen den P7-Käfig von 1 unter Bildung von PX3 und (t-Bu)3SiX (X = Cl, Br,) ab.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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