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Synthese,Charakterisierung und Struktur von P7(t-Bu3Si)3 („Tris(supersilyl)heptaphosphan(3)”︁)
Authors:I Kovcs  G Baum  G Fritz  D Fenske  N Wiberg  H Schuster  K Karaghiosoff
Institution:I. Kovács,G. Baum,G. Fritz,D. Fenske,N. Wiberg,H. Schuster,K. Karaghiosoff
Abstract: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 (AMX]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).
Keywords:Tris(tri-tert-butylsilyl)heptaphosphonortricyclane P7(t-Bu3Si)3  synthesis  31P{1H} NMR data  crystal structure
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