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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 602 (1991), S. 73-78 
    ISSN: 0044-2313
    Keywords: 1,2,3,4-Tetrakis(di-tert-butylphosphanyl)-cyclo-tetraphosphane ; 31P n.m.r. ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Cyclotetraphosphane P4[P(tBu)2]4P4[P(tBu)2]4 1 is obtained by thermal decomposition (20°C) of (tBu)2P—P = P(tBu)2Br which is formed from [(tBu)2P]2PLi and 1,2-dibromoethane. The 31P NMR spectrum of 1 shows two complex signal patterns of the AA′ A″ A‴ XX′X″X‴ type; δ = +63 ppm (exocyclic) and δ = -43 ppm (cyclic).1 crystallizes monoclinic in the space group C2/c, (a = 2240.8(17) pm, b = 885.6(7) pm, c = 2221.8(14) pm, β = 101.72(5)°) with Z = 4 molecules in the elementary cell. The molecule has E conformation. The four-membered ring is folded (dieder angle 61°) to give the P(tBu)2 groups nearly equatorial and the lone pairs nearly axial positions.
    Notes: P4[P(tBu)2]4 1 entsteht bei der thermischen Zersetzung des (tBu)2P—P = P(tBu)2Br bei 20°C, das sich aus [(tBu)2P]2PLi und 1,2-Dibromethan bildet. Das 31P-NMR-Spektrum von 1 enthält zwei komplexe Signalgruppen; δ = +63 ppm (exocyclisch) und δ = -43 ppm (cyclisch). Es liegt ein AA′ A″ A‴ XX′X″X‴ Spinsystem vor. 1 kristallisiert monoklin in der Raumgruppe C2/c, a = 2240,8(17) pm, b = 885,6(7) pm, c = 2221,8(14) pm, β = 101,72(5)° mit Z = 4 Molekülen in der Elementarzelle. Das Molekül besitzt E-Konformation. Der Vierring ist gefaltet, Diederwinkel 61°. Dadurch nähern sich die P(tBu)2-Gruppen einer äquatorialen und die nichtbindenden Elektronenpaare am Phosphor einer axialen Position.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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