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Issue 4, 2004
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Synthesis, structure and reactivity of ferrio-chloro-phosphanes, -arsanes and -stibanes [(CO)25-C5Me5)FePn(Cl)R] (Pn = P, As, Sb); R = tetramethylcyclopentadienyl, 2,7-di-tert-butylfluorenyl, 2,7-di-tert-butyl-9-trimethylsilylfluorenyl) as precursor to novel metallo-phosphaalkenes, -arsaalkenes, and -stibaalkenes

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Abstract

Reaction of one equivalent of the complexes [FeCp*(CO)2PnCl2] (Pn = P, As, Sb) with tetramethylcyclopentadienyllithium afforded compounds [FeCp*(CO)2{Pn(Cl)(C5Me4H)}]. Dehydrochlorination by means of tert-butyllithium led to decomposition. Only in the case of the phosphorus compound was evidence for the initial formation of a phosphaalkene given by 31P NMR spectroscopy. Similarly treatment of equimolar amounts of [FeCp*(CO)2PnCl2] with 2,7-di-tert-butyl-9-H-fluorenyllithium or 2,7-di-tert-butyl-9-trimethylsilylfluorenyllithium yielded the asymmetrically substituted ferriopnicogenanes [FeCp*(CO)2{Pn(Cl)-9-R-Fl*}] (Pn = P, As, Sb; R = H, Me3Si; Fl* = 2,7-di-tert-butylfluorenylidene). Dehydrohalogenation of [FeCp*(CO)2{Pn(Cl)-9-H-Fl*}] with lithium diisopropylamide resulted in the formation of the anticipated phosphaalkene [FeCp*(CO)2{P = Fl*}], whereas in the case of the arsenic and antimony derivatives the novel ferriopnicogenanes [FeCp*(CO)2{Pn(9-H-Fl*)2}] (Pn = As, Sb) were obtained as products. The new compounds were characterized by elemental analyses and spectra (IR, 1H, 13C, 29Si, 31P NMR). The molecular structures of [FeCp*(CO)2{Pn(Cl)(C5Me4H]}] (Pn = As, Sb), [FeCp*(CO)2{As(Cl)(9-Me3Si-Fl*)}] and [FeCp*(CO)2{Sb(9-H-Fl*}2] were elucidated by single X-ray diffraction analyses.

Graphical abstract: Synthesis, structure and reactivity of ferrio-chloro-phosphanes, -arsanes and -stibanes [(CO)2(η5-C5Me5)FePn(Cl)R] (Pn = P, As, Sb); R = tetramethylcyclopentadienyl, 2,7-di-tert-butylfluorenyl, 2,7-di-tert-butyl-9-trimethylsilylfluorenyl) as precursor to novel metallo-phosphaalkenes, -arsaalkenes, and -stibaalkenes

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Publication details

The article was received on 24 Nov 2003, accepted on 06 Jan 2004 and first published on 22 Jan 2004


Article type: Paper
DOI: 10.1039/B315221A
Citation: Dalton Trans., 2004,0, 659-667

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    Synthesis, structure and reactivity of ferrio-chloro-phosphanes, -arsanes and -stibanes [(CO)25-C5Me5)FePn(Cl)R] (Pn = P, As, Sb); R = tetramethylcyclopentadienyl, 2,7-di-tert-butylfluorenyl, 2,7-di-tert-butyl-9-trimethylsilylfluorenyl) as precursor to novel metallo-phosphaalkenes, -arsaalkenes, and -stibaalkenes

    L. Weber, L. Pumpenmeier, H. Stammler and B. Neumann, Dalton Trans., 2004, 0, 659
    DOI: 10.1039/B315221A

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