Synthesis, NMR characterisation and X-ray structures of mixed chalcogenido PNP ligands containing tellurium : crystal structures of (SePr2PNP)-Pr-i(H)Pr-i(2) and [NaN((EPPr2)-Pr-i)(2)](infinity) (E = Se, Te)

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Robertson, Stuart D. and Chivers, Tristram (2008) Synthesis, NMR characterisation and X-ray structures of mixed chalcogenido PNP ligands containing tellurium : crystal structures of (SePr2PNP)-Pr-i(H)Pr-i(2) and [NaN((EPPr2)-Pr-i)(2)](infinity) (E = Se, Te). Dalton Transactions (13). pp. 1765-1772. ISSN 1472-7773 (https://doi.org/10.1039/b717287g)

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Abstract

Reaction of HN((PPr2)-Pr-i)(2) with one equivalent of selenium in hexane at room temperature yields the monoselenide as the P-H tautomer Se=(PPr2)-Pr-i-N=P(H)Pr-i(2) (2b). Deprotonation of 2b with (n)butyllithium in the presence of TMEDA at -78 degrees C followed by addition of tellurium produces the air-sensitive, mixed chalcogenido complex [(TMEDA)Li((SePPr)-Pr-i,)((TePPr)-Pr-i,)N] (8Li) in > 97% purity after recrystallisation. Similarly, deprotonation of Te=(PPr2)-Pr-i-N=P(H)Pr-i(2), (2c), followed by addition of sulfur, gives the sulfur analogue [(TMEDA)Li((SPPr2)-Pr-i)((TePPr2)-Pr-i)N] (Mi) in > 99% purity. The symmetrical complexes [(TMEDA)Li(SePiPr,),N] (4Li) and [(TMEDA)Li((TePPr2)-Pr-i),N] (Ki) are produced by similar methods. Compounds 2b, 4Li, 5Li, 7Li and 8Li were characterised in solution by multinuclear (H-1, P-31, Se-77 and Te-125) NMR spectroscopy and their solid-state structures were determined by X-ray crystallography. The X-ray crystal structures of the polymeric chains [NaN((EPPr2)-Pr-i,)(2)](infinity) (4Na, E = Se and 5Na, E = Te) are also reported.

ORCID iDs

Robertson, Stuart D. ORCID logoORCID: https://orcid.org/0000-0002-9330-8770 and Chivers, Tristram;
  • Item type:Article
    ID code:33865
    Dates:
    Date
    Event
    7 April 2008
    Published
    20 February 2008
    Published Online
    Subjects:Science > Chemistry
    Department:Faculty of Science > Pure and Applied Chemistry
    Depositing user: Pure Administrator
    Date deposited:29 Sep 2011 13:09
    Last modified:11 Nov 2024 09:51
    URI:https://strathprints.strath.ac.uk/id/eprint/33865
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