202803-64-3Relevant academic research and scientific papers
Synthesis, Structure, and Reactivity of Novel Intramolecularly Coordinated Organolead(II) Compounds
Jurkschat, Klaus,Peveling, Katja,Schuermann, Markus
, p. 3563 - 3571 (2007/10/03)
The intramolecularly coordinated heteroleptic organolead(II) compounds {4-tBu-2,6-[P(O)(OEt)2]2C6H2}PbX (2, X = Cl; 3, X = SPh) have been synthesized. Single-crystal X-ray analyses reveal that both compounds adopt polymeric chain structures by intermolecular Pb-X...Pb bridges, a structural motif previously unknown for organolead(II) derivatives. Compound 2 reacts with lithium diisopropylamide, iPr 2NLi, and lithium bis(trimethylsilyl)methane, (Me3Si) 2CHLi, respectively, to provide in situ the corresponding organolead(II) compounds {4-tBu-2,6-[P(O)(OEt)2]2C 6H2}PbX (4, X = iPr2N; 5, X = (Me 3Si)2CH], which were identified by NMR spectroscopy but could not be obtained as analytically pure substances. Attempts to isolate the intramolecularly coordinated organolead(II) hexafluorophosphate {4-tBu-2,6-[P(O)-(OEt)2]2C6H 2}Pb+PF6- from the reaction of 2 with TlPF6 also failed. Instead, the unprecedented salt [{5-15-tBu-1,3-[P(O)(OEt)2]2C6H 3}4·(Pb2F)] [PF6] 3·4THF (6) was obtained, in which the [(Pb-F-Pb)] 3+ cation is stabilized by eight intermolecular P=O→Pb interactions. Compound 6 was characterized by single-crystal X-ray analysis and electrospray mass spectrometry. Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2003.
