147102-80-5Relevant academic research and scientific papers
(Tris(trimethylsilyl)silyl)lead(IV) derivatives
Mallela,Geanangel
, p. 602 - 605 (1993)
The reaction of Ph3PbCl with 1 equiv of (THF) 3LiSi(SiMe3)3 in ether afforded Ph 3PbSi(SiMe3)3 in high yield. Our attempts to prepare Ph2Pb(Si(SiMe3)3)2 through a similar reaction of Ph2PbCl2 with 2 equiv of (THF) 3LiSi(SiMe3)3 gave a mixture of the expected product, a pale yellow solid, and [Ph2PbSi(SiMe3) 3]2, a bright yellow-orange, thermochromic solid. These products were separated by fractional crystallization from the reaction mixture and characterized by their elemental analyses, NMR spectra (1H, 13C), and infrared and UV-visible spectra. In order to compare [Ph2PbSi(SiMe3)3]2 with its previously reported digermane counterpart, an X-ray structure determination was carried out on the product as a benzene monosolvate. Crystals of [Ph 2PbSi(SiMe3)3]2 were monoclinic, P21/n, with a = 13.208(2) A, b 16.586(3) A, c = 13.896(3) A, β = 99.29°, V = 3004 A3, and Z = 2. The molecular structure confirmed that the product is indeed a diplumbane exhibiting a Pb-Pb bond 2.911(1) A in length. All three products were unreactive toward atmospheric moisture. NMR studies of Ph2Pb(Si(SiMe 3)3)2 and [Ph2PbSi(SiMe 3)3]2 solutions in ether showed the former to be stable for at least 22 h while the latter decomposed completely within the same period.
