The Reaction of Tin(II) Halides with Li(THF)_2.5 Ge(SiMe₃)₃: The X-ray Crystal Structure of a New Cyclotetrastannane

Article type: Research Article

Authors: Mallela, Siva | Su, Wu-Pei | Chen, Yan-Song | Korp, James D. | Geanangel, R.A.

Affiliations: Departments of Chemistry and Physics, The University of Houston, Houston, Texas 77204-5641

Note: [] Corresponding author

Abstract: Reaction of SnCl2 with two equivalents of Li(THF)2.5Ge(SiMe3)3 in hexane at −78°C gave both red and colorless crystalline products. The latter was identified by m.p and NMR spectra as [(Me3Si)3Ge]2SnCl2. FAB mass spectra showed that the red crystals contained an Sn4 cluster and Ge(SiMe3)4. An X-ray structure determination on the red crystals was complicated by several types of disorder but the structure was solved with the aid of a new simulated annealing program revealing the product as the heteroleptic cyclotetrastannane, [(Me3Si)3GeSnC1]4. The product crystallized as a complex with two molecules of Ge(SiMe3)4 in the F23 (cubic) space group with a = 23.120(7) Å, ρ(ca1c) = 1.35 g-cm−3, Z = 4,996 data collected, R = 0.049. Similar reactions of SnX2, (X = F,I) appeared to result in reduction of the tin.

DOI: 10.1080/10241229812331341519

Journal: Main Group Chemistry, vol. 2, no. 4, pp. 315-322, 1998