Journal
ORGANOMETALLICS
Volume 30, Issue 5, Pages 1030-1033Publisher
AMER CHEMICAL SOC
DOI: 10.1021/om101074j
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- Deutsche Forschungsgemeinschaft
- DNRF
- Center for Materials Crystallography
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LGeCl (L = PhC(NtBu)(2)) was treated with elemental sulfur in THF to afford [{PhC(NtBu)(2)}(2)Ge-2(mu-S)(2)Cl-2] (2) in 44% yield instead of yielding a compound containing a Ge=S double bond. It was revealed by the X-ray single-crystal structure that there is no Ge=S unit in 2. Instead, 2 features a four-membered ring containing two germanium and two sulfur atoms. The four-membered Ge2S2 ring is planar and is formed by a weak [2 + 2] cycloaddition interaction. Within the ring skeleton the two germanium atoms are arranged opposite to each other. Furthermore, 2 was reduced with 2 equiv of potassium graphite in THF to yield a potassium salt of a germathiocarboxylate analogue of composition [{PhC(NtBu)(2)}Ge(S)SK(THF)](2) (3). Compounds 2 and 3 were characterized by single-crystal X-ray diffraction studies, NMR spectroscopy, EI-MS spectrometry, and elemental analysis.
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