6533b7d4fe1ef96bd1261c39

RESEARCH PRODUCT

Über polygermane

Karl HäberleMartin Dräger

subject

StereochemistryOrganic ChemistryNuclear magnetic resonance spectroscopyCrystal structureCarbon-13 NMRBiochemistryInorganic ChemistryCrystallographychemistry.chemical_compoundChain lengthchemistryOne pot reactionX-ray crystallographyMaterials ChemistryMoleculePhysical and Theoretical ChemistryTriethylamine

description

Abstract The germylene Ph2Ge of Ph2GeHCl and Net3 inserts in excess Ph2GeHCl and forms polygermanes Cl(Ph2Ge)nH. This one-pot reaction and subsequent chlorination to Cl(Ph2Ge)nCl has been optimized. Increasing amounts of NEt3 step up the yields of higher polygermanes. The 13C NMR phenyl signals for C(ipso) shift to low field with increasing chain length. The crystal structures of Cl(Ph2Ge)3,4Cl (R = 0.072 and 0.087) have been determined. The position of Cl(Ph2Ge)4Cl is split off by disorder (main molecule 82%, side molecule 18%). Two crystallographically different molecules of the trigermane are present; the ClGe3Cl chain contains anti-gauche and gauche-gauche conformation respectively (distances GeGe 241.3–243.7 pm, angles GeGeGe 110.4 and 116.7°). The ClGe4Cl chain is centrosymmetric and has all-anti conformation (distances GeGe 245.0 and 244.2 and 244.2 pm, angle GeGeGe 116.2°).

https://doi.org/10.1016/0022-328x(86)80294-7