6533b82bfe1ef96bd128e00b

RESEARCH PRODUCT

Über polygermane

Stefan RollerDietolf SimonMartin Dräger

subject

ChemistryStereochemistryOrganic ChemistryGrignard reactionEtherNuclear magnetic resonance spectroscopyCrystal structureBiochemistryMedicinal chemistryTolueneHigh-performance liquid chromatographyInorganic Chemistrychemistry.chemical_compoundX-ray crystallographyMaterials ChemistryMoleculePhysical and Theoretical Chemistry

description

Abstract The synthesis of GePh4 and Ge2Ph6 by Grignard reaction in THF or ether/toluene leads to the by-products Ge3Ph8 (up to 11%) and Ge4Ph10 (up to 18%) which is dependant on using an excess of Mg. A quantitative analysis of the resulting products by HPLC and a semipreparative separation by column, flash, and HPL chromatography is described. The crystal structures of Ge3Ph8 (R = 0.075) and Ge4Ph10 · 2C6H6 (R = 0.054) have been determined. Ge4Ph10 has Ci symmetry and both chain conformations are well staggered (49–70° for Ge3Ph8, 53–66° for Ge4Ph10). The GeGe distances and GeGeGe angles are 244 pm and 121° (Ge3Ph8), and 246 pm and 118° (Ge4Ph10).

https://doi.org/10.1016/0022-328x(86)82053-8