UEBER POLYGERMANE XIV. POLYGERMANE ALS NEBENPRODUKTE DER GRIGNARD-REAKTION VON PhMgBr MIT GeCl4

Article abstract of DOI:10.1016/0022-328X(86)82053-8

The synthesis of GePh4 and Ge2Ph6 by Grignard reaction in THF or ether/toluene leads to the by-products Ge3Ph8 (up to 11 percent) and Ge4Ph10 (up to 18 percent) 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 deg for Ge3Ph8, 53-66 deg for Ge4Ph10).The Ge-Ge distances and Ge-Ge-Ge angles are 244 pm and 121 deg (Ge3Ph8), and 246 pm and 118 deg (Ge4Ph10).