Solvent Free and Extreme Synthesis Strategies
The synthetic methods applied in our workgroup are based on the reaction of elemental or metal containing precursors, like chlorides. These substances are combined with nitrogen containing, multidental ligands in evacuated Duran glass ampoules. Ligands are chosen according to the capability of coordinative interaction with metals as well as acidity, thermal stability and coordination modes.
Syntheses are carried out in a solvent free melt of the ligand, thus eliminating the possibility of solvent co-coordination or straight expulsion of ligands by a stronger coordinating solvent. Various methods of activation of the metals are used: amalgamation, liquid ammonia and microwaves.
Another extreme method is the solution of metals in liquid ammonia, leading to electride solutions and in the following to the synthesis of metal amides with organic amines.
The goal of all syntheses is to obtain a product of high crystallinity in high yields in order to solve and refine the structure of the compound with X-ray diffraction on single crystals or powders.