Summer Student Project: ISIS-5

Commissioning and Exploitation of a Schlenk line

The Schlenk line (also known as a vacuum gas manifold) is a commonly used chemistry apparatus for the preparation and manipulation of air- and moisture-sensitive compounds. The aim of this project is to commission a Schlenk line and demonstrate that it is capable of handling air-sensitive materials; TiCl4 will be used for this purpose. The apparatus will then be used to prepare [RuH2(H2)((P(C6H5)3))3] and its selectively deuterated isotopomer [RuH2(H2)((P(C6D5)3))3].

The Schlenk line (also known as a vacuum gas manifold) is a commonly used chemistry apparatus for the preparation and manipulation of air- and moisture-sensitive compounds. It consists of a dual manifold with four ports. One manifold is connected to a source of purified inert gas, while the other is connected to a vacuum pump. The inert-gas line is vented through an oil bubbler, while solvent vapours and gaseous reaction products are prevented from contaminating the vacuum pump by a liquid-nitrogen trap. In 2015 ISIS purchased a Schlenk line but this was only partly commissioned because a staff member left. The aim of this project is to complete the commissioning and demonstrate that it is capable of handling air-sensitive materials; TiCl4 will be used for this purpose. The apparatus will then be used to prepare [RuH2(H2)((P(C6H5)3))3] and its selectively deuterated isotopomer [RuH2(H2)((P(C6D5)3))3]. The compound contains both conventional hydride ligands as well as a coordinated dihydrogen ligand. The products will be analysed by powder X-ray diffraction, infrared, Raman and inelastic neutron scattering spectroscopies. These compounds are of considerable interest for use in organic synthesis as selective hydrogenation agents.

The student will gain skills in the preparation and manipulation of air sensitive compounds. They will also undertake their characterisation using a range of diffraction and spectroscopic techniques on state-of the-art equipment. The outcome is expected to be at least one publication, of which the student would be a co-author.

The Schlenk line commissioning is expected to take two weeks. The synthesis of [RuH2(H2)((P(C6H5)3))3] only requires two steps, each of which can be done in a day. The isotopomer is prepared by the same way but starting from P(C6D5)3. Thus the preparation should take a week. Allowing for training, gremlins and characterisation of the compounds, four weeks is a reasonable time for this part of the project, giving an overall duration of 6 weeks. The starting date would be on or after Monday 17th July 2017.

Supervisors: Stewart Parker (stewart.parker@stfc.ac.uk) / James Taylor (james.taylor@stfc.ac.uk)

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