This is a PhD research project in chemistry. This PhD project will continue our investigations into Rh-catalyzed C-H activation. Currently we have a system that upon photoactivation with 400 nm light undergoes intramolecular activation of sp3 centres forming a metallacycle. We will investigate ligand modifications that will build towards the intermolecular activation of alkanes (including building towards the very challenging substrate methane) by tethering the NHC ligand in order to prohibit reactivity with the Rh center, as well as utilizing smaller Me substitution. In addition, we will make comparisons to a related thermally-activated system that undergoes intermolecular arene C-H borylation that we think may proceed via Rh boryls instead of low coordinate Rh complexes. Finally, this work will provide insight into suitable complexes for performing ultra-fast reactivity studies at the Rutherford Appleton Laboratory in future years.