Work described in this thesis shows the design and synthesis of functionalised, triple stranded, dinuclear, supramolecular helicates. Click chemistry has been utilized to functionalise the parent ligand with dansyl and coumarin moiety’s. These ligands have been used to successfully form four novel metal complexes upon reaction with iron(II) chloride. The stability and fluorescence of these complexes has been monitored. Imidazole ligands has been functionalised by the addition of alkyne and azide side chains to allow them to undergo click reactions. This modification has not been shown to impede complex formation, as the ligand have been utilized to form novel triple stranded iron(II) and nickel(II) complexes. Synchrotron imaging has been used to produce elemental maps of cells treated with the parent metallo cylinder. This has allowed the uptake of the complex to be monitored. Two novel bromine functionalised cylinders has been developed to allow co-localisation experiments to be undertaken using XRF imaging. Cryo-SXT experiments have been undertaken to examine the morphology of HeK cells after treatment with parent metallo cylinder.