The multicomponent coordination chemistry involving Ti(OPr), the ortho-phenylenediamine ligand (opda) and 2,2'-biphenol-based proligands (LH and LH) is described. The proligands LH and LH incorporate two and three 2,2'-biphenol units linked with p-phenylene bridges (p-PLB) respectively. We demonstrate that this selected set of components allows the spontaneous formation of neutral double-stranded helicates. In particular, we report the X-ray crystal structure of a multicomponent helicate formed with L, named Ti(L)(opda). The molecular structure of the helicate shows two inequivalent L ligands. H NMR analysis at variable temperature highlights an intramolecular fluxional phenomenon for this species. An insight into this dynamic behaviour is obtained via the energy profiles of Ti(L)(opda) resulting from the full rotation of the p-PLB rings. Additionally, the thermodynamic parameters associated with the formation of the Ti(L)(opda) complex are modelled and discussed related to the ones linked to the formation of a related monomeric complex.
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