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The structural identification in solution of the Zr(iv) complexes involving two 2,2-biphenol-based proligands is reported. The proligand L(1)H2 contains one 2,2-biphenol unit whereas L(2)H4 incorporates two 2,2-biphenol units linked by a para-phenylene bridge. Diffusion Ordered Spectroscopy (DOSY) combined with electrospray mass spectrometry analysis and density functional theory (DFT) allowed for determining the molecular structures of such Zr(iv)-based architectures. It is proposed that [Zr(OPr(i))4(HOPr(i))] in the presence of L(1)H2 generates an octahedral complex formulated as [ZrL(1)3H2]. Concerning the self-assembled architecture incorporating the L(2) ligand, the analytical data highlight the formation of an unprecedented neutral Zr(iv) triple-stranded helicate ([Zr2L(2)3H4]). Insight into the geometry of these complexes is obtained via DFT calculations. Remarkably, the helicate structure characterized in solution strongly contrasts with the triple-stranded structure of the complex that crystallizes.

Identification of Zr(iv)-based architectures generated from ligands incorporating the 2,2′-biphenolato unit