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Exploring the chemistry of vanadyl ions (VO2+) with bis-β-diketone ligands, in pyridine reactions of vanadyl sulfate with 1,3-bis-(3-oxo-3-(2-hydroxyphenyl)-propionyl)-\udbenzene (H4L1) and 1,3-bis-(3-oxo-3-(2-hydroxyphenyl)-propionyl)-pyridine (H4L2), two\udnovel clusters, [(VIVO)4(H2L1)4(py)4] (1) and [(VVO)4(VIVO)2 (O)4(L2)2(py)6] (2) were\udprepared and characterized. Due to the conformational flexibility of the ligands, both entities exhibit very peculiar metal topologies and composition, differing significantly from structural patterns established in the related chemistry of divalent 3d metals. Structural analysis also unveils the existence of the most complex metallamacrocycles from this family to date. Studies of the magnetic properties via bulk magnetization measurements and EPR spectroscopy confirmed the existence of uncoupled long-distant S = 1/2 metal centers and the spin ground states S = 2 and S = 1 of the clusters.Guillem Aromí thanks the Generalitat de Catalunya for the prize ICREA Academia 2008 and 2013, for excellence in research and the ERC (European Research Council) for a Starting Grant (258060 FuncMolQIP). The authors thank the Spanish MICINN for funding through CTQ2009-06959 (Guillem Aromí, Ivana Borilovic) and MAT2011-24284 (Olivier Roubeau). Ivana Borilovic thanks the Generalitat de Catalunya for a Ph.D. Grant (FI-DGR 2014).We acknowledge support by the CSIC Open Access Publication Initiative through its Unit of Information Resources for Research (URICI).Peer Reviewe

Novel Topologies in Vanadium-bis-β-Diketone Chemistry: A [V4] and a [V6] Metallacyclophane