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A novel synthetic pathway to obtain the first Zn6 hexagon tungstoantimonate [(Zn(H2O))6(B-α-SbW9O33)2]6- ([Zn6-α-SbW9] (1)) via rearrangement of a non-lacunary Krebs-POM precursor (C12N4H11)4K4[(Mn(H2O)3)2((Mn0.5W0.5)O2)2(B-β-SbW9O33)2] ([Mn-β-SbW9]) has been developed. Addition of ortho-phenylenediamine (opda) in order to optimize the synthesis of [Mn-β-SbW9] led to the crystallization of a novel Krebs-type Zn-POM (C12N4H11)4Na5[((Zn0.8W0.2)(H2O)3)2((Zn0.2W0.8)O2)2(B-β-SbW9O33)2] ([(Zn/W)2-β-SbW9] (2)) comprising four disordered Zn-centers after replacement of MnCl2 with ZnCl2. The compounds were characterized in the solid state by single-crystal and powder X-ray diffraction (XRD), IR spectroscopy, thermogravimetric analysis (TGA) and elemental analysis and in solution by UV-vis spectroscopy and ESI-mass spectrometry. The Krebs-POM archetype and the Zn6 hexagon tungstoantimonate have been investigated towards their interactions with Human Serum Albumin (HSA) as a model protein using SDS-PAGE and trypthophan fluorescence quenching.

Synthesis of the first Zn6-hexagon sandwich-tungstoantimonate via rearrangement of a non-lacunary Krebs-type polyoxotungstate

Synthesis of the first Zn₆-hexagon sandwich-tungstoantimonate via rearrangement of a non-lacunary Krebs-type polyoxotungstate