Hybrid Cyclic Dimers of Divacant Heteropolyanions: Synthesis, Mass Spectrometry (MALDI‐TOF and ESI‐MS) and NMR Multinuclear Characterisation

In the field of organic‐inorganic hybrid composites, functionalized polyoxometalates constitute a special class of inorganic nanobuilding blocks (NBBs). This study represents a first approach related to the formation of new oligomeric hybrid species based on the reaction of bis(electrophilic) groups with a divacant heteropolyanion as the NBB. Bis(phosphonates) such as para ‐H 2 O 3 PCH 2 (C 6 H 4 ) n CH 2 PO 3 H 2 ( n = 1 or 2) have been treated with the divacant heteropolyanion [γ‐SiW 10 O 36 ] 8− to form the hybrid cyclic dimer [ H 2 {(SiW 10 O 36 )(O=PCH 2 (C 6 H 4 ) n CH 2 P=O)} 2 ] 6− . MALDI‐TOF and ESI mass spectrometry have been used as essential analytical techniques for the characterization of such composite systems. (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2004)