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Chapter 1 Introduction - 2 γ-[XM 12 O 40 ] n− γ-[XM 10O 36 ] n− Figure 1.8 Dilacunary species derived from the γ-Keggin structure. The color code is the same as in Figure 1.5. 1.4 Wells‐Dawson‐type POMs and derivatives In 1952, Wells synthesized the 18-tungstophosphate complex and proposed its structure as [P 2 W 18 O 62 ] 6− afterwards, in 1953, the structure was determined by a single-crystal X-ray diffraction by Dawson and the structure was named after them. 1a This is now known as α- [P 2 W 18 O 62 ] 6− “Wells-Dawson” structure which consists of two A-α-[PW 9 O 34 ] 9− units (trilacunary Keggin) fused into a cluster of virtual D 3h symmetry. The structure involves two types of tungsten atoms, six ”polar” and twelve “equatorial” forming the two caps and the two belts of the polyanion, respectively. Each cap is composed of three edge-shared octahedra (triad), whereas the two belts are formed via alternative corner- and edge-shared MO 6 units, as depicted in Figures 1.3-b and 1.9. It is noteworthy that the Wells-Dawson structure is known for the heteroatoms P(V), As(V), and S(VI) and for the addenda atoms W(VI) and Mo(VI). The β isomer can be formed by a 60˚ rotation of one cap, reducing the symmetry from D 3h to C 3v . The α and β isomers have been distinguished by 183 W-NMR technique. 15
Chapter 1 Introduction α-[P 2 W 18 O 62 ] 6− - n n = 1 n = 3 n = 6 α 2 -[P 2 W 17 O 61 ] 10− [P 2 W 15 O 56 ] 12− [H 2 P 2 W 12 O 48 ] 12− Figure 1.9 Polyhedral representation of lacunary species of the Wells-Dawson structure. WO 6 octahedra (red), PO 4 tetrahedra (green). 1.4.1 The Mono‐ and tri‐lacunary species Some vacant species corresponding to the complete α-[P 2 W 18 O 62 ] 6− (P 2 W 18 ) anion can be formed and isolated in aqueous solution depending on the pH and counter-cations present during their synthesis. The monovacant anion [P 2 W 17 O 61 ] 10− (P 2 W 17 ) is isolated as a 16
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