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Chapter 3 Published Results tetrahedral hetero group. The claw-shaped [As 2 W 19 O 67 (H 2 O)] 14− (As 2 W 19 ) precursor is a member of this subclass, and its structure can be rationalized as two [B-α-AsW 9 O 33 ] 9− (AsW 9 ) units linked through a WO 6 group via four equatorial W-O-W bonds and two trans-related terminal oxo and aqua ligands (see Figure 3.19). The dilacunary As 2 W 19 was first reported by Tourné et al. in 1973, 7 and its structure was confirmed later by our group using single-crystal X-ray diffraction. 8 Figure 3.19. Ball-and-stick representation of the dilacunary polyanion precursor [As 2 W 19 O 67 (H 2 O)] 14− (As 2 W 19 ). The color code is as follows: W (black), As (yellow), H 2 O (pink), O (red). Incorporation of an additional W-bridge in the dilacunary As 2 W 19 unit results in the monolacunary [As 2 W 20 O 68 (H 2 O)] 10− (As 2 W 20 ), which was first reported by Hervé and coworkers (see Figure 3.20). 9 Interaction of As 2 W 19 with di- and trivalent transition metal and main group elements has been investigated by different groups and has resulted in the 97
Chapter 3 Published Results expected disubstituted products [M 2 As 2 W 19 O 67 (H 2 O) 3 ] n− (n = 10; M = Mn 2+ , Co 2+ , Ni 2+ , Cu 2+ , Zn 2+ , VO 2+ ; n = 8; M = Mn 3+ , Fe 3+ , Ga 3+ ) . 10 Figure 3.20. Ball-and-stick representation of the monolacunary polyanion precursor [As 2 W 20 O 68 (H 2 O)] 10− (As 2 W 20 ). The color code is the same as in Figure 3.19. Our group has also been working in the area of lanthanide-containing polyoxotungstates and we have isolated species incorporating between one and twenty lanthanide centers. 11 We have also investigated the interaction of both As 2 W 19 and As 2 W 20 with ytterbium(III) in aqueous acidic (pH = 2) medium, resulting in both cases in [YbAs 2 W 20 O 68 (H 2 O) 3 ] 7− . 11a This polyanion consists of two AsW 9 units connected by a triangular [YbW 2 O 2 (H 2 O) 3 ] 11+ unit which is composed of two 6-coordinated tungsten centers and a 7-coordinated Yb III ion, all carrying one terminal water ligand. 11a Now, we have focused on the reactivity of lanthanide ions with lone pair-containing lacunary POM precursors such as As 2 W 19 and AsW 9 . This work has resulted in the synthesis and structural characterization of two lanthanide-containing 19-tungsto-2-arsenates(III) reported herein. 98
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