Synthesis and Structural Characterization of ... - Jacobs University

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Chapter 4 Unpublished Results Figure 4.2. Combined polyhedral/ball-and-stick representation of open-ring-shaped polyanions 24 and 25. The color code is as follows: WO 6 octahedral (red); PO 4 tetrahedral (green); W (black); Fe (yellow); Ln (blue); H 2 O (pink); O (red). Furthermore, The Fe 16 nanocluster ring is cleaved between four Fe centers (Fe1–Fe2 from one side and Fe15–Fe16 from the other). Fe1 and Fe2 ions are connected with an extra tungsten atom through two μ 2 -oxo bridges one each with average Fe–O bond lengths ca. 1.96 Å (see Figure 4.3). This extra tungsten atom in 24 and 25 is by its turn connected to the novel open-ring P 8 W 48 * fragment through one μ 4 -oxo bridge and two μ 2 -oxo bridges. 153
Chapter 4 Unpublished Results Figure 4.3. Ball-and-stick representation of {Fe 16 O 2 (OH) 23 (H 2 O) 9 WO 3 } showing the protonation within the cleaved Fe 16 cluster and its coordination to the extra tungsten. The color code is as follows: W (black); Fe (yellow); O (red); HO as mono-protonated μ 2 -oxygen (gray); H 2 O as di-protonated μ 2 -oxygen (pink); disordered H 2 O or HO as protonated μ 2 - oxygen (turquoise). It is noteworthy that in the solid state the extra tungsten atom is disordered over two positions with 60/40 % occupancy within the cavity which due to the C s symmetry of the molecule. In other words, the cleavage of the original cyclic P 8 W 48 unit to form the open-ring P 8 W 48 * has led to an available vacancy with four basic oxygens. This vacancy however could only be occupied by one extra tungsten(VI) atom. Due to the equivalency of the two positions within the vacancy, the extra tungsten is disordered in the solid state over these two positions (see Figure 4.4). 154
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