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Chapter 4 Unpublished Results Figure 4.4. Combined polyhedral/ball-stick representation of polyanions 24 and 25 emphasizing the two equivalent positions within the vacancy which is occupied by the disordered extra tungsten atom. In polyanions 24 and 25 each of the four lanthanide ions is bound to (Fe 16 P 8 W 49 ) via three μ 3 -oxo bridges coming from one Fe–O–Fe and two W–O–Fe bridges. In addition, the remaining coordination sphere is filled by five terminal aqua ligands, giving a total coordination number of eight for each lanthanide in a distorted square-antiprismatic geometry (see Figures 4.2 and 4.5). The Eu–O bond length ranges between 2.26(3) and 2.64(3) Å in 24, and the Gd–O bond length ranges between 2.29(3) and 2.53(3) Å in 25. Single-crystal XRD on the salts of polyanions 24 and 25 showed extra disordered lanthanide atoms acting as counter cations. These results were also confirmed by elemental analysis. 155
Chapter 4 Unpublished Results Figure 4.5. Side view of ball-and-stick representation of the Fe 16 cluster emphasizing the coordination of the four lanthanide ions. The color code is as follows: Fe (yellow); Ln (blue); H 2 O (pink); O (red). Bond valence sum (BVS) calculations for 24 and 25 are consistent with all tungsten atoms being in the +6 oxidation state, and all lanthanide and iron ions being in the +3 oxidation state. 16 In addition, 23 mono- and nine di-protonated oxygen atoms were identified in Fe 16 oxo cluster (see Figure 4.3). The ranges of BVS for mono- and di-protonated oxygen atoms are respectively 1.02 – 1.28 and 0.40 – 0.56. The six terminal oxygens of Fe1, Fe2, Fe15 and Fe16 are diprotonated and correspond to terminal water molecules (pink color in Figure 4.3). Furthermore, 20 of the 28 bridging Fe–O–Fe oxygens are monoprotonated (gray color in Figure 4.3). This leaves eight other bridging oxo atoms. The six bridging Fe3–Fe5, Fe4–Fe6, Fe7–Fe9, Fe8–Fe10, Fe11–Fe13 and Fe12–Fe14 (turquoise color in Figure 4.3) show a BVS range of 0.59 – 0.67, which is between mono- and diprotonation and led us to believe that we are looking at three water and three hydroxo ligand disordered over these six sites. This type 156
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