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Polyoxometalate molybdenum blue (MB) complexes typically exist as discrete multianionic clusters and are composed of repeating Mo building units. MB wheels such as {Mo 176 } and {Mo 154 } are made from pentagon-centered {Mo 8 } building blocks joined by equal number of {Mo 1 } units as loin, and {Mo 2 } dimer units as skirt along the ring edge, with the ring sizes of the MB wheels modulated by the {Mo 2 } units. Herein we report a new class of contracted lanthanide-doped MB structures that have replaced all the {Mo 2 } units with lanthanide ions on the inner rim, giving the general formula {Mo 90 Ln 10 }. We show three examples of this new decameric {Mo 90 Ln 10 } (Ln = La, Ce, and Pr) framework synthesized by high temperature reduction and demonstrate that later Ln ions result in {Mo 92 Ln 9 } (Ln = Nd, Sm), conserving one {Mo 2 } linker unit in its structure, as a consequence of the lanthanide contraction. Remarkably the {Mo 90 Ln 10 } compounds are the first examples of charge-neutral molybdate wheels as confirmed by BVS, solubility experiments, and redox titrations. We detail our full synthetic optimization for the isolation of these clusters and complete characterization by X-ray, TGA, UV-vis, and ICP studies. Finally, we show that this fine-tuned self-assembly process can be utilized to selectively enrich Ln-MB wheels for effective separation of lanthanides.

Synthesis, Assembly, and Sizing of Neutral, Lanthanide Substituted Molybdenum Blue Wheels {Mo90Ln10}

Synthesis, Assembly, and Sizing of Neutral, Lanthanide Substituted Molybdenum Blue Wheels {Mo₉₀Ln₁₀}