Synthesis and Structural Characterization of Multi- Molybdenum-Substituted Preyssler-type Phosphotungstates

We report the synthesis of multi-Mo-substituted Preyssler-type phosphotungstates, [P5W30-xMoxO110Na(H2O)](14-), with different amounts of incorporated Mo via the hydrothermal reactions of H3PO4, Na2WO4, and Na2MoO4; and characterization by P-31 nuclear magnetic resonance (NMR), Fourier-transform infrared (FT-IR), elemental analysis, electrospray ionization-mass spectrometry (ESI-MS), and cyclic voltammetry. The number of substituted Mo increases by increasing the amount of Na2MoO4 in the reaction mixture, and in the [P5W30-xMoxO110Na(H2O)](14-) up to penta-Mo-substituted species can be produced as mixtures of isomers with different Mo numbers and Mo positions. Single crystal X-ray structure analysis and density functional theory calculation indicate that the most suitable substitution position is the belt position.

Automated summary

This study reports the synthesis of multi-Mo-substituted Preyssler-type phosphotungstates via hydrothermal reactions. The number of substituted Mo increases with the amount of Na2MoO4 in the reaction mixture, and the most suitable substitution position is the belt position.