A flow-system array for the discovery and scale up of inorganic clusters

The batch synthesis of inorganic clusters can be both time consuming and limited by a lack of reproducibility. Flow-system approaches, now common in organic synthesis, have not been utilized widely for the synthesis of clusters. Herein we combine an automated flow process with multiple batch crystallizations for the screening and scale up of syntheses of polyoxometalates and manganese-based single-molecule magnets. Scale up of the synthesis of these architectures was achieved by programming a multiple-pump reactor system to vary reaction conditions sequentially, and thus explore a larger parameter space in a shorter time than conventionally possible. Also, the potential for using the array as a discovery tool is demonstrated. Successful conditions for product isolation were identified easily from the array of reactions, and a direct route to 'scale up' was then immediately available simply by continuous application of these flow conditions. In all cases, large quantities of phase-pure material were obtained and the time taken for the discovery, repetition and scale up decreased.