Overall, 366 precursor combinations were screened using the same reaction conditions (0.0092 M, 1 mL total volume, CHCl3, RT, 5 days) in 48-well plates. Stock solutions (5-6 mg/mL) of each precursor were transferred from 24-well plates (max. 4 mL volume) into the reaction vials (max. 2 mL volume) in the 48-well plates, before being made up to a total volume of 1 mL using the reaction solvent, ensuring the same overall concentration for each combination. Full experimental conditions are given in the Tables . In addition to the 366 precursor combinations, reactions were repeated across the separate runs in different plate positions to confirm the reproducibility of the workflow. On reaction completion, the turbidity was determined (see automated analysis section), before an EquaVAP was used to remove the reaction solvent from all wells in parallel under a flow of nitrogen. The reaction well-plates were subsequently returned to the OT-2 deck to prepare the samples for characterisation. Both NMR and mass spectroscopy samples were prepared on the platform and dispensed directly into tubes and vials in either a custom 3D-printed 96-NMR tube rack or compatible 54-well plates for the mass spectrometer, respectively. The prepared samples were subsequently submitted for analysis, using a Bruker SampleJET autosampler allowing up to 5 x 96 samples to be queued for 1 H NMR analysis, and direct injection on a high-resolution mass spectrometer (HRMS). Full details for each step of the automated high-throughput screen and data curation are outlined in the Supporting Information and available on GitHub ().