Crystalline samples were obtained through the slow evaporation of organic solvents, as outlined in Supplementary Information Section 11. This process typically yields products in the form of either polycrystalline powders or single crystals, which were categorized using our AI-enhanced computer vision system, as described previously and in Fig. . When single crystals were directly isolated in vials, as shown in Fig. , promising crystals of appropriate size were selected and stored in designated sample pockets. These samples were subsequently analyzed using HT single-crystal diffraction experiments at the Shanghai Synchrotron Radiation Facility, specifically at the Beamline BL10U2. This beamline is equipped with state-of-the-art instrumentation, including a robotic arm, which automates sample loading and facilitates HT data collection. The integration of advanced robotic systems and synchrotron technology greatly accelerates the structural determination process. For polycrystalline powders, laboratory powder X-ray diffraction (PXRD) was used to collect diffraction patterns. These experimental patterns were then compared with simulated patterns derived from known single-crystal structures to determine the phase identity of the polycrystalline samples, as shown in Fig. and Supplementary Fig. . If no match was found between the experimental and simulated patterns, it indicated the need for further experiments. In such cases, we proceeded with recrystallization to promote the formation of single crystals from the polycrystalline material. The newly obtained single crystals were then subjected to single-crystal diffraction analysis, enabling us to resolve their structures accurately.