TiO2 and related titanium oxide materials are widely used in the field of photolysis of hydrogen from aquatic products, and have important research significance for developing clean energy and reducing environmental pollution. In recent years, the synthesis and characterization of titanium-oxygen clusters have been a hotspot in the field of inorganic and material chemistry as simulating molecules for the structure and properties of TiO2 materials. How to prepare high-titanium oxygen cluster molecules that can rival the size of TiO2 nanoparticles and have high-efficiency and stable photolysis of water-producing hydrogen is a key scientific problem in this field. State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Structures, Chinese Academy of Sciences, Zhang Jian and Zhang Lei, Inorganic Synthetic Chemistry Team led by the Ministry of Science and Technology, “973†Program, “Inorganic-Organic Hybrid Functional Materials†Innovation Group, Strategy of the Chinese Academy of Sciences Under the support of the Special Pilot Science and Technology Program (Class B) and the National Outstanding Youth Fund, a step-by-step approach was adopted to expand Ti6 oxygen clusters from Ti6 oxygen clusters and remove the organic hindered ligand to obtain Ti17 oxygen clusters, further increasing the assembly concentration. The highest nucleus Ti52 oxygen clusters have been prepared. The cluster size reaches 3.6 nm. These cluster materials all have high air and aqueous stability and can maintain their structure in the pH range of 3-13. UV-driven photocatalytic decomposition of hydrogen from aquatic products shows that these titanium oxide clusters have good catalytic activity and stability, and also exhibit interesting cluster size effect, in which the hydrogen production efficiency of Ti52 oxygen cluster is Ti6. double. This research result not only provides an effective solution for the construction of high-nuclear titanium-oxygen cluster molecules, but also can provide reference for studying the structure-performance structure-activity relationship of titanium oxide nanoparticles. Related results have been published online at J. Am. Chem. Soc. 2016, 10.1021/jacs.6b03489. The research team previously synthesized the world’s first fullerene-type titanium oxygen cluster (J. Am. Chem. Soc. 2016, 138, 2556) and systematically investigated the energy band regulation of titanium oxide clusters (Angew. Chem Int. Ed. 2016, 55, 5160) and the preparation of titanium oxide cluster supported metal-organic framework films (ACS Nano 2016, 10, 977). Flashlight,Flashlight Rechargeable,LED Flashlight,USB Rechargeable Flashlight,Blaze Flashlight Yuyao Flylit Appliance Co.,Ltd , https://www.flylitlight.com