Our research group has long been engaged in the design, synthesis, assembly process and mechanism of 3d metal coordination molecular clusters and lay a good foundation in the directional design, controllable preparation and performance regulation of coordination molecular clusters3. Relying on the relevance of solid-liquid structure information, we establish a real-time monitoring mechanistic research method for the coordination cluster assembly process using the combination of crystallography and mass spectrometry. For the directional construction of cubane structure, we successfully prepared a series of molecular clusters with a cubane structure (Table S5),