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Compounds with ordered structures in one or two dimensions are exciting materials and investigated intensively in many different areas of science. Many activities have been put into the preparation of low‐dimensional nano‐scaled structures and many compounds in this size regime are known. Contrary, the number of known compounds that have low‐dimensional macroscopic sized structures that form directly in a chemical reaction is very limited. Here, we present the synthesis of the niobium cluster compound [(Et 2 O) 2 H] 2 [Nb 6 Cl 18 ], crystals of which grow in form of large hexagonal empty tubes of several centimeter length and diameters in the range of 2 mm. The single‐crystal X‐ray structure of this compound has been refined. Under warming, the compound readily eliminates diethyl ether molecules and decomposes. From a closer look at the crystallization process a step‐by‐step scheme of the procedure of the tube growth is proposed. The overall conclusion from this proposal is that a crucial balance between the cluster solution concentration, the crystal growth speed and the ether diffusion speed results in the formation of macroscopic crystal tubes.

A Hexanuclear Niobium Cluster Compound Crystallizing as Macroscopic Tubes