The sheaf-like metallo-organic crystals (MOF-NiCl2) are formed under solvothermal reaction conditions. The ligand (CSB) was reacted with nickel dichloride (NiCl2) in a chloroform/dimethyl-formamide (DMF) solution (1:3 v/v) for 5 days at 105 °C. The molar ratio of NiCl2:CSB = 2:1 (Scheme 1a). Scanning electron microscopy (SEM) and optical images showed the formation of sheaf-like superstructures with two fantails consisting of a closely packed bundle of nanorods (Figure ). These nanorod aggregates are arranged around one central rod. Analysis of the morphology indicate a high level of uniformly: individual sheafs have a length of 12.0 ± 2.5 μm and the width of the fantails are in the range of 9.2 ± 2.8 μm (Figure ). Each fantail consists of 25 ± 4 nanorods, as indicated by examining 20 sheafs. The individual nanorods of the fantails have cross sections 1.2 ± 0.3 μm and the length of the free bridge of the central rod is 4.6 ± 0.9 μm (estimated from 30 crystals). Moreover, we see that both fantails of the individual sheaf-like superstructures are similar in size and composition. We also observed some relatively small, isolated rods (l = 4.0 ± 1.1 µm) as a minor product (Figure ).