The nanobeam electron diffraction (NBED) patterns of selected areas of sheaf-type MOF-NiCl2 consist of well-defined sharp spots indicating single-crystallinity (Figure ). The analyzed fantail nanorods are isomorphous crystals. However, the spatial orientation (based on the electron diffraction data) of individual nanorods deviates slightly (~3°) from each other. Such a minor deviation in the spatial orientation between neighboring nanorods is typical for superstructures formed by a non-crystallographic branching mechanism. This misorientation results in the overall polycrystalline character of the sheaf-like superstructures. The electron diffraction from the free bridge was opaque for electrons, and no information could be obtained about the crystallographic properties. Therefore, diffraction data was obtained at the thinner edges. MOF-NiCl2 and MOF-NiBr2 are isomorphous, as indicated by PXRD, and is confirmed by the symmetry match of the NBED for MOF-NiCl2 with zone-axis patterns calculated from the refined structure of MOF-NiBr2 (Figure ). By indexing hkl reflections we can infer that the orientation of the nanorods is correlated with their shape. The long direction of the rods runs along the a-axis and the crosssection of the rods is the bc-plane. The plane of the metal atoms on the b-axis are parallel to one of the side faces and the radial fan direction is coincident with the <101> direction of the nanorods. The channels along the c-axis are inclined with respect to radial fan direction. The diffraction patterns of the minor rod-like product of MOF-NiCl2 (Figure ) show that these structures are isostructural with both the sheaf-like crystals of MOF-NiCl2 and with MOF-NiBr2.