The synthesis of nanoscale AlO(OH) hollow spheres was performed as described elsewhere (cf. [11]). In general, the micellar system was established by n-hexane as the non-polar dispersant phase, a mixture of methanol and water (1:1) as the polar phase, cetyltrimethylammonium bromide (CTAB) as surfactant and 1-hexanol as cosurfactant. At ambient temperature, Al(sec-OC 4 H 9 ) 3 was added to the dispersant phase of the equilibrated, transparent w/o-microemulsion and left to react for 12 h. The

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... repared hollow spheres were collected as a colorless solid by centrifugation and purified by sequential resuspension/ centrifugation in/from isopropanol. Finally, the as-prepared AlO(OH) hollow spheres were dried for 12 h while concurrently increasing the temperature (293 → 333 K) and reducing the pressure (1 → 10 −3 mbar) to remove all water/methanol inside of the inner cavity. Transmission electron microscopy (TEM) of the as-prepared AlO(OH) hollow spheres was performed on a Philips CM 200 FEG/ST microscope, operating at 200 kV. TEM samples were prepared by ultrasonic nebulisation of γ-AlO(OH) suspensions in pentane on a holey carbon-film copper grid. X-ray powder diffraction (XRD) and selective area electron diffraction (SAED) of nanoscale AlO(OH) hollow spheres Chemical composition and crystallinity of the as-prepared -AlO(OH) hollow spheres are confirmed by X-ray powder diffraction pattern as well as by selective area electron diffraction ( Figure S1 ). Both are in agreement to the expected Bragg peaks as reported for reference data. With regard to the XRD pattern the following aspects have to be considered. First, the scattering power is comparably weak due to the very thin crystalline sphere wall. Therefore, the Bragg peaks are broad and observed with low intensity. Second, the crystalline sphere wall does definitely not represent an isotropic bulk-crystal. As a consequence, the intensity as Electronic Supplementary Material (ESI) for Chemical Communications This journal is