Characterization of hybrid materials is crucial for gaining an in-depth understanding of nano-objects. Here, it is evidenced that the use of multinuclear 1H, 2H, 13C, 15N, 67Zn and 17O MAS NMR spectroscopy is a very powerful approach to acquire both structural and dynamic information on hybrid ZnO nanomaterials prepared from an organometallic approach. Not only is the coordination mode of the organic part onto the inorganic surface evidenced but also important information about the dynamics of the organic capping molecules and some particularities of the nanocrystal structure itself are obtained.