Abstract: Empty fruit bunches are a lignocellulosic waste byproduct of palm oil production. As is typical for many such fibres from a waste stream, the utilization of these fibres as material, or source of carbon for the production of bioethanol, is hampered by a poor knowledge of the solid state polymer nanostructure where a long fibrous crystalline polymer is embedded in an amorphous matrix. In this study we characterize the bionanocomposite structure, long fibrous cellulose crystals in an amorphous matrix, with X-ray scattering and solid state NMR of empty fruit bunches. Our aim is to provide a structural basis to understand the processing of fibres and their degradation. X-ray scattering both at small and wide angles provided a complementary perspective on the fundamental unit of cellulose organization, long fibrous crystallites called microfibrils: the spiral angle of microfibrils around fiber axis; and the organization of individual cellulose chains in the crystallites. Solid state NMR provides structural and compositional perspectives on the amorphous component. Some general comments on the complementary use of these two techniques in biofibers are given.