<jats:p>Crystal structures of (Z)-O-β-D-xylopyranosyl(1→6)-β-D- glucopyranosyloxy-NNO-azoxymethane (macrozamin) (1) and 5-O-methy-myo-inositol (sequoyitol) (4)-both of which are constituents of Macrozamia riedlei (Fisch. ex Gaud.) C. A. Gardn.-have been determined by X-ray diffraction. Diffractometer data at 295 K were refined by least-squares techniques to residuals of 0.050 (1537 'observed' reflections) for macrozamin and 0.060 (1052) for sequoyitol. Crystals of macrozamin are monoclinic, P2I, a 8.315(3), b 10.410(4), c 10.423(5) Ǻ, β 106.42(3)°, Z 2. Crystals of sequoyitol are triclinic, Pī, a 4.780(5), b 6.502(6), c 14.668(10) Ǻ, α 96.43(7), β 94.20(8), γ 109.31(8)°, Z 2.