-Fe
2O
3 has been synthesized with an ordered mesoporous structure and crystalline walls thatexhibit a near-single crystal-like order. The unique magnetic beha
vior of the material, distinct from bulknanoparticles of
-Fe
2O
3 or mesoporous Fe
2O
3 with disordered walls, has been established. Magneticsusceptibility, Mössbauer, and neutron diffraction data show that the material possesses the same long-range magnetic order as bulk
-Fe
2O
3, despite the wall thickness being less than the 8 nm limit belowwhich magnetic ordering breaks down in nanoparticulate
-Fe
2O
3, yet the Morin transition of bulk
-Fe
2O
3is absent. It is also shown by TEM, PXRD, and EXAFS that
-Fe
2O
3 with the same ordered mesoporousstructure but disordered walls contains small crystalline domains. Mössbauer and magnetic susceptibilitydata demonstrate that this material exhibits no long-range magnetic order but superparamagnetic beha
vior.