Layered organic-inorganic hybrid materials represent a quasi-two-dimensional system that may exhibit interesting behaviour. Transition metal ions were incorporated in a tungsten oxide/alpha,omega-diaminoalkane layered hybrid system via three synthesis techniques. X-ray diffraction indicates an expansion of the interlayer spacing with increasing alkyl length. Infrared vibrational spectra of hybrid manganese tungstate hybrid compounds demonstrate that the inorganic framework is unaltered with different intercalates, and that the organic amines are included as neutral species. The magnetic behaviour of a variety of the compounds demonstrates low-dimensional behaviour, with 2D-3D coupling at low temperatures. Manganese tungstate hybrids exhibit antiferromagnetic correlations, while a nickel tungstate hybrid studied indicates ferromagnetic correlations and forms a spin-canted antiferromagnet. AC susceptibility measurements of iron tungstate hybrids reveal spin-glass-like behaviour. (c) 2005 Elsevier B.V. All rights reserved.