The structure of Ni(OH)(2)/MoS2 nanocomposite material obtained via MoS2 single-layer dispersion and the products of its annealing in the 100-400 degrees C temperature range were studied using X-ray diffraction (XRD) and X-ray absorption fine structure (XAFS). The transformation of the initial MoS2 superlattice structure with Mo-Mo bonding to the usual structure with unique Mo-Mo distance was found to occur upon annealing. The decomposition of two-dimensional Ni(OH)(2)-like species in the interlayer space of MoS2 at 400 degrees C leads to complete substitution of O by S in the Ni local environment.