The local structures of 'host' and 'guest' layers of MoS 2 intercalated with M(OH) 2 (M = Mn, Co, and Ni) prepared via interaction of single-layer MoS 2 dispersions and solutions of M 2 + salts were studied by X-ray absorption spectroscopy. According to M K-edge extended X-ray absorption fine structure (EXAFS) and X-ray absorption near-edge structure (XANES) results, the electronic structure and atomic environment of the M atoms in the intercalates are similar to that of the crystalline hydroxides M(OH) 2 . In the Ni intercalate, Mo K-edge EXAFS revealed a structural change of the 'host' MoS 2 layers similar to that reported for water dispersions of MoS 2 single layers. S K-edge XANES data indicate that the change is associated with increased electron density on the S atoms in the matrix. SO 4 2 - and Mo n + (4 < n<6) were detected in the intercalated materials exposed to air, suggesting that transition metal intercalation may increase the susceptibility of the MoS 2 layers to oxidation.