This work investigates synthesizing of MnPS3 layered compound and its intercalation with pyridinium ion (PyH+). The XRD results indicate that there are four phases due to intercalation with different d-spacing, d = 9.7, 10.6, 7.3 and 12.3 Angstrom. These phases are related to the guest positions in the interlayer of the P2S64-, except the d = 7.3 A phase. There are some factors help to control the intercalation and orientation of intercalated compound, such as, temperature during XRD scan and stirring time. The guest intercalation leads to a change in symmetry of the host lattice from C2/m to R3m. The XRD pattern (d = 9.7 A) for the resultant compound of the formula, Mn0.854PS3(PyH+)(0.293)(H2O)(0.322) (X = 0.146 and y = 0.322) indicates that the intercalated compound could be described by a trigonal unit cell and the lattice parameters a = b = 3.50263 Angstrom, c = 29.07435 Angstrom and y = 120degrees. As well as, the trigonal unit cell could describe the other phases with different c-parameter length of each phase. IR spectra confirmed the intercalation. (C) 2003 Elsevier B.V. All rights reserved.