gamma-Zirconium and gamma-titanium phosphates (gamma-ZrP, gamma-TiP) with layered structure are well known as ion exchangers as well as agents intercalating organic bases. In the latter case, the intercalation compounds may exchange transition metal ions coordinated by the ligands, giving rise to in situ formed complexes. We prepared phases derived from gamma-ZrP, containing organic diamines (gamma-ZrPL) (L = ligand), such as 2,2＇-bipyridyl (bipy), 1,10-phenanthroline (phen), and 2,9-dimethyl-1,10-phenanthroline (dmp). These materials exchange Pd2+ ions when they are in batch contact with a PdCl2 solution and this produces solids with Pd2+/L = 1. The X-ray diffraction (XRD) patterns of some materials containing Pd2+ showed an increase of 2 Angstrom in d(002). The differential thermal analysis (DTA) curves of the Pd2+ materials showed a lowering of diamine temperature decomposition (100 degrees C) with respect to those of their precursors. In the case of gamma-TiP, we also obtained intercalation compounds with the above-mentioned diamines : Similar experiments showed that gamma-TiPL exchanges very few Pd2+ ions, except for the one derived from gamma-TiPdmp. The thermogravimetric (TG) curves show the same lowering of ligand temperature decomposition for all materials except gamma-TiPPdphen. The XRD patterns for all gamma-ZrPPdL and gamma-TiPPdL materials show peaks at d(hkl) = 7.89, 8.59-8.04, and 9.31 Angstrom, for compounds containing Pdbipy, Pdphen, and Pddmp, respectively. Due to the correspondent complexes into the exchanger, these peaks disappeared when the materials, except for those containing the Pddmp complex, were stirred into CH2Cl2.