Present work reports the synthesis of zirconium phosphate nanoparticles containing dirhenium(III) substance bis-dimethylsulfoxide-cis-tetrachlorodi-?-pivalatodirhenium(III) with formula cis-Re2(C(CH3)3COO)2Cl4?2DMSO (I) and q-zirconium phosphate with formula q-Zr(HPO4)2?6H2O (ZrP). The intercalation process was monitored by EAS. Due to the spectral characteristics of the quadruple bond the conclusion was made that the obtained intercalated compounds had cis-configuration of ligands around cluster dirhenium fragment. The proposed mechanism of intercalation includes the substitution of the axial ligands of I by phosphate groups of ZrP first on the surface of ZrP, than in the inner layers. Two received products of the intercalation were characterized by SEM, XRPD, FT-IR, TGA analysis witnessing about successful intercalation process. The formation of new phases with interlayer distances of 10.53 - 16.6 ? was found, the average size of obtained platelets was 100-200 nm.