Present work reports the synthesis of zirconium phosphate nanoparticles containing dirhenium(III) substance bis-dimethylsulfoxide-cis-tetrachlorodi-μ-pivalatodirhenium(III) with formula cis-Re 2 (C(CH 3 ) 3 COO) 2 Cl 4 • 2DMSO (I) and θ-zirconium phosphate with formula θ-Zr(HPO 4 ) 2 • 6H 2 O (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 Å was found, the average size of obtained platelets was 100-200 nm.