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.
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