Abstract: This paper reports the ⁹⁵Mo and ³¹P NMR results of a series of heterometallic cluster compounds containing coinage metal and tetraselenomolybdate.The investigation results indicate that ⁹⁵Mo NMR chemical shifts and linewidths are not only related to the number of coordination of Cu atoms, but also very sensitive to structural variations.The ⁹⁵Mo NMR shielding effect is mainly caused by the coiage metal atoms in the tetraselenomolybdate system and the shielding order is Au > Cu > Ag.The saturation of Mo nucleus shielding effect from the coordination of MoSe₄ moiety by four Cu atoms and very little influence on ⁹⁵Mo nucleus from the outsphere ligands are observed. Additionally, kinetic ⁹⁵Mo NMR technique was used to monitor ligand substitution reactions and cluster skeleton transformation processes from MoCu₄ to MoCu₁₀ cores. A variety of characteristics of the ³¹P NMR chemical shifts of Mo(W)-Cu(Ag, Au)-Se compounds among different structural types are also discussed.

Key words: ⁹⁵Mo NMR, ³¹P NMR, Heteroseleometallic compounds, Tetraselenomolybdate