C5Me4(benzyl)H reacted with Mo(CO)6 in refluxing xylene to give the new complex(C5Me4benzyl)2Mo2(CO)6.Its molecular structure was characterized by elemental analysis,IR spectra,1H NMR and X-ray diffraction.Crystal data for this compound:Triclinic,space group P1,Mr=782.56,a=0.854 43(17) nm,b=0.991 0(2) nm,c= 1.035 5(2) nm,α=67.25(3)°,β=87.38(3)°,γ=85.99(3)°,V=0.806 4(3) nm3,Z=1,Dc=1.611 g·cm3,μ(Mo Kα)=0.825 mm-1,F(000)=398,R=0.032 9,wR=0.083 6(observed reflections with Ⅰ>2σ(Ⅰ)) and R=0.036 2,wR=0.084 3(all reflections).The X-ray crystal structure of the dimer confirms the structure with terminal CO groups and the Mo-Mo bond distance is 0.326 6 nm.CCDC:693386.