The ligands (C5Me4R) [R =n-Butyl (1), Benzyl (2), PhMe-2 (3)] reacted with Ru3(CO)12 in refluxing xylene to give corresponding new substituted tetramethylcyclopentadienyl diruthenium metal carbonyl complexes [(η5-C5Me4R)Ru(CO)( μ-CO)]2 [R=n-Butyl (4), Benzyl (5), PhMe-2 (6)], respectively. The three new complexes were characterized by elemental analysis, IR and 1H NMR spectra. The crystal structure of complex 5 was determined by single crystal X-ray diffraction. The X-ray crystal structure of complex 5 confirms the structure with bridging and terminal CO groups. CCDC: 709601.
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.
The complex(C5Me4iBu)2Ru2(CO)4 has been synthesized by the reaction of C5Me4iBuH with Ru3(CO)12 in refluxing xylene and its molecular structure was characterized by elemental analysis,IR spectra,1H NMR and X-ray crystal structure determination.Crystal data for this compound:Triclinic,space group P1,Mr=668.78,a=0.865 96(17)nm,b=0.892 90(18)nm,c=0.975 7(2)nm,α=88.39(3)°,β=71.64(3)°,γ=84.99(3)°,V=0.713 3(2)nm3,Z=1,Dc=1.557 g.cm-3,μ(Mo Kα)=1.091mm-1,F(000)=342,R1=0.025 3,wR2=0.067 6(observed reflections with I>2σ(I))and R1= 0.026 9,wR2=0.068 2(all reflections).The structure of the dimer confirms the structure with bridging and terminal CO groups,and the Ru-Ru bond distance is 0.275 19(8)nm.CCDC:693389.
