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The reaction of trinuclear molybdenum cluster{Mo_3S_4(μ-dtp)(dtp)_3(H_2O)}1[dtp=S_2P(OEt)_2]with RCO_2Na(R=H,CH_3)in the presence of Py gave the black compounds{Mo_3S_4(μ-O_2CR)(dtp)_3(Py)}(2,R=H,3,R=CH_3).Both compounds are characterized by X-ray crystallo-graphy.It is shown that crystals 2 and 3 belong to space group P with Z=2 and a=10.519(2),b=12.121(2),c=15.757(2),α=93.27(1),β=94.63(1),γ=105.22(1)°,V=1925~3 for crystal 2,whereasa=9.556(2),b=14.067(7),c=15.914(9),α=101.41(4),β=101.44(4),γ=74.26(3)°,V=1994~3for crystal 3.The final R factors are 0.041 and 0.048 for crystal 2 and 3 respectively.The structureanalysis indicates that(O_2CR)~- ligand selectively substitutes the bridging(dtp)ligand.This type ofMo_3 cluster molecule where structure contains two species of bidentate ligand is for the first time tobe obtained by us.
The reaction of trinuclear molybdenum cluster {Mo_3S_4 (μ-dtp) (dtp) _3 (H_2O)} 1 [dtp = S_2P (OEt) _2] with RCO_2Na (R = H, CH_3) in the presence of Py gave the black compounds { Mo3S_4 (μ-O_2CR) (dtp) _3 (Py)} (2, R = H, 3, R = CH_3) .Both compounds are characterized by X-ray crystallo- graphy. It is shown that the crystals 2 and 3 belong to space group P with Z = 2 and a = 10.519 (2), b = 12.121 (2), c = 15.757 (2),? = 93.27 (1),? = 94.63 (1),? = 105.22 , V = 1925-3 for crystal 2, wherea = 9.556 (2), b = 14.067 (7), c = 15.914 (9),? = 101.41 (4),? = 101.44 (4),? = 74.26 ) °, V = 1994 ~ 3 for crystal 3. The final R factors are 0.041 and 0.048 for crystal 2 and 3 respectively.The structure analysis indicates that (O_2CR) ~ - ligand selectively substitutes the bridging (dtp) ligand. This type of Mo_3 cluster molecule where structure contains two species of bidentate ligand is for the first time tobe obtained by us.