STRUCTURE OF {Mo_4S_4(μ-OAc)_2[S_2P(OC_2H_5)_2]_4H}

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{Mo4S4(μ-OAc)2(dtp)4H}3,(dtp=S2P(OEt)2),Mr=1371.60,Or-thorhombic, space group Pcab, a = 18. 90 (2) ,b = 21. 678 (4 ) , c = 24. 491 (4 ) A , V = 10031(7)A3,Z=8,Dc=1.818g/cm-3,F(000)=5464,λ(MoKa)=0.71073A,finalR= 0. 069 for 3738 independent reflections. This is a successful example of the formation of [Mo4S4]5+ from[3+1] reaction mode. The results of the structure determination indicate that the configuration of the title compound exhibits a tetranuclear cubane-type core [Mo4S4]5+ with six Mo - Mo distances in the range 2. 685~2. 969A and is very similar to that of the previously characterized compound {Mo4S4(μ-OAc)2(dtp)4}2, [Mo4S4]6+, which was obtained directly by the reaction of MoCl3·3H2O with dtp. Some notable differences, however, can be found when six Mo - Mo bond distances and bonding parameters of the four terminal bidentate ligands (dtp) are compared between these two compounds , That can be attributed to the difference in the oxidation state of these two clusters . {Mo4S4 (μ-OAc) 2 (dtp) 4H} 3, (dtp = S2P (OEt) 2), Mr = 1371.60, Or-thorhombic, space group Pcab, a = 18. 90 (2), b = 21. 678 (4), c = 24. 491 (4) A, V = 10031 (7) A3, Z = 8, Dc = 1.818 g / cm -3, F (000) = 5464, λ (MoKa) = 0.71073A , finalR = 0. 069 for 3738 independent reflections. This is a successful example of the formation of [Mo4S4] 5+ from [3 + 1] reaction mode. The results of the structure determination indicate that the configuration of the title compound exhibits a MoS4] 5+ with six Mo-Mo distances in the range 2. 689 ~ 2.969A and is very similar to that of the previously characterized compound {Mo4S4 (μ-OAc) 2 (dtp) 4} 2, [Mo4S4] 6+, which was obtained directly by the reaction of MoCl3 · 3H2O with dtp. Some notable differences, however, could be found when six Mo - Mo bond distances and bonding parameters of the four terminal bidentate ligands (dtp) are compared between these two compounds, That can be attributed to the difference in the oxidation state of these two clusters.
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