Syntheses,crystal structures,and characterizations of two novel cubane-like and double cubane-like molybdenum-copper-sulphur clusters {MoCu3S3(S2COEt)}(O)(Ph3P)3 and {Mo2Cu6S6(SCMe3)2}(O)2(Ph3P)4 |
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Authors: | Nianyong Zhu Shaowu Du Pengcheng Chen Xintao Wu |
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Institution: | (1) State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, 350002 Fuzhou, Fujian, P. R. China |
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Abstract: | Two novel heterometallic cubane-like and double cubane-like clusters, {MoCu3S3(S2COEt)}(O)(Ph3P)3
I and {Mo2Cu6S6(SCMe3)2}(O)2(Ph3P)4
II, were synthesized by reaction of {MoCu2S3}(O)(Ph3P)3 with CuS2COEt and CuSCMe3, respectively. ClusterI crystallized in the triclinic space group
(2) witha=12.766(6) Å,b=22.904(5) Å,c=10.522(3) Å, =99.86(2)°, =109.68(2)°, =86.84(3)°,V=2854(2) Å3,Z=2,R=0.049 for 6622 observed reflections (I>5 (I)) and 410 variables. ClusterII crystallized in the triclinic space group
(2) with dimensionsa=14.212(4) Å,b=14.725(5) Å,c=12.396(8) Å, =110.32(4)°, =90.40(5)°, =62.88(2)°,V=2129(2) Å3,Z=1,R=0.039 for 6020 observed reflections (I>3 (I)) and 461 variables. ClusterI consists of a neutral cubane-like molecule with the core {MoCu3S3(S2COEt)}2+, in which one corner of the cubane-like core is a novel triply bridging bidentate 1,1-dithiolato (xanthate, S2COEt–) ligand. ClusterII is a double cubane-like one, in which two cubane-like cores {MoCu3S3(SCMe3)}2+ are connected by two Cu-S bonds of the triply bridging monothiolato (SCMe
3
–
) ligand. Two different pathways of unit construction from a small heterometallic cluster {MoCu2S3}(O)(Ph3P)3 have been outlined. Comparisons of the selected bond lengths and bond angles for the cubane-like core {MoCu3S3
X} (X=Cl–, Br–, S2COEt–, SCMe
3
–
) are given. Spectroscopic properties of the title clusters are also reported. |
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Keywords: | Cubane-like double cubane-like Molybdenum-copper-sulphur clusters |
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