The title V-Cu-S heterometallic cluster compound C84 H86Cl4Cu6N2O4P4S6V2, crystallizes in the monoclinic space group P21/n with a=16.381(5), b=17.114(3),c=16.749(6) A,β=107. 04(3)°,V=4490(2)A3, Mr=2128.84,Z=2,Dc=1. 57 g/cm3,μ= 19. 6 cm-1,F(000)=2160. Final R=0.074(Rw=0.082) for 2662 unique reflections with I≥3σ(I). The V atom in the compound retains the tetrahedral geometry of the VS3O with S-V-S or S-V-O angles of 108.6(6)～110.3 (6)°.The cluster core [V2Cu6S6O2] of the compound can be regarded as two cluster cores [VCu3S3O] bonded by bondings of the Cu-Cu'(distances of 2.774(3)～2.707(5) A) and Cu-S (distances of 2.463(7)～2.396(9) A) with centrosymmetric. Atoms of the cluster core V2Cu6 form a distorted cube with the Cu Cu'or the V-Cu distances of 2. 774(3)～2. 707(5) A.
In this paper detailed studies of the cyclic voltammetry(CV) of trinuclear metal cluster compounds [M_3O_2(O_2CCH_3,)6(H,O),j z+ (M,=Mo3,MoW2,W3) are reported.The result of CV shows that they are similar to each other.There are a reversible redox peak near-0. 48 V and an irreversible reduced peak near-1.10 V in the scan range of + l.0 V to l. 5 V.It implies that the M_3O_2,clusters might gain one electron to be further reduced.But the two-electron-reduced product of M_3O_2 clusters are instable.The theoretical calculations(EHMO) agree well with the result of the CV experiment.
In this paper we report the structure of another new W3 cluster compound H[W3O2(O2CCH3)9]·5H2O prepared by the method reported previously. The title compound crystal lizes in monoctinic system, space group P21 with cell dimensions: a = 8. 237(3),6=13. 273(2),c=14.508(4)A,β=92.97°(3),V=1584A3.Z=2,and Dc=2. 529g/cm3.The average W - W, W -U_3-O,W -Oac and W -Ot distances are 2. 775, 2. 01,2. 09 and 2. 04 A, respectively.
