Synthesis and crystal structure of alpha-Mo4XS3(mu-dtp)(3)(dtp)(3)(X=0.6S+0.40)

The title compound (Mo4XS15P6O12C24H30), alpha-Mo4XS3(mu-dtP)(3)(dtP)(3) (X = 0. 6S + 0. 4O; dtp = -S2P[OEt](2)), isolated as a prismatic black crysta l, was prepared from ethanolic solution of Mo(CO)(6), MoCl5 and P2S5. It cr ystallizes in triclinic system, space group P (1) over bar with a = 14. 031 (4), b = 13. 372 (2), c = 16. 270 (8) Angstrom, alpha = 92. 15(2), beta = 72. 91 (3), gamma = 95. 20 (2)degrees, V = 2905. 4 (2) Angstrom(3), Z = 2, D-c = 1. 82 g/cm(3), M-r = 1598. 93, F(000) = 1564. 8, lambda = 0. 71069 An gstrom (MoK alpha), mu = 1. 584 mm(-1). The final R = 0. 058, R-w = 0. 057 for 5016 observed reflections with I greater than or equal to 3. 0 sigma(I) . The structure analysis reveals that the title compound has a [Mo4XS3] cor e, belonging to the cubane-type tetranuclear molybdenum clusters family, wi th one of its four mu(3)-caps being statistically occupied by S and O. Thre e dtp ligands chelated three mu-X capped Mo atoms as terminal ligands, whil e another three dtp bridged these three Mo atoms and the fourth one, formin g an alpha-type cluster compound.