New clusters MRuCo(CO)(8)(mu(3)-S)[eta(5)-C5H4C(O)CH3] (M=Mo 2, W 3) and [MRuCo(CO)(8)(mu(3)-S)](2)[eta(5)-C5H4C(O)C6H4C(O)C5H4-eta(5)][M=Mo 4, W 5] have been isolated from the reaction of RuCo2(mu(3)-S)(CO)(9) 1 with [eta(5)-C5H4C(O)CH3(CO)(3)M](-) (M=Mo, W) and (-)[M(CO)(3){eta(5)-C5H4C(O)C6H4C(O)C5H4-eta(5)}(CO)(3)M](-) [M=Mo, W], respectively. Clusters 2 and 5 have been established by single crystal X-ray diffraction methods. The crystals of cluster 2 are orthorhombic with space group Pbca, a = 26.229(7), b = 18.200(3), c = 15.929(4) Angstrom, V = 7604(6) Angstrom(3) and Z = 18; final R = 0.033, R-w = 0.045. The crystals of cluster 5 are triclinic space group P (1) over bar, a = 12.688(4), b = 20.290(7), c = 9.429(3) Angstrom, alpha = 99.78(3), beta = 90.64(2), gamma = 78.28(3)degrees, V = 2341(1) Angstrom(3) and Z = 4; final R = 0.042, R-w = 0.063. (C) 1998 Elsevier Science S.A. All rights reserved.