SYNTHESIS AND CRYSTALLINE-STRUCTURE OF CL USTER )(7)(MU(3)-S)[MU,ETA(2)-SCNC(O)C(R-1)(R-2)N(COR3)]

Through the reaction of CO2(CO)(8) with four thiohydantoins, S=CNHC(O) C(R-1)(R-2)N<COR3), four new sulfur-capped trinuclear cobalt carbonyl clusters 3(CO)(7)(mu(3)-S)mu,eta(2)-SCNCOC(R-1)(R-2)N(COR3) [I:R-1=R-2 =H; n:R-1=H, R-2=CH3, R-3=Ph; m: R-1=R-2=H, R-3=CH3; nr : R-1=R-2=R-3= CH3], were prepared and characterized by elementary analysis, IR, H-1 NMR and MS spectroscopy. The crystal structure of the cluster )(7)(mu( 3)-S)[mu,eta(2)-SC=NC(O)C(CH3)(2)N(COCH3)] (N) was determined by X-ray single crystal diffraction method. The crystal of the cluster is tric linic belonging to space group P (1) over bar and the cell parameters are as follows: a = 0.845 6(3) nm, b=1.153 4(3) nm, c=1.199 0(4) nm; a =107.36(3)degrees, beta=108.44(5)degrees, gamma=90.18(3)degrees; V=1.0 52(6) nm(3), Z = 2, F (O 0 0) = 584, D-c = 1.86 g/cm(3), mu = 25.71 cm (-1), R = 0.046, R-w=0.058. The molecule has revealed to have a pyrimi dal Co3S framework and contain a heterocyclic bridging bidentate ligan d SCNC(O)C(R-1)(R-2)N(COR3) linked to the Co(1) and Co(2) atoms of the cluster by a cobalt-nitrogen and a cobalt-sulfur bond respectively.