THE SYNTHESIS AND CRYSTAL-STRUCTURES OF 2 TETRANUCLEAR CLUSTER COMPOUNDS CONTAINING [MO3M'S4]5+ (M'=MO,W)

Taking Mo3S4(dtP)4 . H2O and M'(CO)6(M' = MO, W) as starting materials , one homo- and one hetero-tetranuclear cluster compounds [Mo4S4(mu-C2 H5CO2)2(dtpH)(dtp)3] 4, [Mo3WS4(mu-CH3CO2)2(dtPH)(dtp)3] 5 [dtp = (Eto )2PS2-; dtpH = (EtO)2P(S)] are obtained by using [3+1] reaction mode u nder the carboxylic medium. Both compounds contain a [M4S4]5+ cubane-t ype cluster core possessing 11 cluster electrons. This kind of core re sult from the reduction of M' (CO)6 whereas the (dtpH) ligands are for med by dtp groups under the presence of carboxylic acid.The crystal da ta are as follows 4 Mo4S4(C2H5CO2)2[(OC2H5)2PS2]3[(OC2H5)2P(S)SH] M(r) = 1400.01, Orthorhombic Pbca, a = 2.4230(8), b = 2.2403(5), c = 1.913 1(8)nm, V = 10.385(6)nm3, Z = 8, D(c) = 1.79g / cm3. F(000) = 5584, mu (MoKalpha) = 15.51 cm-1, The values of R and R(w) are 6.8% and 7.7% re spectively for 2443 observed reflections. 5 Mo3WS4(CH3CCO)2[(OC2H5)2PS 2]3[(OC2H5)2P(S)SH] M(r) = 1459.87, Orthorhombic Pbca, a = 2.4465(7), b = 2.1773(6), c = 1.8880(8)nm, V = 10.057(8)nM3, Z = 8, D(c) = 1.93g / cm3, F(000) = 5720, mu(MoKalpha) = 36.92cm-1. The values of R and R( w) are 5.9% and 6.8% respectively for 2758 observed reflections.