MoFe3S4 singel cubane-like cluster compounds, [MoFe3S4(RCS2)5].DMF and [MoFe3S4(RCS2)5].CH2Cl2 (I) (R = piperidino) were obtained by 1-step spontaneous self-assembly reaction of FeCl2, (NH4)2MoS4 with RCS2Na in DMF or CH2Cl2, resp. I is orthorhombic, space group Pbca, with a 19.222(7), b 27.853(4), c 19.456(3) ? d.(calcd.) = 1.645 g cm3, Z = 8, R = 0.097. Its structural feature, as compared with [MoFe3S4(Et2NCS2)5], exhibits obvious differences resulting from the disparity of the core oxidation states. The effect of reactant ratio on the product and the substitution reaction of solvent mol. in these compounds were also discussed.

Key words: CRYSTAL STRUCTURE DETERMINATION, X-RAY DIFFRACTION ANALYSIS, SUBSTITUTION REACTION, IRON COMPLEX, NITROGENASE, MOLYBDENUM COMPLEX, CLUSTER COMPOUND, MOLECULAR ORBITAL THEORY, SULFIDE COMPLEX, SPONTANEOUS SELF-ASSEMBLE REACTION