The reaction of Na2MoO4 . 2H(2)O with Mo(CO)(6) in (CF3CO)(2)O produces Na-4[Mo2O2(O2CCF3)(10)]4CF(3)CO(2)H (1). 1 is dissolved in a EtOH solution of P2S5, a solution containing Et(4)NCl, and a (PrOH)-Pr-i solution of P2S5 to yield [Mo2O2S2(S2P(OEt)(2))(2)] (2), Et(4)N[Mo2O2S2(mu-O2CCF3)(S2P(OEt)(2))(2)] (3), and [Mo2O3(S2P((OPr)-Pr-i)(2))(4)] (4), respectively. 3 provides the first example of six-coordinate [Mo(2)O(2)S(2)L(2)] (L = bidentate sulfide ligands) complexes. The solution UV-vis spectrum of 3 differs greatly from that of 2, indicating that there is still a significant bonding interaction between the Mo atoms and CF3CO2 group in solution.