The novel tri-nuclear metal-sulfur cluster [Mo 3 S(S 2 ) 6 ] 2- can be obtained as its ammonium salt by the reaction of a Mo iv containing aqueous solutions with polysulfide. Its crystal and molecular structure has been determined by a single crystal X-ray study. The crystals are monoclinic (space group Cm, with a = 11.577(6) Å, b = 16.448(7) Å, c = 5.716(2) Å, β = 117.30(3)°, V = 967.2 Å 3 , Z = 2, d exptl. = 2.54(2) g/cm 3 , d cal = 2.54 g/cm 3 ). The structure consists of isolated [Mo 3 S(S 2 ) 6 ] 2- units, with three Mo atoms at the vertices of a triangle. There are bridging as well as terminal S 2 2- -ligands lying above and below the Mo 3 -plane (bond distances: Mo-Mo = 2.722 Å, Mo-S(terminal) = 2.435, Mo-S(bridging) = 2.452, Mo 3 -S = 2.353(4) Å and S-S = 2.04 Å (mean values)).
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Müller et al. (1979) studied this question.