SYNTHESIS AND CRYSTAL-STRUCTURE OF [MO3S7(S2CNET2)3]2(TCNQ)2 - SALT OF A RADICAL-ANION AND A CLUSTER CATION

[Mo3S7(dtc)3]dtc (dtc = S2CNEt2) reacts with one or more equivalents of TCNQ (7,7,8,8-tetracyanoquinodimethane) in CH3CN to form radical-anion salts [Mo3S7(dtc)3]2(TCNQ)2 (1) and [Mo3S7(dtc)3](TCNQ)2 (2), respectively. By an analogous method from [Mo3Se7(dtc)3]dtc the seleno complex [Mo3Se7(dtc)3](TCNQ)2 (3) was obtained. The structure of 1 was established by X-ray structural analysis. The crystals are orthorhombic, space group Pbca, a = 24.388(4), b = 14.043(2), c = 25.224(6) angstrom. The structure has been solved to R(F) 0.049. The geometry of the [Mo3S7(dtc)3]+ cation is normal; the most interesting feature of the structure is the presence of rather short contacts between N atoms of TCNQ and S atoms of S2 ligands of the cation (the S...N distances are 2.91-2.95 angstrom). The TCNQ anions form centrosymmetrical dimers (the separation between the corresponding planes is 3.16 angstrom), so the formula of I can be written as [Mo3S7(dtc)3]2(TCNQ)2.