Di- and trinuclear complexes of WS42- with tricarbonylrhenium(I) and -manganese(I) fragments. Structure, spectroscopy, and electrochemistry
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Zeitschrift fuer Anorganische und Allgemeine Chemie 624 (7): 1211--1220 (1998)

The reaction of (NEt4)2WS4 with 2 equiv. of M(CO)5(O3SCF3), M = Mn or Re, in MeCN yielded the crystallog. characterized neutral compds. (MeCN)(OC)3M(m-S2WS2)M(CO)3(NCMe) (I, M = Mn) and (II, M = Re). Crystal data: I triclinic, space group P1̅, a = 973.85(6), b = 1031.55(7), c = 1058.25(7) pm, a = 71.375(5), b = 76.550(6), g = 82.824(6)°, V = 0.97831(11) nm3, Z = 2, rc = 2.282 g/cm3, m(MoKa) = 7.589 mm-1, F(000) = 632, 5517 obsd. reflections, 227 refined parameters, R1 = 0.0316, wR2 = 0.0705 for I \textgreater 2s(I); II triclinic, space group P1̅, a = 995.0(1), b = 1037.8(1), c = 1076.4(1) pm, a = 71.39(1), b = 77.18(1), g = 83.53(1)°, V = 1.0261(2) nm3, Z = 2, rc = 3.025 g/cm3, m(MoKa) = 17.792 mm-1, F(000) = 832, 4043 obsd. reflections, 227 refined parameters, R1 = 0.0438, wR2 = 0.1106 for I \textgreater 2s(I). The individual mols. are chiral and contain WS4 and MS2(CO)3(MeCN) moieties in approx. tetrahedral and octahedral configurations, resp. Vibrational and electronic absorption spectra are in agreement with the crystal structure, comparable results were obtained for trinuclear complexes (L)(OC)3Re(m-S2WS2)Re(CO)3(L)(NEt4)2, L = Cl- or CN-, and for the dinuclear systems (WS4).Re(CO)3(MeCN)(NEt4) and (WS4)Re(CO)3Cl(NEt4)2. Electrochem. processes are irreversible due to the lability of MeCN or Cl ligands in corresponding complexes, however, the cyanide compd. (NC)(OC)3Re(m-S2WS2)Re(CO)3(CN)2- showed reversible 1-electron redn. to a 1st tetrathiotungstate(V) species as detected by UV/vis/IR spectroelectrochem. on SciFinder(R)
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