Application of the hydro(solvo)thermal technique to the synthesis of metal carbonyl chalcogenide clusters Part 3. Synthesis, structural characterization, and spectroscopic studies of the clusters [{M(CO)4}n(MS4)]2- (M Mo, W; n=1, 2)

Song Ping Huang, Mercouri G. Kanatzidis

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The methanothermal reactions of M(CO)6 (M Mo, W) with Na2S2 gave a series of homonuclear clusters [{M(CO)4}n(MS4)]2- (M=Mo, W; n=1, 2), i.e. (Ph4P)2[(CO)4Mo(MoS4)] (I), (Ph4P)2[(CO)4W(WS4)] (II), (Ph4P)2[(CO)4Mo(MoS4)Mo(CO)4] (III) and (Ph4P)2[(CO)4W(WS4)W(CO)4] (IV). The two dimers, I and II, as well as the two trimers, III and IV, are isostructural to each other, respectively. All compounds crystallize in the triclinic space group P1 with Z=2. The cell dimensions are: a=12.393(8), b=19.303(9), c=11.909(6) Å, α=102.39(5), β=111.54(5), γ=73.61(5)°, V=2522(3) Å3 at T=23 °C for I; a=12.390(3), b=19.314(4), c=11.866(2) Å, α=102.66(2), β=111.49(1), γ=73.40(2)°, V=2511(1) Å3 at T=23 °C for II; a=11.416(3), b=22.524(4), c=10.815(4) Å, α=91.03(2), β=100.57(3), γ=88.96(2)°, V=2733(1) Å3 at T=-100 °C for III, a=11.498(1), b=22.600(4), c=10.864(3) Å, α=90.92(2), β=100.85(1), γ=88.58(1)°, V=2771(2) Å3 at T=23 °C for IV. The dimers are each formed by the coordination of the tetrathiometalate as a bidentate chelating ligand to an M(CO)4 fragment while addition of another M(CO)4 fragment to the dimers results in the trimers. All compounds contain both tetrahedral and octahedral metal centers with the formal 6+ and 0 oxidation states, respectively.

Original languageEnglish
Pages (from-to)9-17
Number of pages9
JournalInorganica Chimica Acta
Issue number1-2
Publication statusPublished - Mar 1 1995


ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Inorganic Chemistry
  • Materials Chemistry

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