Application of the Hydro (solvento) thermal Technique to the Synthesis of Metal Carbonyl Chalcogenide Clusters. 2. Synthesis and X-ray Structures of [{Fe4Te4(CO)10}2(Te2)]2− and [{Fe2Se(CO)6}2(Se2)]2−

Song Ping Huang, Mercouri G. Kanatzidis

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The hydrothermal reaction of Fe(CO)5 with Na2Te2 in the presence of Ph4PCl at 110 °C forms (Ph4P)2[{Fe4Te4-(CO)10}2(Te2)] (I) while the reaction of Fe(CO)5 with Na2Se2 in superheated methanol at 80 °C results in (Ph4P)2[{Fe2-Se(CO)6}2(Se2)] (II) The structures of (I) and (II) were determined by X-ray single-crystal analysis. (I) crystallizes in the space group P1̄, and (II) in the space group P21/n. The cell parameters are a = 14.930(4) Å, b = 24.070(3) Å, c = 13.045(2) Å, α = 93.19(1)°, β = 113.36(1)°, γ = 76.61(2)°, V = 4183(3) Å3, and Z = 2 at 23 °C for (I) and a = 10.561(6) Å, b = 14.021(5) Å, c = 20.46(1) Å, β = 91.89(4)°, V = 3028(2) Å3, and Z = 4 at −100 °C for (II). The [{Fe4Te4(CO)10}2(Te2)]2- anion in (I) forms a ditelluride, Te22−, bridged double cubane-like structure with eight iron atoms in two Fe4Te4 cubes being octahedrally-coordinated by bridging tellurium ligands and terminal CO groups. The [{Fe2Se(CO)6}2(Se2)]2- molecule in (II) adopts a double “butterfly” conformation caused by an intramolecular Se-Se linkage between two Fe2Se2(CO)6 units. All iron atoms in this structure have a distorted octahedral geometry achieved by selenium ligands, CO groups, and a Fe-Fe single bond. The average Fe-Te bond distance is 2.619(4) Å, and Fe-Se = 2.386(17) Å.

Original languageEnglish
Pages (from-to)821-825
Number of pages5
JournalInorganic Chemistry
Issue number6
Publication statusPublished - Jan 1 1993


ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Inorganic Chemistry

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