Zusammenfassung
The reaction of K3AsS3 with [(CpCo)-Co-#(CO)I-2] (Cp-# =Cp* (C3Me5) or Cp-x (C5Me4Et)) in DMF at 120 degreesC gave violet [Cp-2(#) Co2As2S3] 1(#), dark brown [Cp-3(#) Co3AsS6]I 2 (#), and dark brown [Cp-3(#) Co3AsS5]I 3(#). Whereas compounds 1(#) are already known, 2(#) and 3 (#) were characterized by IR, H-1-NMR and mass spectra. A crystal structure determination of 3(Cp)(x) reveals a salt-like ...
Zusammenfassung
The reaction of K3AsS3 with [(CpCo)-Co-#(CO)I-2] (Cp-# =Cp* (C3Me5) or Cp-x (C5Me4Et)) in DMF at 120 degreesC gave violet [Cp-2(#) Co2As2S3] 1(#), dark brown [Cp-3(#) Co3AsS6]I 2 (#), and dark brown [Cp-3(#) Co3AsS5]I 3(#). Whereas compounds 1(#) are already known, 2(#) and 3 (#) were characterized by IR, H-1-NMR and mass spectra. A crystal structure determination of 3(Cp)(x) reveals a salt-like character with [(CP3Co3AsS5)-Co-x](+) cations and iodide in a 1:1 ratio. In the cation the three Co atoms are connected by a mu (3)-S and a mu (3)-AsS4 ligand, thus forming a distorted Co3AsS4-cube. An additional sulfur atom is inserted into one of the As-S edges. The reaction of [Cp-2(#) Co2I4] with K2As4Se6 in DMF at 120 degreesC gave the brown salts [Cp-3(#) Co3AsSe5]I 5(#)". For characterization, compound 5(Cp-x) was reacted with [Cr(CO)(5)THF]. An X-ray diffraction analysis of the resulting [(Cp3Co3AsSe5)-Co-x][Cr(CO)(5)I] 8(Cp-x) reveals a molecular structure similar to that of 3(Cp)(x), but with a [Cr(CO)(5)I]- anion. In the cation all sulfur atoms are replaced by Se atoms. (C) 2001 Elsevier Science B.V. All rights reserved.
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