Preparation and structure of oxo-rhenium(V) complexes with 7-azaindole

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Abstract
Four Re(V) oxo compounds were obtained from 7-azaindole (Haza) and ReOCl3(PPh3)2: the oxo-bridged dimer Re2O3Cl4(Haza)4 (1), the oxo–ethoxo monomers ReO(OEt)Cl2(Haza)2 (2) and ReO(OEt)Cl2(Haza)(PPh3) (3), and the dioxo [ReO2(Haza)4]Cl salt (4a). [ReO2(Haza)4]I (4b) was also prepared from ReO2I(PPh3)2. The ReO(OEt)Cl2(Haza)2 complex was shown by X-ray diffraction (C2/c, a = 16.292, b = 9.395, c = 12.104 Å, β = 101.47°, R = 0.041) to consist of individual molecules of the trans-trans isomer in which azaindole is N7-bonded. Crystals of [Formula: see text] (C2/m a = 15.422, b = 13.055, c = 9.086 Å, β = 91.13°, R = 0.059) contain well separated Cl− anions and trans-dioxo cations. The N7-bonded azaindole ligands are held parallel to the O=Re=O direction by intramolecular [Formula: see text] hydrogen bonds, but the relative orientation of the four ligands cannot be determined because of disorder. Characteristic Re—oxygen vibrations are observed in infrared for each type of compounds. The 1H and 13C NMR spectra are discussed in relation with the azaindole binding mode.

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