Abstract
Ditungsten(II) tetrabenzoate reacts with the lithium salt of 7-azaindole to form tetrakis(7-azaindolato)ditungsten in 75% yield. The compound crystallizes as the tetrahydrofuran solvate, W 2(C 7H 5N 2) 4·2THF and its structure has been determined by X-ray crystallography. It forms crystals in space group P2 1/ c, with the following unit cell dimensions: a=9.185(2), b=13.263(3), c=14.168(8) Å, β=104.46(3)°, V=1671(4) Å 3, Z=2. The molecules reside on crystallographic centers of inversion and the ligands are disordered, necessitating refinement by a method employing rigid-body treatment of oppositely oriented half-molecules of the ligand at each position. The W–W distance, 2.227(2) Å, is the longest one so far observed for a ligand of this type and it is argued that this is due to the geometry and rigidity of the bidentate bridging 7-azaindolate ligand. The greater W–W bond length, in turn, causes the δ→ δ * electronic transition to fall at a relatively low frequency, 16 000 cm −1, where it is very clearly resolved from strong absorption at higher energies.
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