Abstract
The reaction between NbSCl 3 and triphenylphosphine sulphide leads to the formation of the 1:1 adduct, crystals which are triclinic, space group P 1 , with a = 12.524(5), b = 10.193(4), c = 17.823(6) Å, α = 103.80(3), β = 102.60(4), γ = 72.02(4)°, Z = 4. The structure was solved by Patterson and Fourier methods using diffractometer data and refined to R 0.058 for 2880 significant reflections. The unit cell contains two five-coordinate monomers and one centrosymmetric six co-ordinate dimer, the coexistence of which is a most unusual feature in the solid state. The niobium atom is displaced from the plane formed by the three chlorine atoms and the ligand sulphur atom towards the sulphido sulphur atom [0.553(2) Å, monomer, 0.397(2) Å, dimer]. This displacement is larger than any yet found in adducts of NbOCl 3.
Published Version
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