{Cu 4W 2S 6}(PPh 3) 4O 2, a compound with a metal sulfur cage generated by the WOS 2−3 ligand. Preparation, crystal and molecular structure

Abstract

{Cu 4W 2S 6}(PPh 3) 4O 2 has been prepared by the reaction of an aqueous solution of Cs 2WOS 3 with a mixture of CuCl 2·2H 2O in H 2O and P(C 6H 5) 3 in CH 2Cl 2. The structure was determined from single crystal X-ray diffractometer data and was refined by least-squares methods to R = 0.071 for 5869 independent data. The compound crystallizes in the triclinic space group P 1 with one molecule in the unit cell ( a = 12.432(4), b = 12.567(2), c = 13.123(4) Å, α = 93.02(2), β = 117.43(2), γ = 95.05(2)°, V = 1803.4 Å 3, d calcd = 1.75 g/cm 3). The structure can be described as a cage (with a centre of inversion), fused by two six-membered SCu 2S 2W rings. W(107.53(33)–113.52(12)°) and Cu (distorted, angles varying between 102.16(13) and 121.08(13)°) are tetrahedrally coordinated.