Structural studies on catalysts and catalyst precursors. The X-ray structure determination of (3-Allylpentane-2,4 dithionato)chloro(triethylphosphine)nickel(II), Ni(asacsac)(Pet₃)Cl

Abstract

The preparation and characterization of Ni(asacsac)(PEt₃)Cl by single-crystal X-ray diffraction [refined to R = 0,049, R' = 0,052 with 1888 data having I ≥ 3σ(I)], are reported. The compound crystallizes as discrete molecules in the monoclinic space group P2₁/c, with a = 10,078(2), b = 8.202(3), c = 22.984(5) Å, β = 97.57(2)º, U = 1883.3 ų and Z = 4. The nickel-donor atom bond distances are Ni-S (trans Cl) 2.083(2), Ni-S (trans P) 2.127(2), Ni-Cl 2.208(2) and Ni-P 2,234(2) Å, with the ligands at angles S-Ni-S 96.8(1), S-Ni-C1 86.2(1), S-Ni-P 90.7(1) and Cl-Ni-P 86.9(1)º. The coordination about the nickel(11) centre is approximately planar, but the planes NiSS and NiPCl are inclined at 8.3º. Comparisons are made with the structures of related compounds, in particular, that of Ni(sacsac)PEt₃Cl.