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Preparation and characterization of NiCl(NO)(PPh3)2

Previous work [1] on the title compound reports an intractable disorder problem; the complex was prepared again following the method of Feltham [2], and purple crystals were prepared by vapour diffusion of hexane into a benzene solution. The compound crystallizes in a C-centered monoclinic space group, with a cell of dimensions: a = 17.399(3), b = 13.136(3), c = 16.954(3) Ǻ, β = 104.74(1), Z = 4 and T = 296 K. FTIR spectral absorptions attributed to aromatic ν(C−H) at 3050 cm, ν(N−O) at 1716 cm, aromatic ν(C−C) at 1434 cm, and bands for CH inand out-of-plane bending at 1095 cm and 693 cm, respectively. The supramolecular structure contains the expected [3] six-fold phenyl embrace, 6PE, chains linking nickel bis(phosphine) moieties into one-dimensional zigzag chains. However, the lattice also contains a benzene solvate. The benzene molecule is able to form considerably more C−H···π interactions than a phenyl ring and becomes the major link, interconnecting three of the 6PE chains via ten C−H···π interactions centered about the benzene of crystallization. Additional weak noncovalent interactions supplement these major interactions to form an extensive three-dimensional crystal structure.