X-ray crystal structure of (tetraphenyldithiomidodiphosphinato) (triphenylphosphine)copper(I), (Ph 3P)Cu(SPPh 2) 2N, a monocyclic inorganic (carbon-free) chelate ring compound

Abstract

The mononuclear (Ph 3P)Cu(SPPh 2) 2N compound was prepared by reacting (Ph 3P) 2CuNO 3 with K[(SPPh 2) 2N] in MeOH/CHCl 3 solvent mixture. The 31P NMR spectrum has confirmed the loss of a triphenylphosphine molecule and the formation of the title compound. The crystal and molecular structure was determined by X-ray diffractometry. The compound is monoclinic, space group P2 1/c, a = 18.826(2), b = 10.619(2), c = 20.587(2) A ̊ , β = 112.46(2)°, V = 3803.6(8) A ̊ 3, Z = 4 . The lattice contains monomeric (Ph 3P)Cu(SPPh 2) 2N units, with three-coordinated copper(I) atoms in a distorted trigonal geometry [S(1)CuS(2) 121.5(1), S(1)CuP(3) 126.1(1) and S(2)CuP(3) 112.2(1)°]. The dithioligand is monometallic biconnective and within the resulted CuS 2P 2N inorganic ring the CuS [2.215(2), 2.258(2) Å], SP [2.017(2), 2.012(3) Å] and PN [1.582(5), 1.592(5) Å] bond lengths suggest a π-electron delocalization over the PNP fragment. The conformation of the six-membered ring is non-planar.