Synthesis, properties, and X-ray structural characterization of [tris(2-diphenylphosphinoethyl)phosphine]nickel(I) perchlorate and triphenylphosphine[tris(2-diphenylarsinoethyl)amine]nickel(I) perchlorate
Abstract
The cationic nickel(I) complexes [Ni{P(CH2CH2PPh2)3}]ClO4(1) and [Ni{N(CH2CH2AsPh2)3}(PPh3)]ClO4(2) have been synthesized by reaction of the nickel(0) derivative [Ni(C2H4)(PPh3)2] with [C3Ph3]ClO4 and the appropriate tripod-like ligand. The crystal structures of these two complexes have been determined from counter X-ray diffraction data. Crystal data : (1), space group Cc, a= 16.599(9), b= 12.810(7), c= 18.650(9)Å, β= 90.3(1)°, and Z= 4; (2), space group P21/a, a= 24.051(10), b= 13.267(7), c= 17.048(9)Å, β= 92.7(1)°, and Z= 4. Both structures were solved by the heavy-atom method and refined by full-matrix least-squares techniques to R of 0.060. Compound (1) exhibits the uncommon trigonal-pyramidal geometry, the nickel atom being surrounded by the four phosphorus atoms of the ligand. In compound (2) the nickel atom is five-co-ordinated by the four donor atoms of the arsine ligand and by the phosphorus atom of the triphenylphosphine in a distorted trigonal-bipyramidal geometry.