Synthesis and X‐ray Structural Characterization of (Di<i>iso</i>propylamino)(Morpholino)(Phenyl)Phosphine and its Dimeric Copper(I)
作者:T. Arun Luiz、M. N. Sudheendra Rao、Babu Varghese
DOI:10.1080/15533170701672623
日期:2007.11.1
An electron rich "hybrid" asymmetric aminophosphine, (diisopropylamino)(morpholino) (phenyl)phosphine, L, was synthesized in good yield by step-wise aminolysis reactions with dichloro(phenyl)phosphine and structurally characterized. The complex, CuCl(L) was readily isolated from both 1:1 and 1:2 reactions of L with CuCl. Single crystal X-ray structures of L and two copper complexes, [CuCl(L) center dot CH3CN](2) (1) and [CuCl(L) center dot CH2Cl2](2) (2) have been determined. X-ray structures reveal pyramidal nature of phosphorus and near planar geometry of nitrogen of the phosphine ligand and the dimeric nature of the complexes with tricoordinate copper(I) centers. The asymmetric phosphine crystallizes in monoclinic system with space group P21/c and unit cell dimensions as a 17.219(1) angstrom, b = 13.469(1) angstrom, c = 7.395(5) angstrom, alpha = 90.00 degrees, beta = 93.11(1)degrees, gamma = 90.00 degrees. Both acetonitrile (1) and dichloromethane (2) solvates; crystallize in triclinic system with space group P (i) over bar. The unit cell dimensions of (1) are a = 10.143(2) angstrom, b = 13.681(3) angstrom, c = 16.647(3) angstrom, alpha = 83.14(1)degrees, beta = 76.91(1)degrees, gamma = 68.83(1)degrees and that of (2) are a = 8.899(1) angstrom, b = 11.727(1) angstrom, c = 11.784(1) angstrom. alpha = 66.73(1)degrees, beta = 82.27(1)degrees, gamma = 84.04(1)degrees. This is the first report of copper(I) phosphine complexes in which the coordinated asymmetric phosphine carries two different amino substituents.