461643-76-5Relevant articles and documents
Crystal structures of the phosphoraneiminato complex [INi(NPMe3)]4·C4H8 O·C7H8 and of the phosphanimine complex [INi{Me2Si(NPMe3)2}(HNPMe3)] +I-
Mller, Ulrich,Bock, Oliver,Sippel, Heike,Grb, Thorsten,Dehnicke, Kurt,Greiner, Andreas
, p. 1703 - 1707 (2008/10/08)
The phosphoraneiminato complex [INi(NPMe3)]4 was obtained by reaction of NiI2 in molten Me3SiNPMe3 in the presence of potassium fluoride at 200°C. Dark-green single crystals of [INi(NPMe3)]4·C4H8 O·C7H8 were formed from THF-toluene solution. According to the X-ray crystal structure determination the complex has a Ni4N4 heterocubane core and its symmetry deviates only marginally from Td (space group Pca21, Z = 4, a = 3160.7(6), b = 1001.5(1), c = 1422.6(8) pm). The [INi(NPMe3)]4 molecules are stacked to columns parallel to b, with a nearly tetragonal pattern in projection on (010). The solvent molecules reside in channels between the columns. A side product of the synthesis were blue single crystals of the phosphanimine complex [INi{Me2Si(NPMe3)2}(HNPMe3)] +I-. The crystal structure determination (space group Pca21, Z = 4, a = 1213.3(4), b = 1582.7(6), c = 1339.7(4) pm) revealed a distorted tetrahedral coordination of the Ni atom in the cation; the coordinated atoms are the two N atoms of the chelating bis(phosphane)imine molecule, the N atom of the phosphaneimine molecule HNPMe3 and one iodo ligand.