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Preparation and Properties of, and Reactions with, Metal-Containing Heterocycles, XXVI. Nickelaphosphacycloakanes with Different Ring Sizes - Crystal Structure of 5-C5H5)NiP(C6H5)2CH2>2
Lindner, Ekkehard,Bouachir, Faouzi,Hiller, Wolfgang
, p. 1146 - 1154 (2007/10/02)
Substitution of CO in LNi(I)CO (1) (L = h5-C5H5) by the ω-chloro-1-(diphenylphosphino)alkanes Cl-n-PR2 (2a-d) a), 2 (b), 3 (c), 4 (d)> leads to the formation of the intermediates for cyclisation LNi(I)PR2-n-Cl (3a-d).When 3a is treated with sodium amalgam, the dimeric phosphino methanide complex 2 (4'a) is formed.On the basis of an X-ray crystallographic investigation 4'a has a boat conformation and crystallizes monoclinicly in the space group P21/c with Z = 2.The monomeric species (4a) could not be observed.Five- and six-membered nickelacycloalkanes of the type (4c, d) are obtained by reductive cycloelimination of 3c, d.Because of ring strain the nickelaphosphacyclobutane 4b is not accessible under the necessary cyclisation conditions.Into the Ni-C ? bond of 4c, d SO2 can be inserted to give the cyclic sulfinato complexes (5c, d). - Key words: Phosphino Methanide Complex, Structure of 5-C5H5)NiP(C6H5)2CH2>2, Nickelaphosphacycloalkanes, NMR Spectra
