Synthesis and crystal structure of the first base-free diarylgermylene-transition metal mononuclear complexes
作者:Norihiro Tokitoh、Kyoko Manmaru、Renji Okazaki
DOI:10.1021/om00013a027
日期:1994.1
The first base-free diarylgermylene-transition metal mononuclear complexes Tb(Tip)Ge = M-(CO)5 (1, M = W; 2, M = Cr; Tb = 2,4,6-tris[bis(trimethylsilyl)methyl]phenyl, Tip = 2,4,6-triisopropylphenyl) were synthesized by the reaction of a new type of kinetically stabilized diarylgermylene Tb(Tip)Ge: (3), obtained by the treatment of germanium(II) iodide with bulky aryllithiums (TbLi and TipLi), with the corresponding pentacarbonylmetal(0)-tetrahydrofuran complexes of group 6 metals (W and Cr). Of the two diarylgermylene-group 6 metal complexes (1 and 2), the molecular structure of 1 was determined by X-ray crystallographic analysis. Crystal data with Mo Kalpha radiation (lambda = 0.710 69 angstrom): 1, C47H82GeO5Si6W, triclinic, space group P1BAR, a = 12.490(2) angstrom, b = 23.890(3) angstrom, c = 10.254(l) angstrom, a = 96.21(l)-degrees, beta = 105.52(1)-degrees, gamma = 89.82(1)-degrees, V = 2930(1) angstrom3, z = 2, R = 0.045, R(w) = 0.045 based on 8032 reflections with I > 3sigma(I) together with 541 variable parameters.