作者: Hans-F. Klein , Thomas Wiemer , Marie-J. Menu , Michélle Dartiguenave , Yves Dartiguenave
DOI: 10.1016/S0020-1693(00)85157-9
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摘要: Abstract Several new methyl-nickel(II) compounds NiMe- X(PMe 3 ) [X=8-hydroxyquinolate, 1; X=1/2[O 2 C(CH n CO ), 2: =0; 3: =1; 4 : =2; 5 =3; 6 =4] were prepared by reacting [NiMe(PMe )(OMe)] and the corresponding acid. Compound 1 crystallizes in space group P with a =8.868(1), b =9.303(2), c =8.452(1) A, α=94.29(1)°, β= 105.85(1)°, γ=82.63(1)°, V =671.8(1) A , Z = 2. Final discrepancy indices are R =0.0291 w =0.0303 for 2255 independent data ( I >3σ( )). The coordination geometry around nickel is square planar. NiP NiC distances of 2.125(1) 1.917(2) on shortest range usually observed values, while NiO NiN values 1.923(2) 1.953(2) upper one. oxygen atom oxinate ligand trans to methyl group. / =9.266(1), =11.113(2), =8.169(2) β=93.46(2)°, =839.5 =4. final =0.0325 0.0334 1221 molecule shows two atoms bridged oxalato acting as bidentate both metals (NiO1=1.990(3) NiO2=1.961(3) A). dimer possesses crystallographic center symmetry, which located middle CC bond. about each metal planar, sphere being completed trimethylphosphine ligands. Compounds have been characterized IR spectroscopy, together 4a 6a obtained reaction PMe excess.