Methylnickel compounds with chelating anionic ligands. Crystal and molecular structures of methyl(trimethylphosphine)nickel oxinate and oxalate dimer

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. NiP NiC distances of 2.125(1) 1.917(2) on shortest range usually observed values, while NiO NiN 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 (NiO1=1.990(3) NiO2=1.961(3) A). dimer possesses crystallographic center symmetry, which located middle CC bond. about each metal planar, sphere being completed trimethylphosphine ligands. Compounds  have been characterized IR spectroscopy, together 4a 6a obtained reaction PMe excess.

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