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Synthese und charakterisierung von Cp2∗M(DAD)-komplexen (M = Y oder La) : Molekülstruktur von Cp2∗Y[N(C6H4-4-Me) = C(Ph)C(Ph) = N(C6H4-4-Me)]

1995; Elsevier BV; Volume: 501; Issue: 1-2 Linguagem: Inglês

10.1016/0022-328x(95)05646-7

1872-8561

A. Scholz, Karl‐Heinz Thiele, Joachim Scholz, Roman Weimann,

Synthesis and characterization of novel inorganic/organometallic compounds

The treatment of (η5-C5Me5)2La(μ-Cl)2K(dme)2 (3) with an equimolar amount of Na2(DAD) [DAD = (Ph)N=C(Ph)C(Ph)=N(Ph)] in the presence of DAD or with two equivalents of Na(DAD) results in the formation of the ionic complex [Na(DAD)][(η5-C5Me5)2La(DAD)] (4), which has been characterized by IR and NMR spectroscopy. Complex 4 exhibits dynamic NMR spectra indicating rapid migration of the (η5-C5Me5)2La unit from one side of the reduced DAD ligand to the other. (η5-C5Me5)2Y(μ-Cl)2Li(OEt2)2 (5) reacts with Na(DAD) [DAD= (Me-4-C6H4)-N=C(Ph)C(Ph)=N(Me-4-C6H4)] to yield dark-red crystals of the complex (η5-C5Me5)2Y(DAD) (6). Complex 6 is monoclinic, of space group C2/c (No. 15), with Z = 4, with a = 1345.2(3), b = 1702.9(2) and c = 1811.3(2) pm and with β = 106.73(1)°. The structure was refined to R = 0.040 for 2399 observed reflections (F0 > 4σ(F0)). The DAD ligand in 6 is reduced to the radical anion and forms a planar five-membered Y(N-C-C-N) ring.