In competition experiments with heptanal/diethyl ketone (1 : 1) it could be shown that 1, 3b and 4b olefinate aldehyde groups without the keto groups being attacked.Presumably the carbonyl olefinations proceed as formulated for lc7l. The postulated product 2a, however, has so far evaded detection. 933.[21 Procedure for synthesis of 1 : A suspension of Mo02(Me2NCS2)2 (3.25 mmol) and NHZNHC(S)SEt (16 mmol) in 60 mL methanol is stirred for 4 Angew. Chem. Int. Ed. Engl. 22 (1983) No. 3 0 Verlag Chemie GmbH. 6940 Weinheim, 1983 0570-0833/83/0303-0245 $02.50/0
X‐ray structure investigations of the complexes (III) and (VI), obtained by the title reaction, show that (III) (space group P21/c, Z=4) contains a "side‐on" bound hydrazido(1‐) ligand NH2NC(O)SMe, whereas in (VI) (space group P1, Z=1) the same ligand is N,O‐chelated.
Die Reaktion von NH2NHC(O)SMe mit MoO2(S2CNEt2)2 und MoO2(ONEt2)2 ergibt die Diazenido‐Hydrazido‐Komplexe [Mo(NNC(O)SMe)(NH2NC(O)SMe)(S2CNEt2)2] · CH2Cl2 (2) bzw. [(μ‐OMe)Mo(NNC(O)SMe)(NH2NC(O)SMe)(ONEt2)]2 (4). Röntgenstrukturanalysen von 2 und 4 ergaben, daß der Hydrazido(1 – )‐Ligand NH2NC(O)SMe in 2 symmetrisch “side on”, im dimeren 4 dagegen als N,O‐Chelat gebunden ist. Die Mo–N‐Abstände in 2 betragen 213.1(7) und 213.4(5) pm, der N – N‐Abstand 140.4(9) pm. Die Stickstoffatome sind sp3‐hybridisiert. Mögliche Faktoren für die “side‐on”‐, “end‐on”‐oder chelatartige Koordination von Hydrazido(1 – )‐Liganden werden diskutiert.
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