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The reaction of alkyldithiocarbazates NH 2 NHC(S)SR′ with MoO 2 (S 2 CNR 2 ) 2  R, R′ = Me, Et) yields the diazenido hydrazido complexes Mo(NNC(S)SR′)(NH 2 NC(S)SR′)(S 2 CNR 2 ) 2  (1), reaction with the molybdenum hydroxylamidate complex MoO 2 (ONMe 2 ) 2  gives the diazenidobis( hydrazido) complex Mo(NNC(S)SMe)(NH 2 NC(S)SMe) 2 (Me 2 NO)-CH 3 OH The crystal structures of  1 a  (R = Me, R′ = Et) and  2  have been determined. The metal atoms in  1 a  and  2  are seven coordinated and have MoN 2 S 5  and MoN 3 O 2 S 2  ligand arrays, respectively. Both compounds contain the approximately linear diazenido ligand NNC(S)SR in addition to one  (1a)  or two  (2)  N,S-chelating hydrazido(1-) ligands NH 2 NC(S)SR. When  1a  is treated with HCl, the dimeric complex (Me 2 NCS 2 )(O)Mo(μ-NNC(S)SEt) 2  Mo(S 2 CNMe 2 )  (4)  is obtained. X-ray crystallography showed  4  to be an asymmetric dinuclear complex, with a Mo-Mo distance of 267.2(1) pm. One Mo site has a square pyramidal MoOS 2 N 2  geometry, while the other one has an approximately trigonal prismatic MoN 2 S 4  geometry. The mean N-N distance in  4  is 135(1) pm. The reaction of NH 2 NHC(S)SMe with MoO 2 (acac) 2  yields Mo(Me 2 CNNC(S)SMe)(NNC(S)SMe)(MeSC(S)NNC(S)SMe) (3). Its structure has been determined by X-ray crystallography. 3 contains a unique combination of three different N- and S-chelating ligands: the Schiff base Me 2 C=NNC(S)SMe, the highly bent bidentate diazenido ligand NNC(S)SMe (∡ Mo-N-N = 142.1(5)°), and the novel planar tridentate ligand MeSC(S)NNC(S)SMe. The latter can be taken as neutral diacyldiazene or, more likely, as the dianion of the as yet unknown MeSC(S)NH -NHC(S)SMe. The N - N distance in this ligand is 136.1(9) pm.

zeitschrift für naturforschung b

Reaktion von Oxomolybdän-Komplexen mit Alkyldithiocarbazaten. Darstellung und Charakterisierung von Hydrazido- und Diazenido-Komplexen des Molybdäns /  Reaction of Oxomolybdenum Complexes with Alkyldithiocarbazates. Synthesis and Characterization of Hydrazido- and Diazenido Complexes of Molybdenum