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Inne
Dithiolate-hydrazido(2-) molybdenum complexes: synthesis and structure.
Autorzy
Rok wydania
2003
Czasopismo
Numer woluminu
350
Strony
379-386
DOI
10.1016/S0020-1693(03)00051-3
Kolekcja
Język
Angielski
Typ publikacji
Artykuł
Reaction of [MoO2(acac)2] with an excess of X(CH2CH2SH)2 where X=O, S leads to the formation of mononuclear complexes [MoO2{X(CH2CH2S)2}]: (1a) for X=O and (1b) for X=S. The complexes 1a and 1b react with organohydrazines in methanol, MeCN or THF to give the family of hydrazido(2-)-oxo-molybdenum compounds [MoO(NNRR′){X(CH2CH2S)2}]: (2a) for R=R′=Me and X=O; (2b) for R=R′=Me and X=S; (2c) for R=Me, R′=Ph and X=O; (2d) for R=Me, R′=Ph and X=S. Similar reaction carried out in CH2Cl2 with an excess of NH2NMe2 leads to the formation of 2a and hydrazinium salt [NH2N(CH2Cl)Me2]Cl consisting of tetrahedral cations bonded by hydrogen bonds to chloride ions as shown by X-ray studies. The X-ray crystal structures of 2a and 2b have been determined. These molecules have a distorted trigonal bipyramidal configuration with the hydrazido(2-) ligand bonded linearly in a trans position to either the ether oxygen or the thioether sulfur atoms of the dithiolate ligand. Me3SiCl causes abstraction of the oxo group in 2a–2d to create the six-coordinate compounds [MoCl2(NNRR′){X(CH2CH2S)2}] (3a–3d), respectively. The chlorides in 3d can be easily substituted by oxygen and nitrogen donor ligands to give the new compounds [Mo(di-t-Bu-cat)(NNRR′){X(CH2CH2S)2}] (4) and [Mo(NNRR′)2{X(CH2CH2S)2}] (5), respectively. Dioxodithiolate molybdenum compounds [MoO2{X(CH2CH2S)2}] (1) where X=O, S react with organohydrazines to afford a family of mononuclear oxo–hydrazido(2-) complexes [MoO{X(CH2CH2S)2}(NNRR′)] (2). The oxo group in 2 can be easily substituted by chlorides to form six-coordinated compounds [MoCl2{X(CH2CH2S)2}(NNRR′)] (3), which with catecholates (cat) and organohydrazines generate [Mo(cat){X(CH2CH2S)2}(NNRR′)] (4) and bishydrazido(2-) [Mo(NNRR′)2{X(CH2CH2S)2}] (5) products, respectively.
Adres publiczny
https://doi.org/10.1016/S0020-1693(03)00051-3
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