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首页> 外文期刊>Chemistry: A European journal >Facile metalation of silicon and germanium analogues of thiocarboxylic acids with a manganese(II) hydride precursor
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Facile metalation of silicon and germanium analogues of thiocarboxylic acids with a manganese(II) hydride precursor

机译：用氢化锰（II）前体轻松硫代羧酸的硅和锗类似物的金属化

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摘要

Synthesis and characterization of the first manganese(II)-containing heavier thiocarboxylate analogues, [L~(Dip)Si(=S)OMnL~(Dep)] (4; L~(Dip)=CH[C(Me)N(2,6-iPr_2C_6H_3)] _2, L~(Dep)=CH[C(Me)N(2,6-Et_2C_6H _3)]_2) and [L~(Dip)Ge(=S)OMnL~(Dep)] (5) are described. They are accessible through reaction of the silicon and germanium analogues of the respective thiocarboxylic acids [L~(Dip)E(=S)OH] (E=Si, Ge) with the β-diketiminato (nacnac) manganese(II) hydride precursor [(L~(Dep)Mn)_2(μ-H)_2] (3) in high yield. The first Mn nacnac hydride 3 has been prepared by the reaction of manganese bromide [(L~(Dep)Mn)_2(μ-Br)_2] (2) with KBEt _3H. Compounds 4 and 5 represent the first transition-metal heavier thiocarboxylates with the Si=S and Ge=S functionalities. All new compounds are paramagnetic and were characterized by elemental analysis, IR spectroscopy, MS (EI), and single-crystal X-ray diffraction analyses. Due to the N→E (E=Si, Ge) and E=S→Mn donor-acceptor interaction as well as the carboxylate-like π-electron delocalization within the E(S)O moieties, the E=S double bonds in these compounds are resonance stabilized. Active guys: The first transition-metal sila- and germathiocarboxylates were obtained by facile metalation of the corresponding heavier thiocarboxylic acids with currently unknown β-diketiminato manganese hydride. Preliminary investigations revealed that these complexes are capable of activating dioxygen and oxygenating triphenylphosphane at ambient temperature (see scheme).
机译：第一个含锰（II）的较重硫代羧酸酯类似物[L〜（Dip）Si（= S）OMnL〜（Dep）]（4; L〜（Dip）= CH [C（Me）N（ 2,6-iPr_2C_6H_3）] _2，L〜（Dep）= CH [C（Me）N（2,6-Et_2C_6H _3）] _ 2）和[L〜（Dip）Ge（= S）OMnL〜（Dep）对（5）进行说明。它们可以通过相应硫代羧酸[L〜（Dip）E（= S）OH]（E = Si，Ge）的硅和锗类似物与β-二酮亚胺基（nacnac）锰（II）氢化物前体的反应来获得[（L〜（Dep）Mn）_2（μ-H）_2]（3）高产。通过溴化锰[（L〜（Dep）Mn）_2（μ-Br）_2]（2）与KBEt _3H的反应制备了第一锰氢化萘3。化合物4和5代表具有Si ＝ S和Ge ＝ S官能度的第一过渡金属重硫代羧酸盐。所有新化合物都是顺磁性的，并通过元素分析，红外光谱，MS（EI）和单晶X射线衍射分析进行了表征。由于N→E（E = Si，Ge）和E = S→Mn供体-受体相互作用以及E（S）O部分内的类似羧酸盐的π电子离域作用，E = S双键在这些化合物是共振稳定的。活跃的家伙：第一种过渡金属硅烷和a硫代羧酸盐是通过将相应的较重的硫代羧酸与目前未知的β-二酮亚胺基化锰氢化物轻松地金属化而获得的。初步研究表明，这些络合物能够在环境温度下活化双氧并氧化三苯膦（参见方案）。

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