Reduction of terphenyl iron(II) or cobalt(II) halides in the presence oftrimethylphosphine: an unusual triple dehydrogenation of an alkyl group

Chengbao Ni; Bobby D. Ellis; Troy A. Stich; James C. Fettinger; Gary J. Long; R. David Britt; Philip P. Power

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Reduction of terphenyl iron(II) or cobalt(II) halides in the presence oftrimethylphosphine: an unusual triple dehydrogenation of an alkyl group

机译：在三甲基膦的存在下还原三苯基卤化铁（II）或卤化钴（II）：烷基的异常三重脱氢

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The reduction of {ArFeBr}_2 (Ar = terphenyl) with KC_8 in the presence of excess PMe_3 afforded theFe(I) complex 3.5-Pr~i_2-Ar′Fe(PMe_3) (1) (Ar′-3,5-Pr~i_2 = C_6H-2,6-(C_6H_3-2,6-Pr~i_2)-3,5-Pr~i_2), which has astructure very different from the previously reported, linear Cr(I) species 3,5-Pr~i_2-Ar~*Cr(PMe_3)(3.5-Pr~i_2-Ar~* = C_6H-2,6-(C_6H_2- 2,4.6-Pr~i_3)_2-3.5-Pr~i_2) and features a strong Fe-η~6-aryl interaction withthe flanking aryl ring of the terphenyl ligand. In sharp contrast, the reduction of {ArCoCl}_2(Ar =3,5-Pr~i_2-Ar′ and Ar′) afforded the allyl complexes Co(η~3-{1-(H_2C)_2C-C_6H_3-2-(C_6H_2-2,4-Pr~i_2-5-(C_6H_3 2,6-Pr~i_2))-3-Pr~i})(PMe_3)_3(4) and Co(η~3-{1-(H_2C)_2C-C_6H_3-2-(C_6H_4-3-(C_6H_3-2,6-Pr~i_2))-3-Pr~i})(PMe_3)_3 (5) formed by an unusual triple dehydrogenation of an isopropyl group. It is proposedthat the reduction initially generates an intermediate 3,5-Pr~i_2-Ar′Co(PMe_3), which is similar in structureto 1, followed by 3,5-Pr~i_2,-Ar′Co(PMe_3) decomposition to a cobalt hydride intermediate anddehydrogenation of the isopropyl group via remote C-H activation induced by PMe_3complexation.Complexes 1, 4, and 5 were characterized by X-ray crystallography. In addition, 1 was studied by NMRand EPR spectroscopy: 4 and 5 were characterized by NMR spectroscopy.

机译：在过量的PMe_3存在下，用KC_8还原{ArFeBr} _2（Ar =三联苯），得到Fe（I）络合物3.5-Pr〜i_2-Ar'Fe（PMe_3）（1）（Ar'-3,5-Pr 〜i_2 = C_6H-2,6-（C_6H_3-2,6-Pr〜i_2）-3,5-Pr〜i_2），其结构与先前报道的线性Cr（I）物种3,5-非常不同Pr〜i_2-Ar〜* Cr（PMe_3）（3.5-Pr〜i_2-Ar〜* = C_6H-2,6-（C_6H_2- 2,4.6-Pr〜i_3）_2-3.5-Pr〜i_2） Fe-η〜6-芳基与三联苯配体的侧基芳环之间有很强的相互作用。形成鲜明对比的是，{ArCoCl} _2（Ar = 3,5-Pr〜i_2-Ar'和Ar'）的还原得到烯丙基配合物Co（η〜3- {1-（H_2C）_2C-C_6H_3-2- （C_6H_2-2,4-Pr〜i_2-5-（C_6H_3 2,6-Pr〜i_2））-3-Pr〜i}）（PMe_3）_3（4）和Co（η〜3- {1-（ H_2C）_2C-C_6H_3-2-（C_6H_4-3-（C_6H_3-2,6-Pr〜i_2））-3-Pr〜i}）（PMe_3）_3（5）由异丙基的不寻常三重脱氢形成。建议还原首先生成一个中间3,5-Pr〜i_2-Ar'Co（PMe_3），其结构类似于1，然后分解3,5-Pr〜i_2，-Ar'Co（PMe_3）分解为通过X射线晶体学表征复合物1、4和5，通过PMe_3络合诱导的CH远程活化激活氢化钴中间体和异丙基的脱氢反应。此外，通过NMR和EPR光谱研究了1个：通过NMR光谱表征了4个和5个。

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来源
《Dalton transactions: An international journal of inorganic chemistry》 |2009年第27期|共5页
作者
Chengbao Ni; Bobby D. Ellis; Troy A. Stich; James C. Fettinger; Gary J. Long; R. David Britt; Philip P. Power;
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正文语种 eng
中图分类化学;
关键词
Reduction; presence; dehydrogenation;

机译：还原;存在;脱氢;

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1. Reduction of terphenyl iron(II) or cobalt(II) halides in the presence oftrimethylphosphine: an unusual triple dehydrogenation of an alkyl group [J] . Chengbao Ni, Bobby D. Ellis, Troy A. Stich, Dalton transactions: An international journal of inorganic chemistry . 2009,第27期

机译：在三甲基膦的存在下还原三苯基卤化铁（II）或卤化钴（II）：烷基的异常三重脱氢
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机译：Sr2FeO3F中的异常磁结构以及K2NiF4型铁（III）氧化物和氧化物卤化物的磁结构，包括钴取代的Sr2Fe1-xCoxO3Cl系列
3. Reduction of terphenyl Co(II) halide derivatives in the presence of arenes: Insertion of Co(I) into a C-F bond [J] . Lei H., Fettinger J.C., Power P.P. Inorganic Chemistry: A Research Journal that Includes Bioinorganic, Catalytic, Organometallic, Solid-State, and Synthetic Chemistry and Reaction Dynamics . 2012,第3期

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4. Reduction of alkyl halides by electrogenerated cobalt(I) salen and nickel(I) salen: reactions of alkyl radicals with no and O_2 [C] . Dennis G. Peters, Chang Ji, Benjamin J. Wozniak, International Manuel M. Baizer Symposium . 2002

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机译：用含烷基或烷基卤化物悬垂臂的吡啶基 - 四唑配体的铜（II），镍（II），镍（II），钴（II）和锌（II）盐的配位研究

Reduction of terphenyl iron(II) or cobalt(II) halides in the presence oftrimethylphosphine: an unusual triple dehydrogenation of an alkyl group

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