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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >Synthesis and characterisation of halide, separated ion pair, and hydride cyclopentadienyl iron bis(diphenylphosphino)ethane derivatives
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Synthesis and characterisation of halide, separated ion pair, and hydride cyclopentadienyl iron bis(diphenylphosphino)ethane derivatives

机译：卤化物，分离的离子对和氢化物环戊二烯基铁双（二苯基膦基）乙烷衍生物的合成与表征

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Treatment of anhydrous FeX2 (X = Cl, Br, I) with one equivalent of bis(diphenylphosphino)ethane (dppe) in refluxing THF afforded analytically pure white (X = Cl), light green (X = Br), and yellow (X = I) [FeX2(dppe)](n) (X = Cl, I; Br, II; I, III). Complexes I-III are excellent synthons from which to prepare a range of cyclopentadienyl derivatives. Specifically, treatment of I-III with alkali metal salts of C5H5 (Cp, series 1), C5Me5 (Cp*, series 2), C5H4SiMe3 (Cp', series 3), C5H3(SiMe3)(2) (Cp '', series 4), and C5H3(Bu-t)(2) (Cp-tt, series 5) afforded [Fe(Cp-dagger)(Cl)(dppe)] 1Cl-5Cl, [Fe(Cp-dagger)(Br)(dppe)] 1Br-5Br, and [Fe(Cp-dagger)(I)(dppe)] 1I-5I (Cp-dagger = Cp, Cp*, Cp', Cp '', or Cptt). Dissolution of 1I-5I in acetonitrile, or treatment of 1Cl-5Cl with Me3SiI in acetonitrile (no halide exchange reactions were observed in other solvents) afforded the separated ion pair complexes [Fe(Cp-dagger)(NCMe)(dppe)][I] 1SIP-5SIP. Attempts to reduce 1Cl-5Cl, 1Br-5Br, and 1I-5I with a variety of reductants (Li-Cs, KC8, Na/Hg) were unsuccessful. Treatment of 1Cl-5Cl with LiAlH4 gave the hydride derivatives [Fe(Cp-dagger)(H)(dppe)] 1H-5H. This report provides a systematic account of reliable methods of preparing these complexes which may find utility in molecular wire and metal-metal bond chemistries. The complexes reported herein have been characterised by X-ray diffraction, NMR, IR, UV/Vis, and Mossbauer spectroscopies, cyclic voltammetry, density functional theory calculations, and elemental analyses, which have enabled us to elucidate the electronic structure of the complexes and probe the variation of iron redox properties as a function of varying the cyclopentadienyl or halide ligand.
机译：在回流的THF中用一当量的双（二苯基膦基）乙烷（dppe）处理无水FeX2（X = Cl，Br，I），得到分析纯白色（X = Cl），浅绿色（X = Br）和黄色（X ＝ I）[FeX 2（dppe）]（n）（X ＝ Cl，I; Br，II; I，III）。配合物I-III是出色的合成子，可用来制备一系列环戊二烯基衍生物。具体而言，用C5H5（Cp，系列1），C5Me5（Cp *，系列2），C5H4SiMe3（Cp'，系列3），C5H3（SiMe3）（2）（Cp''，系列4）和C5H3（Bu-t）（2）（Cp-tt，系列5）得到[Fe（Cp-dagger）（Cl）（dppe）] 1Cl-5Cl，[Fe（Cp-dagger）（Br （dppe）] 1Br-5Br和[Fe（Cp-dagger）（I）（dppe）] 1I-5I（Cp-dagger = Cp，Cp *，Cp'，Cp''或Cptt）。将1I-5I溶解在乙腈中，或用Me3SiI在乙腈中处理1Cl-5Cl（在其他溶剂中未观察到卤化物交换反应）得到分离的离子对络合物[Fe（Cp-dagger）（NCMe）（dppe）] [ I] 1SIP-5SIP。用多种还原剂（Li-Cs，KC8，Na / Hg）还原1Cl-5Cl，1Br-5Br和1I-5I的尝试均未成功。用LiAlH4处理1Cl-5Cl得到氢化物衍生物[Fe（Cp-dagger）（H）（dppe）] 1H-5H。该报告提供了制备这些配合物的可靠方法的系统说明，这些方法可用于分子线和金属-金属键合化学中。本文报道的配合物已通过X射线衍射，NMR，IR，UV / Vis和Mossbauer光谱，循环伏安法，密度泛函理论计算和元素分析进行​​了表征，这使我们能够阐明配合物的电子结构和考察了铁氧化还原特性随环戊二烯基或卤化物配体的变化。

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