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首页> 外文期刊>Chemistry: A European journal >Formation of Two Isomeric closo-[(eta~5-C_5H_5)FePC_2B_8H_10] Phosphadicarbaborane Analogues of Ferrocene via Isolable eta~1-Bonded Complexes of the [7-{(eta~5-C_5H_5)Fe(CO)_2}-(eta~1-nido-PC_2B_8H_10)] Type
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Formation of Two Isomeric closo-[(eta~5-C_5H_5)FePC_2B_8H_10] Phosphadicarbaborane Analogues of Ferrocene via Isolable eta~1-Bonded Complexes of the [7-{(eta~5-C_5H_5)Fe(CO)_2}-(eta~1-nido-PC_2B_8H_10)] Type

机译：通过[7-{（eta〜5-C_5H_5）Fe（CO）_2}-（eta）的可分离的eta〜1-键合络合物形成二茂铁Closo-[[（eta〜5-C_5H_5）FePC_2B_8H_10]膦二茂铁类似物〜1-nido-PC_2B_8H_10）]类型

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The reaction of nido-[7,8,9-PC_2B_8H_11] (1) with [{CpFe(CO)_2}_2] (Cp = eta~5-C_5H_5~-) in benzene (reflux, 3 days) gave an eta~1-bonded complex [7-Fp(eta~1-nido-7,8,9,-PC_2B_8H_10)] (2; Fp = CpFe(CO)_2; yield 38%). A similar reaction at elevated temperatures (xylene, reflux 24 h) gave the isomeric complex [7-Fp-(eta~1-nido-7,9,10-PC_2H_8H_10)] (3; yield 28%) together with the fully sandwiched complexes [1-Cp-closo-1,2,4,5-FePC_2B_8H_10] 4a (yield 30%) and [1-Cp-closo-1,2,4,8-FePC_2B_8H_10] 4b (yield 5%). Compounds 2 and 3 are isolable intermediates along the full eta~5-complexation pathway of the phosphadicarbaborane cage; their heating (xylene, reflux, 24 h) leads finally to the isolation of compounds 4a (yields 46 and 52%, respectively) and 4b (yields 4 and 5%, respectively). Moreover, compound 3 is isolated as a side product from the heating of 2 (yield 10%). The structure of compound 4a was determined by an X-ray structural analysis and the constitution of all compounds is consistent with the results of mass spectrometry and IR spectroscopy. Multinuclear (~1H, ~11B, ~31P, and ~13C), two-dimensional [~11B-~11B]-COSY, and ~1H{~11B(selective)} magntic resonance measurements led to complete resonance measurements led to complete assignments of all resonances and are in excellent agreement with the structures proposed.
机译：nido- [7,8,9-PC_2B_8H_11]（1）与[{CpFe（CO）_2} _2]（Cp = eta〜5-C_5H_5〜-）在苯中的反应（回流，3天），得到eta约1键合的复合物[7-Fp（eta-1-nido-7,8,9，-PC_2B_8H_10）]（2; Fp = CpFe（CO）_2;产率38％）。在升高的温度下（二甲苯，回流24小时）进行类似的反应，得到同分异构的复合物[7-Fp-（eta〜1-nido-7,9,10-PC_2H_8H_10）]（3;收率28％）以及完全夹心的结构配合物[1-Cp-closo-1,2,4,5-FePC_2B_8H_10] 4a（产率30％）和[1-Cp-closo-1,2,4,8-FePC_2B_8H_10] 4b（产率5％）。化合物2和3是沿着磷二碳硼烷笼的完整eta-5络合路径分离的中间体。它们的加热（二甲苯，回流，24小时）最终导致分离出化合物4a（分别产率46和52％）和4b（产率4和5％）。另外，从2的加热中分离出化合物3作为副产物（收率10％）。通过X射线结构分析确定化合物4a的结构，并且所有化合物的组成与质谱和IR光谱的结果一致。多核（〜1H，〜11B，〜31P和〜13C），二维[〜11B-〜11B] -COSY和〜1H {〜11B（选择性）}的磁共振测量可导致完整的谐振测量，从而完成所有共振的分配，并与拟议的结构极为一致。

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