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首页> 外文期刊>Chemistry: A European journal >Cyclopentadienyl Ruthenium(II) Complexes with Bridging Alkynylphosphine Ligands: Synthesis and Electrochemical Studies
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Cyclopentadienyl Ruthenium(II) Complexes with Bridging Alkynylphosphine Ligands: Synthesis and Electrochemical Studies

机译：具有桥烷基炔膦配体的环戊二烯基钌（II）配合物：合成和电化学研究

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摘要

The reaction of [CpRuCl-ACHTUNGTRENUNG(PPh3)2] (Cp=cyclopentadienyl) and [CpRuClACHTUNGTRENUNG(dppe)] (dppe=Ph2PCH2CH2PPh2) with bis- and trisphosphine ligands 1,4-(Ph2PCC)2C6H4 (1) and 1,3,5-(Ph2PC C)3C6H3 (2), prepared by Ni-catalysed cross-coupling reactions between terminal alkynes and diphenylchlorophosphine,has been investigated. Using metal-directed self-assembly methodologies,two linear bimetallic complexes,[{CpRuClACHTUNGTRENUNG(PPh3)}2ACHTUNGTRENUNG(m-dppab)] (3)and [{CpRuACHTUNGTRENUNG(dppe)}2ACHTUNGTRENUNG(m-dppab)]ACHTUNGTRENUNGPF6)2 (4),and the mononuclear complex [CpRuClACHTUNGTRENUNG(PPh3)CHTUNGTRENUNG(h1-dppab)] (6), which contains a “dangling arm” ligand, were prepared (dppab=1,4-bis[(diphenylphosphino) ethynyl]benzene).Moreover, by using the triphosphine 1,3,5- tris[(diphenylphosphino)ethynyl]benzene (tppab), the trimetallic [{CpRuCl- ACHTUNGTRENUNG(PPh3)}3ACHTUNGTRENUNG(m3-tppab )] (5) species was synthesised, which is the first example of a chiral-at-ruthenium complex containing three different stereogenic centres. Besides these open-chain complexes, the neutral cyclic species [{CpRuClACHTUNGTRENUNG(mdppab)} 2] (7) was also obtained under different experimental conditions. The coordination chemistry of such systems towards supramolecular assemblies was tested by reaction of the bimetallic precursor 3 with additional equivalents of ligand 2. Two rigid macrocycles based on cis coordination of dppab to [CpRu- ACHTUNGTRENUNG(PPh3)] were obtained, that is, the dinuclear complex [{CpRuACHTUNGTRENUNG(PPh3)ACHTUNGTRENUNG(mdppab)} 2]ACHTUNGTRENUNG(PF6)2 (8) and the tetranuclear square [{CpRuACHTUNGTRENUNG(PPh3)ACHTUNGTRENUNG(mdppab)} 4]ACHTUNGTRENUNG(PF6)4 (9). The solid-state structures of 7 and 8 have been determined by X-ray diffraction analysis and show a different arrangement of the two parallel dppab ligands. All compounds were characterised by various methods including ESIMS, electrochemistry and by X-band ESR spectroscopy in the case of the electrogenerated paramagnetic species.
机译：[CpRuCl-ACHTUNGTRENUNG（PPh3）2]（Cp =环戊二烯基）和[CpRuClACHTUNGTRENUNG（dppe）]（dppe = Ph2PCH2CH2PPh2）与双膦和三膦配体1,4-（Ph2PCC）2C6H4（1）和1,3的反应研究了由Ni催化的末端炔烃与二苯基氯膦的交叉偶联反应制得的1,5-（Ph2PC C）3C6H3（2）。使用金属定向自组装方法，两个线性双金属络合物，[{CpRuClACHTUNGTRENUNG（PPh3）} 2ACHTUNGTRENUNG（m-dppab）]（3）和[{CpRuACHTUNGTRENUNG（dppe）} 2ACHTUNGTRENUNG（m-dppab）] ACHTUNGTRENUNGPF6） 4），并制备了含有“悬臂”配体的单核络合物[CpRuClACHTUNGTRENUNG（PPh3）CHTUNGTRENUNG（h1-dppab）]（6）（dppab = 1,4-双[（二苯基膦基）乙炔基]苯）此外，通过使用三膦1,3,5-三[（二苯基膦基）乙炔基]苯（tppab），合成了三金属[{CpRuCl- ACHTUNGTRENUNG（PPh3）} 3ACHTUNGTRENUNG（m3-tppab）]（5）种，这是包含三个不同的立体异构中心的手性钌络合物的第一个例子。除了这些开链配合物外，还可以在不同的实验条件下获得中性环状物种[{CpRuClACHTUNGTRENUNG（mdppab）} 2]（7）。通过双金属前体3与另外等价的配体2的反应，测试了此类系统对超分子组装体的配位化学。获得了两个基于dppab与[CpRu-ACTHUNGTRENUNG（PPh3）]顺式配位的刚性大环，即双核复合物[{CpRuACHTUNGTRENUNG（PPh3）ACHTUNGTRENUNG（mdppab）} 2] ACHTUNGTRENUNG（PF6）2（8）和四核正方形[{CpRuACHTUNGTRENUNG（PPh3）ACHTUNGTRENUNG（mdppab）} 4] ACHTUNGTRENUNG（PF6）4（9）。 7和8的固态结构已通过X射线衍射分析确定，并显示了两个平行dppab配体的不同排列。对于所有化合物，均采用多种方法进行了表征，包括ESIMS，电化学方法以及在产生电顺磁物质的情况下通过X波段ESR光谱学进行了表征。

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