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首页> 外文期刊>Zeitschrift fur Anorganische und Allgemeine Chemie >Synthesis and structure of two- and three-nuclear heterometallic complexes with nitrido bridges between Re and Mo [German]
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Synthesis and structure of two- and three-nuclear heterometallic complexes with nitrido bridges between Re and Mo [German]

机译：Re和Mo之间带有亚硝基桥的二核和三核异金属配合物的合成和结构[德语]

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The reaction of ReNCl2(PMe2Ph)(3) with MoCl4(NCEt)(2) yields the heterometallic threenuclear complex [{(Me2PhP)(3)(EtCN) ClRe = N-}(2)MoCl4][MoNCl5]. The anion [MoNCl5](2-) presumably results from a transfer of the nitrido ligand from the Re to the Mo atom. The air-sensitive compound is paramagnetic with mu(eff) = 2.87 B. M. at room temperature. A reduction of the magnetic moment to 1.74 B.M at 20 K starts at 140K. The complex crystallizes in the orthorhombic space group Pca2(1) with a = 2430(1), b = 1328(1), c = 2436.3(2) pm, Z = 4. With bond angles Re-N-Mo of 164 degrees and 167 degrees the nitrido bridges are almost linear. The distances Re-N of 169 and 170 pm can be interpreted with triple bonds. The Mo-N bond lengths of 210 and 211 pm correspond to single bonds. In the anion [MoNCl5](2-) the distance Mo = N is 167 pm. Hydrolysis of the threenuclear complex results in a cleavage of one of the nitrido bridges to yield (Me2PhP)(3)(EtCN) ClRe = N-MoOCl4. The compound is paramagnetic with mu(eff) = 1.71 B.M. at room temperature. It crystallizes in the orthorhombic space group Pbca with a = 1718.5(4), b = 2037(1), c = 2041.1(7) pm, Z = 8. In the dinu- clear complex the [MoOCl4](-) unit is only weakly coordinated to the nitrido ligand with Mo-N = 246.5 pm, while the distance of the Re = N bond of 168.1 pm is almost unchanged in comparison with a terminal bond. The bond angle Re = N-Mo is 165.6 degrees. [References: 21]
机译：ReNCl2（PMe2Ph）（3）与MoCl4（NCEt）（2）反应生成异金属三核络合物[{（Me2PhP）（3）（EtCN）ClRe = N-}（2）MoCl4] [MoNCl5]。阴离子[MoNCl5]（2-）可能是由于亚硝基配体从Re转移到Mo原子而产生的。空气敏感化合物在室温下为顺磁性，mu（eff）= 2.87 B. M.。在20 K时将磁矩减小到1.74 B.M从140K开始。该复合物在正交晶体空间群Pca2（1）中结晶，其中a = 2430（1），b = 1328（1），c = 2436.3（2）pm，Z =4。键角Re-N-Mo为164度167度的亚硝基桥几乎是线性的。 Re-N 169和170 pm的距离可以用三键解释。 Mo-N键的长度为210和211 pm对应于单键。在阴离子[MoNCl5]（2-）中，距离Mo = N为167 pm。三核复合物的水解导致一个亚硝基桥的裂解，得到（Me2PhP）（3）（EtCN）ClRe = N-MoOCl4。该化合物是顺磁性的，mu（eff）= 1.71B.M。在室温下。它在正交晶体空间群Pbca中结晶，其a = 1718.5（4），b = 2037（1），c = 2041.1（7）pm，Z =8。在双核络合物中，[MoOCl4]（-）单元为Mo-N = 246.5 pm时，它仅与弱配位基团配合，而Re = N键的距离168.1 pm与末端键相比几乎没有变化。结合角Re ＝ N-Mo为165.6度。 [参考：21]

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