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首页> 外文期刊>Organometallics >A Study of Ligand Coordination at Lanthanide and Group 4 Metal Centers by Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry
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A Study of Ligand Coordination at Lanthanide and Group 4 Metal Centers by Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry

机译：基质辅助激光解吸/电离飞行时间质谱研究镧系元素和第4组金属中心的配体配位

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摘要

Reactions of lanthanide amide reagents Ln {N(SiMe3)(2)}(3) (where Ln = Sm, Gd, Ho, or Yb) with amine-bis(phenol) ligands were probed using inert atmosphere matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry (MS) (anthracene matrix); the technique rapidly confirms ligand coordination, giving excellent agreement with theoretical isotope patterns for lanthanide(amine-phenolate) fragments. Spectra on isolated lanthanide amine-bis(phenolate) amido complexes are similar to those seen from small scale parallel reactions of metal amides and protonated ligands. Although in all cases molecular ion peaks are not observed, peaks for lanthanide arene complexes, [M + arene](+center dot), formed in situ, are seen. The lack of molecular ion peak is due to difficulties in ionizing Ln(3+) complexes by charge transfer. However, if Nujol is used to disperse the analyte and matrix prior to analysis rather than toluene, arene adducts are not observed. Similar phenol-derived ligands can be reacted with diamagnetic M(NMe2)(4) (where M = Ti or Zr), and amine-phenolate complex formation is again confirmed easily by MALDI-TOF MS or LDI-TOF MS (no matrix). These complexes were also characterized by NMR spectroscopy and elemental analysis on isolated samples.
机译：镧系酰胺试剂Ln {N（SiMe3）（2）}（3）（其中Ln = Sm，Gd，Ho或Yb）与胺-双（酚）配体的反应采用惰性气氛基质辅助激光解吸/电离飞行时间（MALDI-TOF）质谱（MS）（蒽基质）;该技术迅速证实了配体的配位，与镧系元素（胺-酚盐）片段的理论同位素图非常吻合。分离的镧系元素胺-双（酚盐）酰胺配合物的光谱类似于从金属酰胺和质子化配体的小规模平行反应中看到的光谱。尽管在所有情况下均未观察到分子离子峰，但可以看到原位形成的镧系元素芳烃络合物[M +芳烃]（+中心点）的峰。分子离子峰的缺乏是由于难以通过电荷转移将Ln（3+）络合物电离。但是，如果在分析之前使用Nujol而不是甲苯来分散分析物和基质，则不会观察到芳烃加合物。相似的酚衍生配体可以与抗磁性M（NMe2）（4）（其中M = Ti或Zr）反应，并且可以通过MALDI-TOF MS或LDI-TOF MS轻松确认胺-酚盐络合物的形成（无基质） 。这些配合物还通过NMR光谱和对分离样品的元素分析来表征。

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