Synthesis and structural characterization of a heptanuclear heterometallic neodymium complex with dinitrogen tetroxide O2N‒NO2 as a tetradentate linker

IF 4.7 2区化学 Q2 CHEMISTRY, PHYSICAL Journal of Molecular Structure Pub Date : 2025-03-26 DOI:10.1016/j.molstruc.2025.142129

Yi-Jie Li, Yao Cheng, Yang Gao, Ai-Quan Jia, Qian-Feng Zhang

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Abstract

A {Mo₄Nd₃} complex of [{η¹-(Me₃tacn)Mo(O)₃}₂Nd(O)₂(μ-N₂O₄)]₂Nd(OH₂)₄ (1) and an ionic {Mo₂Pr} complex [{(Me₃tacn)MoO₂}₂(μ-O)][Pr(NO₃)₅(H₂O)] (2) were obtained from coordination reactions of the metalloligand [(Me₃tacn)MoO₃] with Nd₂O₃ or Pr₆O₁₁ in the presence of nitric acid in aqueous methanol solution. While reactions of [(Me₃tacn)MoO₃] with Ce(NO₃)₃ or Pr(NO₃)₃ afforded two ionic complexes of the type [(Me₃tacn)MoO₂(OH)]₄[M(NO₃)₆](NO₃)·(HNO₃) (3: M = Ce, 4: M = Pr). Complexes 1 − 4 were characterized by infrared, UV–vis, fluorescence, Raman spectroscopies and mass spectrometry. Moreover, molecular structures of complex 1 − 4 are determined by single-crystal X-ray crystallography, as well as powder X-ray diffraction. The study of X-ray crystallography revealed that the three Nd centers in complex 1 are linked by two symmetric dinitrogen tetroxide units via oxygen atoms with Nd‒O_N2O4 bond lengths of 2.259(14) and 2.454(14) Å.

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以四氧化二氮O2N-NO2为四齿连接剂的七核异金属钕配合物的合成及结构表征

在硝酸存在下，金属配体[(Me3tacn)MoO3]与Nd2O3或Pr6O11在甲醇水溶液中进行配位反应，得到了[{η1-(Me3tacn)Mo(O)3}2Nd(O)2(μ-N2O4)]2Nd(OH2)4(1)和离子{Mo2Pr}配合物[{(Me3tacn)MoO2}2(μ-O)][Pr(NO3)5(H2O)](2)。而[(Me3tacn)MoO3]与Ce(NO3)3或Pr(NO3)3反应生成[(Me3tacn)MoO2(OH)]4[M(NO3)6]（NO3）·（HNO3）（3: M = Ce, 4: M = Pr）两种离子配合物。配合物1 ~ 4通过红外、紫外-可见、荧光、拉曼光谱和质谱进行了表征。此外，通过单晶x射线晶体学和粉末x射线衍射确定了配合物1−4的分子结构。x射线晶体学研究表明，配合物1中的三个Nd中心由两个对称的四氧化二氮单元通过氧原子连接，Nd - on2o4键长分别为2.259（14）和2.454（14）Å。

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来源期刊

Journal of Molecular Structure 化学-物理化学

CiteScore

7.10

自引率

15.80%

发文量

2384

审稿时长

45 days

期刊介绍： The Journal of Molecular Structure is dedicated to the publication of full-length articles and review papers, providing important new structural information on all types of chemical species including: • Stable and unstable molecules in all types of environments (vapour, molecular beam, liquid, solution, liquid crystal, solid state, matrix-isolated, surface-absorbed etc.) • Chemical intermediates • Molecules in excited states • Biological molecules • Polymers. The methods used may include any combination of spectroscopic and non-spectroscopic techniques, for example: • Infrared spectroscopy (mid, far, near) • Raman spectroscopy and non-linear Raman methods (CARS, etc.) • Electronic absorption spectroscopy • Optical rotatory dispersion and circular dichroism • Fluorescence and phosphorescence techniques • Electron spectroscopies (PES, XPS), EXAFS, etc. • Microwave spectroscopy • Electron diffraction • NMR and ESR spectroscopies • Mössbauer spectroscopy • X-ray crystallography • Charge Density Analyses • Computational Studies (supplementing experimental methods) We encourage publications combining theoretical and experimental approaches. The structural insights gained by the studies should be correlated with the properties, activity and/ or reactivity of the molecule under investigation and the relevance of this molecule and its implications should be discussed.