Dinuclear dysprosium and ytterbium complexes incorporating N,NBis(pyrrolylαmethyl)-N-methylamine ligand: Syntheses and structures

Zhou F.; Zhang S.; Zhao Y.; Li C.Z.; Cheng X.; Zheng L.; Zhang Y.; Li Y.

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Dinuclear dysprosium and ytterbium complexes incorporating N,NBis(pyrrolylαmethyl)-N-methylamine ligand: Syntheses and structures

机译：N，NBis（吡咯基α甲基）-N-甲胺配体的双核和配合物：合成与结构

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Reaction of DyCl_3 with two equivalents of NaN(SiMe _3)_2 in THF yielded {Dy(μ-Cl)[N(SiMe_3) _2MTHF)}_2 (1). X-ray crystal structure analysis revealed that 1 is a centrosymmetric dimer with asymmetrically bridging chloride ligands. The metal coordination arrangement can be best described as distorted trigonal bipyramid. The bond lengths of Ln-CI and Ln-N showed a decreasing trend with the contraction of the size of Ln~3+. Treatment of N,N-bis(pyrrolyl- &aleha-methyl)-Af-methyl- amine (H2dpma) with 1 and known compound {Yb(μ-Cl)[N- (SiMe_3)_2]_2(THF)} _2, respectively, led to the formations of [Dy(&mu- Cl)(dpma)(THF)_2]_2 (2) and {Yb(μ-Cl)[N(SiMe _3)_2]_2THF)}_2 (3). Com- pounds 2 and 3 were fully characterized by single-crystal X-ray crystallography, elemental analysis, and ~1H NMR spectroscopy. Structure determination indicated that 2 and 3 exhibit as centrosymmetric dimers with asymmetrically bridging chloride ligands. One pot reactions involving LnCl_3 (Ln = Dy and Yb), LiN(SiMe_3)_2, and H2dpma were explored and desired products 2 and 3 were not yielded, which indicated that 1 and {Yb(μ-Cl)[N(SiMe_3)_2]_2(THF)}_2 are the demanding precursors to synthesize Dysprosium and Ytterbium complexes supported by dpma 2-ligand. Compounds 2 and 3 are the first reported lanthanide complexes chelated by dpma 2-ligand.

机译：DyCl_3与两当量的NaN（SiMe _3）_2在THF中反应生成{Dy（μ-Cl）[N（SiMe_3）_2MTHF）} _ 2（1）。 X射线晶体结构分析表明1是具有不对称桥联的氯配体的向心二聚体。金属配位结构可以最好地描述为扭曲的三角双锥。 Ln-Cl和Ln-N的键长随Ln〜3 +尺寸的减小而减小。用1和已知的化合物{Yb（μ-Cl）[N-（SiMe_3）_2] _2（THF）} _2处理N，N-双（吡咯基-＆aleha-甲基）-Af-甲基胺（H2dpma）分别导致[Dy（μCl）（dpma）（THF）_2] _2（2）和{Yb（μ-Cl）[N（SiMe _3）_2] _2THF）} _ 2（3）的形成。通过单晶X射线晶体学，元素分析和〜1H NMR光谱对化合物2和3进行了全面表征。结构确定表明2和3表现为具有不对称桥连的氯配体的中心对称二聚体。探索了涉及LnCl_3（Ln = Dy和Yb），LiN（SiMe_3）_2和H2dpma的一锅反应，未产生所需的产物2和3，表明1和{Yb（μ-Cl）[N（SiMe_3） _2] _2（THF）} _ 2是合成dpma 2-配体支持的Dy和and配合物的前体。化合物2和3是被dpma 2-配体螯合的首次报道的镧系元素络合物。

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《Zeitschrift fur Anorganische und Allgemeine Chemie》 |2009年第15期|共6页
作者
Zhou F.; Zhang S.; Zhao Y.; Li C.Z.; Cheng X.; Zheng L.; Zhang Y.; Li Y.;
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正文语种 eng
中图分类化学;
关键词
Chlorine; Dimer; Dysprosium; X-ray diffraction; Ytterbium;

机译：氯;二聚体;D;X射线衍射;Y;

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Dinuclear dysprosium and ytterbium complexes incorporating N,NBis(pyrrolylαmethyl)-N-methylamine ligand: Syntheses and structures

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