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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >Group 1 and group 2 metal complexes supported by a bidentate bulky iminopyrrolyl ligand: synthesis, structural diversity, and epsilon-caprolactone polymerization study
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Group 1 and group 2 metal complexes supported by a bidentate bulky iminopyrrolyl ligand: synthesis, structural diversity, and epsilon-caprolactone polymerization study

机译：二齿庞大的亚氨基吡咯基配体支持的第1组和第2组金属配合物：合成，结构多样性和ε-己内酯聚合研究

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We report here a series of alkali and alkaline earth metal complexes, each with a bulky iminopyrrolyl ligand [2-(Ph3CN=CH)C4H3NH] (1-H) moiety in their coordination sphere, synthesized using either alkane elimination or silylamine elimination methods or the salt metathesis route. The lithium salt of molecular composition [Li(2-(Ph3CN=CH)C4H3N)(THF)(2)] (2) was prepared using the alkane elimination method, and the silylamine elimination method was used to synthesize the dimeric sodium and tetranuclear potassium salts of composition [(2-(Ph3CN=CH)C4H3N)Na(THF)](2) (3) and [(2-(Ph3CN=CH)C4H3N)K(THF)(0.5)](4) (4) respectively. The magnesium complex of composition [(THF)(2)Mg(CH2Ph){2-(Ph3CN=CH)C4H3N}] (5) was synthesized through the alkane elimination method, in which [Mg(CH2Ph)(2)(OEt2)(2)] was treated with the bulky iminopyrrole ligand 1-H in 1 : 1 molar ratio, whereas the bis(iminopyrrolyl) magnesium complex [(THF)(2)Mg{2-(Ph3CN=CH)C4H3N}(2)] (6) was isolated using the salt metathesis route. The heavier alkaline earth metal complexes of the general formula {(THF)(n)M(2-(Ph3CN=CH)C4H3N)(2)} [M = Ca (7), Sr (8), and n = 2; M = Ba (9), n = 3] were prepared in pure form using two synthetic methods: in the first method, the bulky iminopyrrole ligand 1-H was directly treated with the alkaline earth metal precursor [M{N(SiMe3)(2)}(2)(THF)(n)] (where M = Ca, Sr and Ba) in 2 : 1 molar ratio in THF solvent at ambient temperature. The complexes 7-9 were also obtained using the salt metathesis reaction, which involves the treatment of the potassium salt (4) with the corresponding metal diiodides MI2 (M = Ca, Sr and Ba) in 2 : 1 molar ratio in THF solvent. The molecular structures of all the metal complexes (1-H, 2-9) in the solid state were established through single-crystal X-ray diffraction analysis. The complexes 5-9 were tested as catalysts for the ring-opening polymerization of e-caprolactone. High activity was observed in the heavier alkaline earth metal complexes 7-9, with a very narrow polydispersity index in comparison to that of magnesium complexes 5 and 6.
机译：我们在这里报告了一系列碱金属和碱土金属配合物，每个配合物在它们的配位域中都有一个庞大的亚氨基吡咯基配体[2-（Ph3CN = CH）C4H3NH]（1-H）部分，是使用烷烃消除或甲硅烷基胺消除方法合成的，或者盐易位途径。使用烷烃消除法制备分子组成为[Li（2-（Ph3CN = CH）C4H3N）（THF）（2）]的锂盐，并使用甲硅烷基胺消除法合成二聚钠和四核组成为[（2-（Ph3CN = CH）C4H3N）Na（THF）]（2）（3）和[[2-（Ph3CN = CH）C4H3N）K（THF）（0.5）]（4）的钾盐（ 4）分别。通过烷烃消除法合成了组成为[（THF）（2）Mg（CH2Ph）{2-（Ph3CN = CH）C4H3N}]（5）的镁配合物，其中[Mg（CH2Ph）（2）（OEt2 ）（2）]以1：1的摩尔比用笨重的亚氨基吡咯配体1-H处理，而双（亚氨基吡咯烷基）镁配合物[（THF）（2）Mg {2-（Ph3CN = CH）C4H3N}（2 ）]（6）使用盐易位途径进行分离。通式{（THF）（n）M（2-（Ph3CN = CH）C4H3N）（2）}的较重的碱土金属配合物[M = Ca（7），Sr（8）和n = 2; M = Ba（9），n = 3]是通过两种合成方法以纯净形式制备的：在第一种方法中，将笨重的亚氨基吡咯配体1-H直接用碱土金属前体[M {N（SiMe3）（ 2）}（2）（THF）（n）]（其中M ＝ Ca，Sr和Ba）在室温下在THF溶剂中的摩尔比为2∶1。还使用盐复分解反应获得了配合物7-9，该反应涉及在THF溶剂中以2：1的摩尔比用相应的金属二碘化物MI2（M = Ca，Sr和Ba）处理钾盐（4）。通过单晶X射线衍射分析，确定了所有固态金属配合物（1-H，2-9）的分子结构。测试了配合物5-9作为ε-己内酯的开环聚合的催化剂。在较重的碱土金属配合物7-9中观察到高活性，与镁配合物5和6相比，其多分散指数非常窄。

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