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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >(Iminophosphoranyl)(thiophosphoranyl)methane rare-earth borohydride complexes: synthesis, structures and polymerization catalysis
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(Iminophosphoranyl)(thiophosphoranyl)methane rare-earth borohydride complexes: synthesis, structures and polymerization catalysis

机译：（亚氨基磷杂烷基）（硫代磷杂烷基）甲烷稀土硼氢化物配合物：合成，结构和聚合催化

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摘要

The (iminophosphoranyl)(thiophosphoranyl) methanide {CH(PPh2=NSiMe3)(PPh2=S)}-ligand has been used for the synthesis of divalent and trivalent rare-earth borohydride complexes. The salt metathesis of the potassium reagent [K{CH(PPh2-NSiMe3)(PPh2-S)}](2) with [Yb(BH4)(2)(THF)(2)] resulted in the divalent monoborohydride ytterbium complex [{CH(PPh2-NSiMe3)(PPh2=S)}Yb(BH4)(THF)(2)]. The 2D P-31/Yb-171 HMQC-NMR spectrum clearly showed the coupling between both nuclei. The trivalent bisborohydrides [{CH(PPh2=NSiMe3)(PPh2=S)}Ln(BH4)(2)(THF)] (Ln = Y, Sm, Tb, Dy, Er, Yb and Lu) were obtained by reaction of [K{CH(PPh2=NSiMe3)(PPh2=S)}](2) with [Ln(BH4)(3)(THF)(3)]. All new compounds were characterized by single X-ray diffraction. The divalent and trivalent compounds were next used as initiators in the ringopening polymerization (ROP) of epsilon-caprolactone (CL) and trimethylene carbonate (TMC). All complexes afforded a generally well-controlled ROP of both of these cyclic esters. High molar mass poly(epsilon-caprolactone) diols (M-n,(NMR) < 101 300 g mol(-1), D-M = 1.44), and alpha,omega-dihydroxy and alpha-hydroxy, omega-formate telechelic poly(trimethylene carbonate) s (M-n,M-NMR < 20 000 g mol(-1), D-M = 1.61) were thus synthesized under mild operating conditions.
机译：（亚氨基磷杂烷基）（硫代磷杂烷基）甲烷化物{CH（PPh2 = NSiMe3）（PPh2 = S）}-配体已用于合成二价和三价稀土硼氢化物配合物。钾试剂[K {CH（PPh2-NSiMe3）（PPh2-S）}]（2）与[Yb（BH4）（2）（THF）（2）]的盐复分解反应生成二价一硼氢化y配合物[ {CH（PPh2-NSiMe3）（PPh2 = S）} Yb（BH4）（THF）（2）]。 2D P-31 / Yb-171 HMQC-NMR光谱清楚地显示了两个原子核之间的耦合。三价双硼氢化物[{CH（PPh2 = NSiMe3）（PPh2 = S）} Ln（BH4）（2）（THF）]（Ln = Y，Sm，Tb，Dy，Er，Yb和Lu）通过[K {CH（PPh2 = NSiMe3）（PPh2 = S）}]（2）与[Ln（BH4）（3）（THF）（3）]。所有新化合物均通过单X射线衍射表征。接下来，将二价和三价化合物用作ε-己内酯（CL）和碳酸三亚甲基酯（TMC）的开环聚合（ROP）中的引发剂。所有复合物都提供了这两种环状酯的一般受控的ROP。高摩尔质量的聚（ε-己内酯）二醇（Mn，（NMR）<101300 g mol（-1），DM = 1.44），以及α，ω-二羟基和α-羟基，ω-甲酸酯远螯聚碳酸三亚甲基酯）s（Mn，M-NMR <20 000 g mol（-1），DM = 1.61）因此在温和的操作条件下合成。

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