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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >Cyclopalladation of telluro ether ligands: synthesis, reactivity and structural characterization
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Cyclopalladation of telluro ether ligands: synthesis, reactivity and structural characterization

机译：碲醚配体的环钯缩合：合成，反应性和结构表征

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摘要

Treatment of [PdCl_2(PhCN)_2] with diaryl telluride in 1: 2 molar ratio gave mononuclear palladium complexes, trans-[PdCl_2(TeR_2)_2] (1) (R = Mes (1a) (Mes = 2,4,6-trimethylphenyl), Ph (1b), o-tol (1c) (o-tol = ortho-tolyl)). Reaction of [PdCl_2(TeMes_2)_2] with one equivalent of [PdCl_2(PhCN)_2] or Na_2PdCl_4 with TeRR’ afforded chloro-bridged binuclear complexes, [Pd_2(μ-Cl)_2Cl_2(TeRR’)_2] (2) (R/R’ = Mes/Mes (2a); Mes/Ph (2b); Ph/Ph (2c)). A toluene–methanol solution of trans-[PdCl_2(TeMes_2)_2] on refluxing for 30 minutes yielded a binuclear cyclopalladated complex, [Pd_2(μ-Cl)_2{CH_2C_6H_2(4,6-Me_2)TeMes)}_2] (3). When the refluxing was prolonged, a mononuclear complex cis-[PdCl_2{MesTeCH_2C_6H_2(4,6-Me_2)TeMes}] (4) was isolated. Treatment of palladium acetate with TeMes_2 afforded an acetato-bridged analogue of 3, [Pd_2(μ-OAc)_2{CH_2C_6H_2(4,6-Me_2)TeMes}_2] (5a) together with a very minor component, a tetranuclear complex, [Pd(μ-OAc)(μ-TeMes)]_4 (6). This reaction with unsymmetrical tellurides, MesTeR, also gave cyclopalladated complexes [Pd_2(μ-OAc)_2{CH_2C_6H_2(4,6-Me_2)TeR}_2] (R = o-tol (5b) and Ph (5c)) in which 2-methyl of the mesityl group of the telluride was exclusively metallated. The complex trans-[PdCl_2(TeMes_2)_2] on refluxing in xylene gave palladium telluride, Pd_7Te_3. These complexes were characterized by elemental analyses, IR and NMR (~1H, ~(13)C and ~(125)Te) spectroscopy. The molecular structures of trans-[PdCl_2(TeMes_2)_2] (1a), [Pd_2(μ-Cl)_2Cl_2(TeMes_2)_2]·2acetone (2a·2acetone), cis-[PdCl_2{MesTeCH_2C_6H_2(4,6-Me_2)TeMes}] (4), [Pd_2-(μ-OAc)_2{CH_2C_6H_2(4,6-Me_2)TeMes)}_2]·toluene (5a·toluene), [Pd_2(μ-OAc)_2{CH_2C_6H_2(4,6-Me_2)Tetol-o}_2] (5b) and [Pd(μ-OAc)(μ-TeMes)]_4 (6) were established by single crystal X-ray diffraction analyses. The mononuclear complex 1a was isolated in two polymorphic forms each with the trans configuration.
机译：以1：2摩尔比用二芳基碲化物处理[PdCl_2（PhCN）_2]得到单核钯配合物，反式[PdCl_2（TeR_2）_2]（1）（R = Mes（1a）（Mes = 2,4,6 -三甲基苯基），Ph（1b），邻甲苯基（1c）（邻甲苯基=邻甲苯基）。 [PdCl_2（TeMes_2）_2]与一当量的[PdCl_2（PhCN）_2]或Na_2PdCl_4与TeRR'的反应提供了氯桥联双核络合物[Pd_2（μ-Cl）_2Cl_2（TeRR'）_ 2]（2）（ R / R'= Mes / Mes（2a）; Mes / Ph（2b）; Ph / Ph（2c））。反式[PdCl_2（TeMes_2）_2]的甲苯-甲醇溶液回流30分钟，得到双核环钯配合物[Pd_2（μ-Cl）_2 {CH_2C_6H_2（4,6-Me_2）TeMes）} _ 2]（3 ）。当延长回流时间时，分离出单核复合物顺式-[PdCl_2 {MesTeCH_2C_6H_2（4,6-Me_2）TeMes}]（4）。用TeMes_2处理乙酸钯可得到3 [[Pd_2（μ-OAc）_2 {CH_2C_6H_2（4,6-Me_2）TeMes} _2]（5a）的乙酰桥连类似物，以及极少量的四核配合物， [Pd（μ-OAc）（μ-TeMes）] _ 4（6）。这种与不对称碲化物MesTeR的反应还产生了环钯配合物[Pd_2（μ-OAc）_2 {CH_2C_6H_2（4,6-Me_2）TeR} _2]（R = o-tol（5b）和Ph（5c）），其中碲化物的异丁基的2-甲基仅被金属化。在二甲苯中回流时的复合反式-[PdCl_2（TeMes_2）_2]得到碲化钯，Pd_7Te_3。这些配合物通过元素分析，IR和NMR（〜1H，〜（13）C和〜（125）Te）光谱进行表征。反式-[PdCl_2（TeMes_2）_2]（1a），[Pd_2（μ-Cl）_2Cl_2（TeMes_2）_2]·2丙酮（2a·2丙酮），顺式-[PdCl_2 {MesTeCH_2C_6H_2（4,6-Me_2） ）TeMes}]（4），[Pd_2-（μ-OAc）_2 {CH_2C_6H_2（4,6-Me_2）TeMes）} _ 2]·甲苯（5a·甲苯），[Pd_2（μ-OAc）_2 {CH_2C_6H_2（通过单晶X射线衍射分析建立了[4,6-Me_2）Tetol-o} _2]（5b）和[Pd（μ-OAc）（μ-TeMes）] _ 4（6）。单核络合物1a以两种多态形式分离，每种形式具有反式构型。

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