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首页> 外文期刊>Polyhedron: The International Journal for Inorganic and Organometallic Chemistry >An imidazole-based P-N bridging ligand and its binuclear copper(I), silver(I) and palladium(I) complexes: synthesis, characterizations and X-ray structures
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An imidazole-based P-N bridging ligand and its binuclear copper(I), silver(I) and palladium(I) complexes: synthesis, characterizations and X-ray structures

机译：咪唑基P-N桥联配体及其双核铜（I），银（I）和钯（I）配合物：合成，表征和X射线结构

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摘要

Reaction of I -methylimidazole with n-BuLi in tetrahydrofuran at — 780C followed by addition of chlorodiphenyiphosphine afforded a P—N bridging ligand, 2~(diphenylphosphino)~1-methYlimidaZOle (dpim) in good yield. The structure of the ligand was determined by single crystal X-ray analysis. Reaction of a stoichiometric amount of the ligand with [Cu(MeCN)4]ClO4 in acetonitrile led to the binuclear complex [Cu2(j~i~dpim)3(MeCN)1(CIO4)i2CHiCN (V2CH3CN), whose structure was determined by single crystal X-ray analysis. The solid state structure shows that the two copper ions are held by three dpim ligands and the coordination geometry around each metal atom is different, one being three- and the other being four-coordinated. One of the copper ions forms a distorted tetrahedral array with two P and one N atoms from the dpim ligand and an additional N atom from an acetonitrile ligand, whereas the other copper ion is three coordinated with two N and one P atoms from the dpim ligand. The nitrate-bridged polymeric silver(I) complex. {[Ag2(j.t~dpim)2(NO3)I(NOi)}~ (2) was prepared by the reaction of equimolar amounts of the ligand and silver nitrate in methanol and was characterized by IR, NMR and X-ray analysis. The dimeric unit, [Ag2(p-dpim)j. possesses an eight-membered annular core structure with two ligands bridging the two metal ions in a head-to-tail configuration. Two types of nitrate ions are present in 2: one makes an infinite one-dimensional chain by joining the dimeric units through its two oxygen atoms in an anti—anti bridging mode whereas the other is disordered with a half occupancy and is located at the left and right sides of the chain. The dynamic behavior of 2 in acetone was also studied by variable temperature 31P NMR. The binuclear palladiurn(I) complex [Pd,C12(dpim)2] (4) was prepared by a conproportionation reaction between complex [PdCI2(dpim)j (3) and [Pd(dba)2] (dba = dibenzylideneaceton). Only one geometric isomer, probably head-to-tail (HT), was formed in this reaction. Complex 3 was prepared by treating [PdCI2(PhCN)2] with two moles of ligand in dichloromethane solution. In this complex the ligand acts as a P-monodentate. In solution it exists as a mixture of cis and trans isomers.
机译：I-甲基咪唑与正丁基锂在四氢呋喃中于780°C反应，然后添加氯二苯膦基膦，以高收率得到PN桥联配体2〜（二苯基膦基）〜1-甲基咪唑（dpim）。配体的结构通过单晶X射线分析确定。化学计量的配体与乙腈中的[Cu（MeCN）4] ClO4反应生成双核络合物[Cu2（j〜i〜dpim）3（MeCN）1（CIO4）i2CHiCN（V2CH3CN）通过单晶X射线分析。固态结构表明，两个铜离子由三个dpim配体保持，每个金属原子周围的配位几何结构不同，一个为3配位，另一个为4配位。其中一个铜离子形成扭曲的四面体阵列，其中两个dpim配体中的两个P和一个N原子，另一个来自乙腈配体的N原子，而另一个铜离子与三个dpim配体中的两个N和一个P原子配位。硝酸盐桥接的聚合银（I）配合物。 {[Ag2（j.t〜dpim）2（NO3）I（NOi）}〜（2）是通过等摩尔量的配体与硝酸银在甲醇中反应制备的，并通过IR，NMR和X射线分析对其进行表征。二聚体单位[Ag2（p-dpim）j。拥有一个八元环形核结构，带有两个配体以首尾相连的方式桥接两个金属离子。 2中存在两种类型的硝酸根离子：一种通过反二桥模式通过其两个氧原子连接二聚体单元而构成无限的一维链，而另一种则占据了一半的空间，位于左侧。和链的右侧。还通过可变温度31 P NMR研究了2在丙酮中的动力学行为。通过复合物[PdCI2（dpim）j（3）与[Pd（dba）2]（dba =二苄叉亚丙酮）之间的配位反应制备双核pallaururn（I）复合物[Pd，C12（dpim）2]（4）。在该反应中仅形成了一种几何异构体，可能是头对尾（HT）。配合物3是通过在二氯甲烷溶液中用两摩尔的配体处理[PdCl2（PhCN）2]制备的。在该络合物中，配体起P-单齿的作用。在溶液中，它以顺式和反式异构体的混合物形式存在。

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