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Silver, Gold, Palladium, and Platinum N-heterocyclic Carbene Complexes Containing a Selenoether-Functionalized Imidazol-2-ylidene Moiety
Organometallics ( IF 2.5 ) Pub Date : 2018-01-17 00:00:00 , DOI: 10.1021/acs.organomet.7b00678 Karsten Klauke 1 , Irina Gruber 1 , Tim-Oliver Knedel 1 , Laura Schmolke 1 , Juri Barthel 2 , Hergen Breitzke 3 , Gerd Buntkowsky 3 , Christoph Janiak 1
Organometallics ( IF 2.5 ) Pub Date : 2018-01-17 00:00:00 , DOI: 10.1021/acs.organomet.7b00678 Karsten Klauke 1 , Irina Gruber 1 , Tim-Oliver Knedel 1 , Laura Schmolke 1 , Juri Barthel 2 , Hergen Breitzke 3 , Gerd Buntkowsky 3 , Christoph Janiak 1
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The selenoether-functionalized imidazolium salt N-[(phenylseleno)methylene)]-N′-methylimidazolium chloride (LH+Cl–) was transformed into the metal–carbene complexes [AgCl(L)], [AuCl(L)], [PdCl2(L)], and [PtCl2(L)] by the reaction with Ag2O and an additional transmetalation reaction of [AgCl(L)] with [(THT)AuCl], [(COD)PdCl2], and [(COD)PtCl2], respectively (THT = tetrahydrothiophene, COD = cyclooctadiene). The compound [AuI2Cl(L)] was prepared by oxidation of [AuCl(L)] with elemental iodine. The microwave-assisted decomposition of [PdCl2(L)] in the ionic liquid 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide ([BMIm]NTf2) or in propylene carbonate led to the formation of Pd17Se15 nanoparticles of 51 ± 17 or 26 ± 7 nm diameter, respectively. The decomposition of the platinum complex resulted in either small Pt clusters around 1 nm size from the ionic liquid suspension or Pt nanoparticles of 3 ± 1 nm diameter in propylene carbonate. High-resolution X-ray photoelectron spectroscopy (HR-XPS) and 13C cross-polarization magic-angle spinning (CP MAS) NMR indicated that the surface of Pt clusters and crystalline Pt nanoparticles is formed by an amorphous Pt(II)/Se shell and by carbene ligand residues.
中文翻译：
含硒醚官能化的咪唑-2-亚烷基部分的银，金，钯和铂N-杂环碳配合物
硒醚官能化的咪唑鎓盐N -[（（苯基硒代）亚甲基）]- N'-甲基咪唑鎓氯化物（LH + Cl –）被转化为金属-卡宾络合物[AgCl（L）]，[AuCl（L）]，[ PdCl 2（L）]和[PtCl 2（L）]，方法是与Ag 2 O反应，以及[AgCl（L）]与[（THT）AuCl]，[（COD）PdCl 2 ]的另外的金属转移反应，和[（COD）PtCl 2 ]分别（THT =四氢噻吩，COD =环辛二烯）。通过用元素碘氧化[AuCl（L）]来制备化合物[AuI 2 Cl（L）]。微波辅助分解[PdCl 2（L）]在离子液体1-丁基-3-甲基咪唑双（三氟甲基磺酰基）酰亚胺（[BMIm] NTf 2）或碳酸亚丙酯中导致形成51±17或26±7 nm的Pd 17 Se 15纳米粒子直径分别。铂络合物的分解导致离子液体悬浮液中约1 nm大小的小Pt簇或碳酸亚丙酯中直径3±1 nm的Pt纳米颗粒。高分辨率X射线光电子能谱（HR-XPS）和13 C交叉极化魔角旋转（CP MAS）NMR表明，Pt团簇和结晶Pt纳米颗粒的表面是由非晶Pt（II）/ Se形成的壳中并有卡宾配体残基。
更新日期：2018-01-18
中文翻译：
含硒醚官能化的咪唑-2-亚烷基部分的银，金，钯和铂N-杂环碳配合物
硒醚官能化的咪唑鎓盐N -[（（苯基硒代）亚甲基）]- N'-甲基咪唑鎓氯化物（LH + Cl –）被转化为金属-卡宾络合物[AgCl（L）]，[AuCl（L）]，[ PdCl 2（L）]和[PtCl 2（L）]，方法是与Ag 2 O反应，以及[AgCl（L）]与[（THT）AuCl]，[（COD）PdCl 2 ]的另外的金属转移反应，和[（COD）PtCl 2 ]分别（THT =四氢噻吩，COD =环辛二烯）。通过用元素碘氧化[AuCl（L）]来制备化合物[AuI 2 Cl（L）]。微波辅助分解[PdCl 2（L）]在离子液体1-丁基-3-甲基咪唑双（三氟甲基磺酰基）酰亚胺（[BMIm] NTf 2）或碳酸亚丙酯中导致形成51±17或26±7 nm的Pd 17 Se 15纳米粒子直径分别。铂络合物的分解导致离子液体悬浮液中约1 nm大小的小Pt簇或碳酸亚丙酯中直径3±1 nm的Pt纳米颗粒。高分辨率X射线光电子能谱（HR-XPS）和13 C交叉极化魔角旋转（CP MAS）NMR表明，Pt团簇和结晶Pt纳米颗粒的表面是由非晶Pt（II）/ Se形成的壳中并有卡宾配体残基。
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