Manganese(II), nickel(II), and palladium(II) complexes of a terpyridine-Like ligand containing a sulfur linkage, and an analogous NCN pincer palladium(II) complex: Synthesis, characterization, and Pd-Catalyzed reactions

Hirotsu M.; Tsukahara Y.; Kinoshita I.

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Manganese(II), nickel(II), and palladium(II) complexes of a terpyridine-Like ligand containing a sulfur linkage, and an analogous NCN pincer palladium(II) complex: Synthesis, characterization, and Pd-Catalyzed reactions

机译：含硫键的联吡啶样配体的锰（II），镍（II）和钯（II）配合物以及类似的NCN钳合钯（II）配合物：合成，表征和Pd催化的反应

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Coordination properties of new polypyridines containing a single sulfur linkage, 6-(2″-pyridylthio)-2, 2′-bipyridine (L1) and 1-(2′-pyridyl)-3-(2″-pyridylthio)benzene (HL2), are described. The manganese(II) and nickel(II) complexes of the terpyridine-like ligand L1, [MnCl_2(L1)] (1), [NiCl(μ-Cl)(L1)]_2 (2), and [Ni(L1)_2](SbF_6)_2 (3), were prepared and characterized by UV-vis spectroscopy and X-ray crystallography. The palladium(II) complex [PdCl(L1)]Cl (4) was synthesized from L1 and Li _2[PdCl_1] at room temperature, while the corresponding NCN pincer complex of L2, [PdCl(L2)] (5), was synthesized in DMSO at 150 °C by cyclopalladation of the ligand precursor HL2. The crystal structures of 4 and 5 revealed similar coordination geometries around Pd except for the longer Pd-Cl distance in 5, which is induced by the strong trans influence of the Pd-C bonding. The NMR spectra of 4 showed partial dissociation of L1 in DMSO-d _6, which was not observed for L2 in 5. Catalytic activities of 4 and 5 for the Mizoroki-Heck reaction were investigated, and the lower activity of 5 can be related to the strong σ-donating character of L2.

机译：含单硫键的新聚吡啶，6-（2″-吡啶硫基）-2、2′-联吡啶（L1）和1-（2′-吡啶基）-3-（2″-吡啶硫基）苯（HL2）的配位性能），进行了说明。吡啶类配体L1，[MnCl_2（L1）]（1），[NiCl（μ-Cl）（L1）] _ 2（2）和[Ni（L1）的锰（II）和镍（II）配合物）_2]（SbF_6）_2（3）的制备，并通过紫外可见光谱和X射线晶体学进行表征。在室温下由L1和Li _2 [PdCl_1]合成钯（II）络合物[PdCl（L1）] Cl（4），而相应的L2的NCN钳形络合物[PdCl（L2）]（5）为在DMSO中于150°C下通过配体前体HL2的环钯合成合成。 4和5的晶体结构在Pd周围显示出相似的配位几何结构，除了5中较长的Pd-Cl距离外，这是由Pd-C键的强反式影响引起的。 4的NMR光谱显示DMSO-d _6中L1的部分解离，在5中未观察到L2。研究了4和5对Mizoroki-Heck反应的催化活性，而较低的5活性可能与L2的强σ捐赠特征。

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《Bulletin of the Chemical Society of Japan》 |2010年第9期|共9页
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Hirotsu M.; Tsukahara Y.; Kinoshita I.;
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1. Manganese(II), nickel(II), and palladium(II) complexes of a terpyridine-Like ligand containing a sulfur linkage, and an analogous NCN pincer palladium(II) complex: Synthesis, characterization, and Pd-Catalyzed reactions [J] . Hirotsu M., Tsukahara Y., Kinoshita I. Bulletin of the Chemical Society of Japan . 2010,第9期

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Manganese(II), nickel(II), and palladium(II) complexes of a terpyridine-Like ligand containing a sulfur linkage, and an analogous NCN pincer palladium(II) complex: Synthesis, characterization, and Pd-Catalyzed reactions

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