Abstract

Two equivalents of sulphur and selenium on reaction with 1,1'-bis(diphenylphosphino)ferrocene (dppf) resulted compound of composition [Fe{C₅H₄P(E)Ph₂}₂] (E = S, Se). The latter resulted phosphine derivative on reaction with NiCl₂·6H₂O afforded an additive product [NiCl₂(dppfE₂)] (dppf = Fe{C₅H₄PPh₂}₂; E = S, Se) which on further treatment with another equivalent of [NiCl₂(dppfE₂)] followed by the addition of sodium tetraphenylborate yielded a binuclear complex [Ni₂(µ-Cl)₂(dppfE₂)](BPh₄)₂ (E = S, Se). All these complexes were characterized by elemental analysis, IR, ¹H and ³¹P{¹H} NMR spectroscopy. The molecular structure of [Fe{C₅H₄P(Se)Ph₂}₂] was determined by single crystal X-ray diffraction. The nanoparticles of complex [NiCl₂{Fe(C₅H₄P(S)Ph₂)₂}] (1a) and [NiCl₂{Fe(C₅H₄P(Se)Ph₂)₂}] (1b) was prepared through hydrothermal method. The resulting composites have further been applied for the catalytic oxidation of benzyl alcohol to aldehyde.

中文翻译：

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1,1'-双(二苯基硫属磷酰基)二茂铁类似物镍前体的合成及其催化氧化反应研究

摘要

两个当量的硫和硒与 1,1'-双(二苯基膦基)二茂铁 (dppf) 反应得到组成为 [Fe{C ₅ H ₄ P(E)Ph ₂ } ₂ ] (E = S, Se) 的化合物。后者在与 NiCl ₂ ·6H ₂ O 反应时产生膦衍生物，在进一步处理后得到添加剂产物 [NiCl ₂ (dppfE ₂ )] (dppf = Fe{C ₅ H ₄ PPh ₂ } ₂ ; E = S, Se)与另一当量的 [NiCl ₂ (dppfE ₂ )] 然后加入四苯基硼酸钠产生双核配合物 [Ni ₂(µ-Cl) ₂ (dppfE ₂ )](BPh ₄ ) ₂ (E = S, Se)。所有这些配合物均通过元素分析、IR、¹ H 和³¹ P{ ¹ H} NMR 光谱进行了表征。_{[Fe{C 5} H ₄ P(Se)Ph ₂ } ₂ ]的分子结构通过单晶X射线衍射确定。复合物[NiCl ₂ {Fe(C ₅ H ₄ P(S)Ph ₂ ) ₂ }] ( 1a ) 和[NiCl ₂ {Fe(C ₅ H ₄ P(Se)Ph)的纳米粒子₂ ) ₂ }] ( 1b ) 是通过水热法制备的。所得复合材料已进一步应用于苯甲醇催化氧化成醛。