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One pot synthesis of chalcogenolato and phosphino bridged/ligated Mn(I)- and Re(I)-based mono- and dinuclear metallacycles
Journal of Organometallic Chemistry ( IF 2.3 ) Pub Date : 2020-07-30 , DOI: 10.1016/j.jorganchem.2020.121463
Udit Kumar , Sunipa Goswami , Shaikh M. Mobin , Bala. Manimaran

A series of chalcogenolato and phosphino bridged/ligated Mn(I)- and Re(I)-based mononuclear and dinuclear metallacycles were synthesized in a single step under one pot reaction condition from rudimentary starting materials. Metallacycles 14 were synthesized by the reaction of diphenyl dichalcogenide (S/Se) and 1,4-bis(diphenylphosphino)butane (dppb) with dimetal decacarbonyl (Mn/Re). Two different shapes of metallacyclic compounds were synthesized using similar kind of metal precursors with different chalcogenolate ligands. Compounds 1 and 2 adapted dinuclear framework of general formula [{(CO)3M(μ-SC6H5)2M(CO)3}(μ-dppb)] (M = Mn/Re) when diphenyl disulfide was reacted with M2(CO)10 (Mn/Re) and dppb, whereas compounds 3 and 4 attained mononuclear structure of general formula [(CO)3M(SeC6H5)(η2-dppb)] (M = Mn/Re) while diphenyl diselenide was treated with M2(CO)10 (Mn/Re) and dppb. Compounds 14 were characterized using UV−Vis, IR and NMR spectroscopic techniques and elemental analysis. The molecular masses of metallacycles 14 were evaluated by electrospray ionization-mass spectrometry (ESI-MS). Solid-state structural elucidation of compound 3 was carried out using single-crystal X-ray diffraction methods.



中文翻译:

一锅合成硫属元素素和膦基桥接/连接的Mn(I)和Re(I)基单核和双核金属环。

在单一反应条件下,从基础原料中一步一步合成了一系列硫属元素基和膦基桥连/连接的Mn(I)和Re(I)基单核和双核金属环。Metallacycles 1 - 4通过二苯二硫属化物(S / SE)和1,4-双(二苯基膦基)丁烷(DPPB)与双金属decacarbonyl(锰/ RE)的反应合成。使用具有不同硫属元素酸酯配体的相似种类的金属前体合成了两种不同形状的金属环化合物。化合物12适应了通式[{(CO)3 M(μ- SC 6 H 52当二苯基二硫化物与M 2(CO)10(Mn / Re)和dppb反应时,M(CO)3 }(μ- dppb)](M = Mn / Re),而化合物34获得通式的单核结构[(CO)3 M(SEC 6 ħ 5)(η 2 -DPPB)](M =锰/ RE),而二苯基二硒化物是具有M处理2(CO)10(锰/ Re)和DPPB。化合物1 - 4通过UV-Vis,IR和NMR光谱技术和元素分析进行表征。metallacycles的分子量1 - 4用电喷雾电离质谱法(ESI-MS)评价。使用单晶X射线衍射法进行化合物3的固态结构阐明。

更新日期:2020-08-11
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