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首页> 外文期刊>Organometallics >General Synthetic Route to Double-Butterfly Fe/S Cluster Complexes via Reactions of the Dianions {[(mu-CO)Fe_2(CO)_6]_2(mu-SZS-mu)}~(2-) with Electrophiles
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General Synthetic Route to Double-Butterfly Fe/S Cluster Complexes via Reactions of the Dianions {[(mu-CO)Fe_2(CO)_6]_2(mu-SZS-mu)}~(2-) with Electrophiles

机译：双价离子{[（mu-CO）Fe_2（CO）_6] _2（mu-SZS-mu）}〜（2-）与亲电试剂反应合成双蝴蝶Fe / S簇络合物的一般合成路线

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A simple and convenient route for the synthesis of linear and macrocyclic double-butterfly Fe/S cluster complexes has been developed, which involves a sequential reaction of Fe_3-(CO)_(12) with the dithiol HSZSH in the presence of Et_3N, followed by treatment of the intermediate [Et_3NH]~+ salts of dianions {[(mu-CO)Fe_2(CO)_6]_2(mu-SZS-mu)}~(2-) (4) with electrophiles. For example, treatment of the [Et_3NH]~+ salts of dianions 4 with allyl bromide and PhSBr produces the linear complexes [(mu-CH_2=CHCH_2)Fe_2(CO)_6]_2(mu-SZS-mu) (5a, Z = (CH_2)_4; 5b, Z =CH_2(CH_2OCH_2)_2CH_2; 5c, Z=CH_2(CH_2OCH_2)_3CH_2) and [(mu-PhS)Fe_2(CO)_6]_2(mu-SZS-mu) (6a, Z=CH_2(CH_2OCH_2)_2CH_2; 6b, Z=CH_2(CH_2OCH_2)_3CH_2), whereas treatment with S_2C1_2 and C1SZSC1 yields the macrocyclic complexes [Fe_2(CO)_6]_2(mu-S-S-mu)(mu-SZS-mu) (7a, Z = CH_2(CH_2-OCH_2)_2CH_2; 7b, Z=CH_2(CH_2OCH_2)_3CH_2) and [Fe-2(CO)_6]_2(mu-SZS-mu)_2 (8a, Z=CH_2(CH_2OCH_2)_2-CH_2; 8b, Z = CH_2(CH_2OCH_2)_3CH_2), respectively. In addition, while the [Et_3NH]~+ salts of dianions 4 react in situ with PhNCS and SCN(CH_2)_4NCS to give the linear complexes [(mu-PhNHC=S)Fe_2(CO)_6]_2(mu-SZS-mu) (9a, Z=CH_2CH_2OCH_2CH_2; 9b, Z=CH-2(CH_2OCH_2)_2CH_2; 9c, Z = CH_2(CH_2OCH_2)_3CH_2) and macrocyclic complexes [Fe_2(CO)_6]_2 [mu-S=CNH(CH_2)_4NHC= S-mu](mu-SZS-mu) (10a, Z = (CH_2)_4; l0b, Z = CH_2(CH_2OCH_2)_2CH_2), the in situ reactions with PhC^CPh and PhCident toCH afford the linear complexes [(mu-sigma,pi-PhCH=CPh)Fe_2(CO)_6]_2(mu-SZS-mu) (11a, Z=CH_2(CH_2OCH_2)_2CH_2; 11b, Z=CH_2(CH_2OCH_2)_3CH_2) and [(mu-sigma,pi-PhCH=CH)-Fe_2(CO)_6]_2(mu-SZS-mu) (12a, Z = (CH_2)_4; 12b, Z=CH_2(CH_2OCH_2)_2CH_2; 12c, Z =CH_2(CH_2-OCH_2)_3CH_2). The possible pathways for production of these linear and macrocyclic cluster complexes are suggested, and their structures have been characterized by elemental analysis and IR and ~1H NMR spectroscopy, as well as for 5a, 7a, 8a, and 12a by X-ray diffraction analysis.
机译：已经开发了一种简单且方便的合成线性和大环双蝶Fe / S簇络合物的方法，该方法涉及在Et_3N存在下Fe_3-（CO）_（12）与二硫醇HSZSH的顺序反应，然后用亲电子试剂处理二价阴离子{[（mu-CO）Fe_2（CO）_6] _2（mu-SZS-mu）}〜（2-）的中间体[Et_3NH]〜+盐。例如，用烯丙基溴和PhSBr处理二价阴离子4的[Et_3NH]〜+盐可生成线性络合物[（mu-CH_2 = CHCH_2）Fe_2（CO）_6] _2（mu-SZS-mu）（5a，Z =（CH_2）_4; 5b，Z = CH_2（CH_2OCH_2）_2CH_2; 5c，Z = CH_2（CH_2OCH_2）_3CH_2）和[（mu-PhS）Fe_2（CO）_6] _2（mu-SZS-mu）（6a， Z = CH_2（CH_2OCH_2）_2CH_2; 6b，Z = CH_2（CH_2OCH_2）_3CH_2），而用S_2C1_2和C1SZSC1处理可得到大环配合物[Fe_2（CO）_6] _2（mu-SS-mu）（mu-SZS-mu ）（7a，Z = CH_2（CH_2-OCH_2）_2CH_2; 7b，Z = CH_2（CH_2OCH_2）_3CH_2）和[Fe-2（CO）_6] _2（mu-SZS-mu）_2（8a，Z = CH_2（ CH_2OCH_2）_2-CH_2; 8b，Z = CH_2（CH_2OCH_2）_3CH_2）。此外，当二价阴离子的[Et_3NH]〜+盐与PhNCS和SCN（CH_2）_4NCS原位反应以生成线性络合物[（mu-PhNHC = S）Fe_2（CO）_6] _2（mu-SZS- mu）（9a，Z = CH_2CH_2OCH_2CH_2; 9b，Z = CH-2（CH_2OCH_2）_2CH_2; 9c，Z = CH_2（CH_2OCH_2）_3CH_2）和大环配合物[Fe_2（CO）_6] _2 [mu-S = CNH（CH_2） ）_4NHC ＝S-μ（μ-SZS-μ）（10a，Z ＝（CH_2）_4; 10b，Z ＝ CH_2（CH_2OCH_2）_2CH_2），与PhC ^ CPh和PhCidenttoCH的原位反应得到线性络合物[（mu-sigma，pi-PhCH = CPh）Fe_2（CO）_6] _2（mu-SZS-mu）（11a，Z = CH_2（CH_2OCH_2）_2CH_2; 11b，Z = CH_2（CH_2OCH_2）_3CH_2）和[[ mu-sigma，pi-PhCH = CH）-Fe_2（CO）_6] _2（mu-SZS-mu）（12a，Z =（CH_2）_4; 12b，Z = CH_2（CH_2OCH_2）_2CH_2; 12c，Z = CH_2 （CH_2-OCH_2）_3CH_2）。提出了生产这些线性和大环簇复合物的可能途径，并通过元素分析，IR和〜1H NMR光谱以及通过X射线衍射分析的5a，7a，8a和12a表征了其结构。 。

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