与[FeFe]氢化酶活性中心相关的新型铁硫和铁硒簇合物的设计合成
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摘要
由于[FeFe]氢化酶是一种能高效地催化质子还原为氢气及其可逆反应的生物酶,因此,[FeFe]氢化酶仿生化学模拟研究在理论和实际应用方面都具有极其重要的意义。为了进一步丰富和发展[FeFe]氢化酶仿生化学以及Fe/E(E=S,Se)原子簇的合成化学,本文开展了对[FeFe]氢化酶活性中心结构的设计合成研究工作。本文设计合成了一系列新型[FeFe]氢化酶活性中心模型物和蝶状Fe/E(E=S, Se)簇合物,并对这些化合物进行了结构、性质和功能研究,取得了以下创新性成果：
1.本论文共合成了28个新化合物,其中包括19个[FeFe]氢化酶活性中心模型物以及9个结构新颖的蝶状Fe/S和Fe/Se簇合物。这些新化合物均经元素分析、1H NMR、IR的表征,部分化合物还用13C NMR、31P NMR、77Se NMR、质谱、循环伏安(CV)等手段对其结构、性质及催化产氢的效果进行了表征,并用X-射线衍射技术测定了其中15个化合物的单晶结构。
2.首次合成了含双羟甲基官能团的PDT型氢化酶模型物[(μ-SCH2)2C(CH2OH)2]Fe2(CO)6(1),并对其官能团进行了衍生化,得到了一系列结构新颖的PDT型氢化酶模型物[(μ一SCH2)2C(CH2OH)(CH2OCOCH3)]Fe2(CO)6 (2).[(μ-SCH2)2C(CH2OCOCH3)2]Fe2(CO)6(3)、[(μ一SCH2)2C(CH2OCOC5H4N-4)2] Fe2(CO)6(4)、[(μ-SCH2)2C(CH2OCOC5H4N-3)2]Fe2(CO)6(5)、[(μ-SCH2)2C(CH2O COC6H4PPh2-2)2]Fe2(CO)6(6)、[(μ-SCH2)2C(CH2OCOC6H4PPh2-3)2]Fe2(CO)6(7)、[(μ-SCH2)2C(CH2OH)(CH2OCOC6H4PPh2-3)]2[Fe2(CO)6]2(7a)、[(μ-SCH2)2C(CH2 OH)(CH2OCOC6H4PPh2-3)]Fe2(CO)6(8)、[(μ-SCH2)2C(CH2OCOC6H4PPh2-4)2] Fe2(CO)6(9)和[(μ-SCH2)2C(CH2OCOCH2PPh2)2]Fe2(CO)6(10)。它们均经元素分析、IR和1H NMR的表征,并用31P NMR对其中的模型物6-10进行了表征,还测定了模型物1、2、3、5和7a的单晶结构；用循环伏安法研究了母体化合物1的电化学性质,研究表明在以弱酸醋酸作为质子源时,1能有效地电化学催化质子还原为氢气,并提出了它的催化机理。
3.首次合成了含有丝氨酸结构单元的ADT型氢化酶模型物{μ-SCH2N[CH(CH2OH)(CO2CH3)]CH2S-μ}[Fe2(CO)6](A),并以A为母体化合物进行官能团转化,得到了模型物{μ-SCH2N[CH(CH2OPPh2)(CO2CH3)]CH2S-μ}[Fe2 (CO)5](1)、{μ-SCH2N[CH(CH2OTs)(CO2CH3)]CH2S-μ}[Fe2(CO)6](2)、{μ-SCH2N [CH(CH2OMs)(CO2CH3)]CH2S-μ}[Fe2(CO)6](3)、{μ-SCH2N[C(CH2)(CO2CH3)]CH2 S-μ}[Fe2(CO)6](4)。用元素分析、IR、1H NMR对它们进行了表征,利用13C NMR对其中的模型物4进行了表征,并测定了模型物2和4的单晶结构。
此外,利用氮杂丙撑桥ADT型模型物[(μ-SCH2)2NCH2CH2SC(O)CH3]Fe2(CO)6与立方烷簇合物[Et4N]2[Fe4S4(TriS)(t-BuS)]进行酯交换及脱羰基反应,合成了一个具有[FeFe]氢化酶活性中心整体骨架结构的模型物[Et4N]2[Fe4S4(TriS)]{Fe2N(CH2S-μ)2(CH2CH2S)(CO)5}(5),通过元素分析、IR、1H NMR、循环伏安等手段对其进行了表征。
我们还首次合成了含双羟甲基官能团的ADT型氢化酶模型物{μ-SCH2N[C(CH2OH)2CH3]CH2S-μ}[Fe2(CO)6](6),并对其双羟基官能团进行衍生化,得到了模型物{μ-SCH2N[C(CH2OCOCH3)2CH3]CH2S-μ}Fe2(CO)6(7)。用元素分析、IR、1H NMR对它们进行了表征,并测定了模型物7的单晶结构。
4.首次利用含Mo/W金属的亲电试剂(C5H4COOCH3)Mo(CO)3I和(C5H4COCH3)W(CO)3I分别与相应的Fe/S簇阴离子络盐(μ-SR) (μ-SCS-)Fe2(CO)6(Et3NH)(B)、(μ-S-CH2CH2OCH2CH2-S-μ)[(μ-SCS-)Fe2(CO)6]2 (Et3NH)2(D)和(μ-SEt)(μ4-S))(μ-S-)[Fe2(CO)6]2(Et3NH)(E)反应,生成了7个新型蝶状Fe/S簇合物[μ-S=C-S-Mo(CO)3(C5H4COOCH3)](μ-SEt)[Fe2(CO)6](1a)、[μ-S=C-S-Mo(CO)3(C5H4COOCH3)](μ-S-tBu)[Fe2(CO)6](1b)、[μ-S=C-S-W(CO)3 (C5H4COCH3)](μ-SEt)[Fe2(CO)6](2a)、[μ-S=C-S-W(CO)3(C5H4COCH3)](μ-S-tBu) [Fe2(CO)6](2b)、[(μ-S=C-S-Mo(CO)3(C5H4COOCH3)Fe2(CO)6]2(μ-SCH2CH2OCH2 CH2S-μ)(3)、[(μ-S=C-S-W(CO)3(C5H4COCH3)Fe2(CO)6]2(μ-SCH2CH2OCH2CH2S-μ)(4)和{(μ-SEt)(μ4-S)[Fe2(CO)6]2]}[μ-S-W(CO)3(C5H4COCH3)](5),通过1H NMR、IR和元素分析对它们进行了表征,并对化合物1a和2a的单晶进行了X-射线衍射分析,进一步证实了这类化合物的结构和反应特点。
5.首次合成了蝶状Fe/Se簇合物(μ-SeEt)(μ-SePh2P-μ)Fe2(CO)6(1)和(μ-SeEt){μ-Se[(CH3)2CH]2P-μ)Fe2(CO)6(2),用元素分析、IR、1H NMR、31P NMR 77Se NMR对它们进行了表征,并测定了模型物1的单晶结构。
此外,用单晶X-射线衍射法确证了我们实验室其他同学合成的4个新颖的单蝶状铁硫和铁硒簇合物。
The [FeFe]-hydrogenases are highly efficient enzymes that catalyze the reduction of proton to hydrogen and the oxidation of hydrogen in microorganisms, so studies on biomimetic chemistry of [FeFe]-hydrogenases have important theoretical significance and practical applications. In order to develop biomimetic chemistry of [FeFe]-hydrogenases and synthetic chemistry of metal clusters, we initiated a study concerning the synthesis, structure and properties of a series of new butterfly Fe/E(E =S, Se) cluster compounds related to the [FeFe]-hydrogenase active site. The main results described in this thesis are as follows:
1. A total of 28 new compounds have been successfully synthesized, including 19 [FeFe]-hydrogenase active site model compounds and 9 novel butterfly Fe/E(E= S, Se) cluster compounds. The structures of these new compounds were fully characterized by elemental analysis, IR, and 1H NMR, as well as for some of them by 13C NMR,31P NMR,77Se NMR, MS and cyclic voltammetry. The crystal structures of 15 compounds were determined by X-ray diffraction method.
2. The parent PDT-type model complex with a bis(hydroxymethyl) functionality [(μ-SCH2)2C(CH2OH)2]Fe2(CO)6 (1) was first prepared, and a series of its functional derivatives [(μ-SCH2)2C(CH2OH)(CH2OCOCH3)]Fe2(CO)6(2),[(μ-SCH2)2C(CH2O COCH3)2]Fe2(CO)6 (3), [(μ-SCH2)2C(CH2OCOC5H4N-4)2]Fe2(CO)6 (4), [(μ-SCH2)2C (CH2OCOC5H4N-3)2]Fe2(CO)6(5), [(μ-SCH2)2C(CH2OCOC6H4PPh2-2)2]Fe2(CO)6(6), [(μ-SCH2)2C(CH2OCOC6H4PPh2-3)2]Fe2(CO)6(7), [(μ-SCH2)2C(CH2OH)(CH2OCO C6H4PPh2-3)]2[Fe2(CO)6]2(7a), [(μ-SCH2)2C(CH2OH)(CH2OCOC6H4PPh2-3)]Fe2 (CO)6(8), [(μ-SCH2)2C(CH2OCOC6H4PPh2-4)2]Fe2(CO)6(9) and [(μ-SCH2)2C(CH2O COCH2PPh2)2]Fe2(CO)6(10) were prepared. All of these new compounds were fully characterized by elemental analysis, IR and 1H NMR spectroscopies, as well as for 6-10 by 31P NMR and the molecular structures of 1,2,3,5 and 7a were confirmed by X-ray diffraction techniques. The electrochemical study indicated that model compound 1 can catalyze reduction of acetic acid protons to H2 under CV conditions. The mechanism for this electrocatalytic process is proposed.
3. The ADT-type model complex containing serine framework{μ-SCH2N[CH (CH2OH)(CO2CH3)]CH2S-μ}[Fe2(CO)6] (A) was first prepared, and its four derivatives{μ-SCH2N[CH(CH2OPPh2)(CO2CH3)]CH2S-μ}[Fe2(CO)5] (1),{μ-SCH2N [CH(CH2OTs)(CO2CH3)]CH2S-μ}[Fe2(CO)6](2),{μ-SCH2N[CH(CH2OMs)(CO2CH3 )]CH2S-μ}[Fe2(CO)6] (3),{μ-SCH2N[C(CH2)(CO2CH3)]CH2S-μ}[Fe2(CO)6] (4) were prepared through its functional transformation reactions. These new compounds were characterized by elemental analysis, IR and 1H NMR spectroscopies, as well as for 4 by 13C NMR and the molecular structures of 2 and 4 were confirmed by X-ray diffraction techniques.
In addition, the model compound [Et4N]2[Fe4S4(TriS)]{Fe2N(CH2S-μ)2(CH2CH2S) (CO)5}(5), which contains the whole skeletal structure of the active site of [FeFe]-hydrogenases was synthesized through ester exchange and decarbonylation reactions of [(μ-SCH2)2NCH2CH2SC(O)CH3]Fe2(CO)6 with the cubane cluster [Et4N]2[Fe4S4(TriS)(t-BuS)]. This new compound was characterized by elemental analysis, IR,1H NMR and cyclic voltammetry.
The new parent ADT-type model complex {μ-SCH2N[C(CH2OH)2CH3]CH2S-μ} [Fe2(CO)6](6) was also prepared, and its derivative{μ-SCH2N[C(CH2OCOCH3)2CH3] CH2S-μ}Fe2(CO)6 (7) was synthesized by reaction of 6 with CH2(COOH)2. Compounds 6 and 7 were characterized by elemental analysis, IR and 1H NMR spectroscopies and the structure of 7 was confirmed by X-ray diffraction technique.
4. Seven new butterfly Fe/S cluster complexes [μ-S=C-S-Mo(CO)3(C5H4COO CH3)](μ-SEt)[Fe2(CO)6](la), [μ-S=C-S-Mo(CO)3(C5H4COOCH3)](μ-S-tBu)[Fe2 (CO)6] (lb), [μ-S=C-S-W(CO)3(C5H4COCH3)](μ-SEt)[Fe2(CO)6] (2a),[μ-S=C-S-W (CO)3(C5H4COCH3)](μ-S-tBu)[Fe2(CO)6](2b), [(μ-S=C-S-Mo(CO)3(C5H4COOCH3) Fe2(CO)6]2(μ-SCH2CH2OCH2CH2S-μ)(3), [(μ-S=C-S-W(CO)3(C5H4COCH3)Fe2 (CO)6]2(μ-SCH2CH2OCH2CH2S-μ)(4)and{(μ-SEt)(μ4-S)[Fe2(CO)6]2]}[μ-S-W(CO)3 (C5H4COCH3)] (5) were produced by reactions of electrophiles (C5H4COOCH3)Mo (CO)3I or (C5H4COCH3)W(CO)3I with the corresponding anionic salts (μ-SR)(μ-SCS")Fe2(CO)6(Et3NH)(B),(μ-S-CH2CH2OCH2CH2-S-μ)[(μ-SCS-)Fe2 (CO)6]2(Et3NH)2(D) and (μ-SEt)(μ4-S))(μ-S-)[Fe2(CO)6]2(Et3NH) (E). These products were characterized by elemental analysis, IR and 1H NMR. The structures of la and 2a were confirmed by X-ray diffraction techniques.
5. Two new Fe/Se cluster complexes (μ-SeEt)(μ-SePh2P-μ)Fe2(CO)6 (1) and (μ-SeEt){μ-Se[(CH3)2CH]2P-μ)Fe2(CO)6 (2) were first prepared, and they were characterized by elemental analysis, IR,1H NMR,31P NMR and 77Se NMR spectroscopies and the structure of 1 was confirmed by X-ray diffraction technique.
In addition, the molecular structures of four compounds prepared by others in our group were confirmed by X-ray diffraction techniques.
1.本论文共合成了28个新化合物,其中包括19个[FeFe]氢化酶活性中心模型物以及9个结构新颖的蝶状Fe/S和Fe/Se簇合物。这些新化合物均经元素分析、1H NMR、IR的表征,部分化合物还用13C NMR、31P NMR、77Se NMR、质谱、循环伏安(CV)等手段对其结构、性质及催化产氢的效果进行了表征,并用X-射线衍射技术测定了其中15个化合物的单晶结构。
2.首次合成了含双羟甲基官能团的PDT型氢化酶模型物[(μ-SCH2)2C(CH2OH)2]Fe2(CO)6(1),并对其官能团进行了衍生化,得到了一系列结构新颖的PDT型氢化酶模型物[(μ一SCH2)2C(CH2OH)(CH2OCOCH3)]Fe2(CO)6 (2).[(μ-SCH2)2C(CH2OCOCH3)2]Fe2(CO)6(3)、[(μ一SCH2)2C(CH2OCOC5H4N-4)2] Fe2(CO)6(4)、[(μ-SCH2)2C(CH2OCOC5H4N-3)2]Fe2(CO)6(5)、[(μ-SCH2)2C(CH2O COC6H4PPh2-2)2]Fe2(CO)6(6)、[(μ-SCH2)2C(CH2OCOC6H4PPh2-3)2]Fe2(CO)6(7)、[(μ-SCH2)2C(CH2OH)(CH2OCOC6H4PPh2-3)]2[Fe2(CO)6]2(7a)、[(μ-SCH2)2C(CH2 OH)(CH2OCOC6H4PPh2-3)]Fe2(CO)6(8)、[(μ-SCH2)2C(CH2OCOC6H4PPh2-4)2] Fe2(CO)6(9)和[(μ-SCH2)2C(CH2OCOCH2PPh2)2]Fe2(CO)6(10)。它们均经元素分析、IR和1H NMR的表征,并用31P NMR对其中的模型物6-10进行了表征,还测定了模型物1、2、3、5和7a的单晶结构；用循环伏安法研究了母体化合物1的电化学性质,研究表明在以弱酸醋酸作为质子源时,1能有效地电化学催化质子还原为氢气,并提出了它的催化机理。
3.首次合成了含有丝氨酸结构单元的ADT型氢化酶模型物{μ-SCH2N[CH(CH2OH)(CO2CH3)]CH2S-μ}[Fe2(CO)6](A),并以A为母体化合物进行官能团转化,得到了模型物{μ-SCH2N[CH(CH2OPPh2)(CO2CH3)]CH2S-μ}[Fe2 (CO)5](1)、{μ-SCH2N[CH(CH2OTs)(CO2CH3)]CH2S-μ}[Fe2(CO)6](2)、{μ-SCH2N [CH(CH2OMs)(CO2CH3)]CH2S-μ}[Fe2(CO)6](3)、{μ-SCH2N[C(CH2)(CO2CH3)]CH2 S-μ}[Fe2(CO)6](4)。用元素分析、IR、1H NMR对它们进行了表征,利用13C NMR对其中的模型物4进行了表征,并测定了模型物2和4的单晶结构。
此外,利用氮杂丙撑桥ADT型模型物[(μ-SCH2)2NCH2CH2SC(O)CH3]Fe2(CO)6与立方烷簇合物[Et4N]2[Fe4S4(TriS)(t-BuS)]进行酯交换及脱羰基反应,合成了一个具有[FeFe]氢化酶活性中心整体骨架结构的模型物[Et4N]2[Fe4S4(TriS)]{Fe2N(CH2S-μ)2(CH2CH2S)(CO)5}(5),通过元素分析、IR、1H NMR、循环伏安等手段对其进行了表征。
我们还首次合成了含双羟甲基官能团的ADT型氢化酶模型物{μ-SCH2N[C(CH2OH)2CH3]CH2S-μ}[Fe2(CO)6](6),并对其双羟基官能团进行衍生化,得到了模型物{μ-SCH2N[C(CH2OCOCH3)2CH3]CH2S-μ}Fe2(CO)6(7)。用元素分析、IR、1H NMR对它们进行了表征,并测定了模型物7的单晶结构。
4.首次利用含Mo/W金属的亲电试剂(C5H4COOCH3)Mo(CO)3I和(C5H4COCH3)W(CO)3I分别与相应的Fe/S簇阴离子络盐(μ-SR) (μ-SCS-)Fe2(CO)6(Et3NH)(B)、(μ-S-CH2CH2OCH2CH2-S-μ)[(μ-SCS-)Fe2(CO)6]2 (Et3NH)2(D)和(μ-SEt)(μ4-S))(μ-S-)[Fe2(CO)6]2(Et3NH)(E)反应,生成了7个新型蝶状Fe/S簇合物[μ-S=C-S-Mo(CO)3(C5H4COOCH3)](μ-SEt)[Fe2(CO)6](1a)、[μ-S=C-S-Mo(CO)3(C5H4COOCH3)](μ-S-tBu)[Fe2(CO)6](1b)、[μ-S=C-S-W(CO)3 (C5H4COCH3)](μ-SEt)[Fe2(CO)6](2a)、[μ-S=C-S-W(CO)3(C5H4COCH3)](μ-S-tBu) [Fe2(CO)6](2b)、[(μ-S=C-S-Mo(CO)3(C5H4COOCH3)Fe2(CO)6]2(μ-SCH2CH2OCH2 CH2S-μ)(3)、[(μ-S=C-S-W(CO)3(C5H4COCH3)Fe2(CO)6]2(μ-SCH2CH2OCH2CH2S-μ)(4)和{(μ-SEt)(μ4-S)[Fe2(CO)6]2]}[μ-S-W(CO)3(C5H4COCH3)](5),通过1H NMR、IR和元素分析对它们进行了表征,并对化合物1a和2a的单晶进行了X-射线衍射分析,进一步证实了这类化合物的结构和反应特点。
5.首次合成了蝶状Fe/Se簇合物(μ-SeEt)(μ-SePh2P-μ)Fe2(CO)6(1)和(μ-SeEt){μ-Se[(CH3)2CH]2P-μ)Fe2(CO)6(2),用元素分析、IR、1H NMR、31P NMR 77Se NMR对它们进行了表征,并测定了模型物1的单晶结构。
此外,用单晶X-射线衍射法确证了我们实验室其他同学合成的4个新颖的单蝶状铁硫和铁硒簇合物。
The [FeFe]-hydrogenases are highly efficient enzymes that catalyze the reduction of proton to hydrogen and the oxidation of hydrogen in microorganisms, so studies on biomimetic chemistry of [FeFe]-hydrogenases have important theoretical significance and practical applications. In order to develop biomimetic chemistry of [FeFe]-hydrogenases and synthetic chemistry of metal clusters, we initiated a study concerning the synthesis, structure and properties of a series of new butterfly Fe/E(E =S, Se) cluster compounds related to the [FeFe]-hydrogenase active site. The main results described in this thesis are as follows:
1. A total of 28 new compounds have been successfully synthesized, including 19 [FeFe]-hydrogenase active site model compounds and 9 novel butterfly Fe/E(E= S, Se) cluster compounds. The structures of these new compounds were fully characterized by elemental analysis, IR, and 1H NMR, as well as for some of them by 13C NMR,31P NMR,77Se NMR, MS and cyclic voltammetry. The crystal structures of 15 compounds were determined by X-ray diffraction method.
2. The parent PDT-type model complex with a bis(hydroxymethyl) functionality [(μ-SCH2)2C(CH2OH)2]Fe2(CO)6 (1) was first prepared, and a series of its functional derivatives [(μ-SCH2)2C(CH2OH)(CH2OCOCH3)]Fe2(CO)6(2),[(μ-SCH2)2C(CH2O COCH3)2]Fe2(CO)6 (3), [(μ-SCH2)2C(CH2OCOC5H4N-4)2]Fe2(CO)6 (4), [(μ-SCH2)2C (CH2OCOC5H4N-3)2]Fe2(CO)6(5), [(μ-SCH2)2C(CH2OCOC6H4PPh2-2)2]Fe2(CO)6(6), [(μ-SCH2)2C(CH2OCOC6H4PPh2-3)2]Fe2(CO)6(7), [(μ-SCH2)2C(CH2OH)(CH2OCO C6H4PPh2-3)]2[Fe2(CO)6]2(7a), [(μ-SCH2)2C(CH2OH)(CH2OCOC6H4PPh2-3)]Fe2 (CO)6(8), [(μ-SCH2)2C(CH2OCOC6H4PPh2-4)2]Fe2(CO)6(9) and [(μ-SCH2)2C(CH2O COCH2PPh2)2]Fe2(CO)6(10) were prepared. All of these new compounds were fully characterized by elemental analysis, IR and 1H NMR spectroscopies, as well as for 6-10 by 31P NMR and the molecular structures of 1,2,3,5 and 7a were confirmed by X-ray diffraction techniques. The electrochemical study indicated that model compound 1 can catalyze reduction of acetic acid protons to H2 under CV conditions. The mechanism for this electrocatalytic process is proposed.
3. The ADT-type model complex containing serine framework{μ-SCH2N[CH (CH2OH)(CO2CH3)]CH2S-μ}[Fe2(CO)6] (A) was first prepared, and its four derivatives{μ-SCH2N[CH(CH2OPPh2)(CO2CH3)]CH2S-μ}[Fe2(CO)5] (1),{μ-SCH2N [CH(CH2OTs)(CO2CH3)]CH2S-μ}[Fe2(CO)6](2),{μ-SCH2N[CH(CH2OMs)(CO2CH3 )]CH2S-μ}[Fe2(CO)6] (3),{μ-SCH2N[C(CH2)(CO2CH3)]CH2S-μ}[Fe2(CO)6] (4) were prepared through its functional transformation reactions. These new compounds were characterized by elemental analysis, IR and 1H NMR spectroscopies, as well as for 4 by 13C NMR and the molecular structures of 2 and 4 were confirmed by X-ray diffraction techniques.
In addition, the model compound [Et4N]2[Fe4S4(TriS)]{Fe2N(CH2S-μ)2(CH2CH2S) (CO)5}(5), which contains the whole skeletal structure of the active site of [FeFe]-hydrogenases was synthesized through ester exchange and decarbonylation reactions of [(μ-SCH2)2NCH2CH2SC(O)CH3]Fe2(CO)6 with the cubane cluster [Et4N]2[Fe4S4(TriS)(t-BuS)]. This new compound was characterized by elemental analysis, IR,1H NMR and cyclic voltammetry.
The new parent ADT-type model complex {μ-SCH2N[C(CH2OH)2CH3]CH2S-μ} [Fe2(CO)6](6) was also prepared, and its derivative{μ-SCH2N[C(CH2OCOCH3)2CH3] CH2S-μ}Fe2(CO)6 (7) was synthesized by reaction of 6 with CH2(COOH)2. Compounds 6 and 7 were characterized by elemental analysis, IR and 1H NMR spectroscopies and the structure of 7 was confirmed by X-ray diffraction technique.
4. Seven new butterfly Fe/S cluster complexes [μ-S=C-S-Mo(CO)3(C5H4COO CH3)](μ-SEt)[Fe2(CO)6](la), [μ-S=C-S-Mo(CO)3(C5H4COOCH3)](μ-S-tBu)[Fe2 (CO)6] (lb), [μ-S=C-S-W(CO)3(C5H4COCH3)](μ-SEt)[Fe2(CO)6] (2a),[μ-S=C-S-W (CO)3(C5H4COCH3)](μ-S-tBu)[Fe2(CO)6](2b), [(μ-S=C-S-Mo(CO)3(C5H4COOCH3) Fe2(CO)6]2(μ-SCH2CH2OCH2CH2S-μ)(3), [(μ-S=C-S-W(CO)3(C5H4COCH3)Fe2 (CO)6]2(μ-SCH2CH2OCH2CH2S-μ)(4)and{(μ-SEt)(μ4-S)[Fe2(CO)6]2]}[μ-S-W(CO)3 (C5H4COCH3)] (5) were produced by reactions of electrophiles (C5H4COOCH3)Mo (CO)3I or (C5H4COCH3)W(CO)3I with the corresponding anionic salts (μ-SR)(μ-SCS")Fe2(CO)6(Et3NH)(B),(μ-S-CH2CH2OCH2CH2-S-μ)[(μ-SCS-)Fe2 (CO)6]2(Et3NH)2(D) and (μ-SEt)(μ4-S))(μ-S-)[Fe2(CO)6]2(Et3NH) (E). These products were characterized by elemental analysis, IR and 1H NMR. The structures of la and 2a were confirmed by X-ray diffraction techniques.
5. Two new Fe/Se cluster complexes (μ-SeEt)(μ-SePh2P-μ)Fe2(CO)6 (1) and (μ-SeEt){μ-Se[(CH3)2CH]2P-μ)Fe2(CO)6 (2) were first prepared, and they were characterized by elemental analysis, IR,1H NMR,31P NMR and 77Se NMR spectroscopies and the structure of 1 was confirmed by X-ray diffraction technique.
In addition, the molecular structures of four compounds prepared by others in our group were confirmed by X-ray diffraction techniques.
引文
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