无机化学学报
無機化學學報
무궤화학학보
JOURNAL OF INORGANIC CHEMISTRY
2003年
10期
1090-1094
,共5页
Fe3(CO)12与配位基前体P(NEt2)2Cl反应,给出4个新的两核和三核铁羰基簇合衍生物:Fe2(CO)6(μ-Cl)[μ-(NEl2)2](I),Fe2(CO)6[μ-P(NEt2)2]2(Ⅱ),Fe3(CO)9(μ-CO)(μ3-PNEt2)(Ⅲ)和Fe3(CO)9(μ3-PNEt2)[P(NEt2)3](Ⅳ).在反应期间,配前体分子中的P-Cl和P-N键劈开,形成的分子片Cl、PNEt2、P(NEt2)2和P(NEt2)3作为配体与铁羰合物重新组建成上述簇合物.利用X射线衍射法测定了它们的晶体结构.I属三斜晶系,P1空间群,晶胞参数a=0.8745(6)nm,b=0.9601(7)nm,c=1.3996(10)nm,α=74.131(11)°,β=79.480(12)°,γ=69.727(12)°,V=1.0553(13)nm3,Dc=1.543g@cm-3,Z=2,R=0.0443,wR=0.0831.Ⅱ属正交晶系,Pbcn空间群,晶胞参数a=1.0153(3)nm,b=1.7543(5)nm,c=1.6860(5)nm,V=3.0031(15)nm3,Dc=1.394g@cm-3,Z=4,R=0.0519,wR=0.1035.Ⅲ属单斜晶系,P21/c空间群,晶胞参数a=1.0280(5)nm,b=1.2113(5)nm,c=1.7192(7)nm,β=93.560(7)°,V=2.1366(16)nm3,Dc=1.712g@cm-3,Z=4.Ⅳ属单斜晶系,Cc空间群,晶胞参数a=1.5875(7)nm,b=1.0359(5)nm,c=2.1919(9)nm,β=101.266(8)°V=3.535(3)nm3,Dc=1.443g@cm-3,Z=4.Ⅰ和Ⅱ为两核铁簇,其簇骨架Fe2PCl和Fe2P2呈蝶状.Ⅲ和Ⅳ为三核铁簇,其簇骨架Fe3P为含面桥μ3-PNEt2的三角锥构型.
Fe3(CO)12與配位基前體P(NEt2)2Cl反應,給齣4箇新的兩覈和三覈鐵羰基簇閤衍生物:Fe2(CO)6(μ-Cl)[μ-(NEl2)2](I),Fe2(CO)6[μ-P(NEt2)2]2(Ⅱ),Fe3(CO)9(μ-CO)(μ3-PNEt2)(Ⅲ)和Fe3(CO)9(μ3-PNEt2)[P(NEt2)3](Ⅳ).在反應期間,配前體分子中的P-Cl和P-N鍵劈開,形成的分子片Cl、PNEt2、P(NEt2)2和P(NEt2)3作為配體與鐵羰閤物重新組建成上述簇閤物.利用X射線衍射法測定瞭它們的晶體結構.I屬三斜晶繫,P1空間群,晶胞參數a=0.8745(6)nm,b=0.9601(7)nm,c=1.3996(10)nm,α=74.131(11)°,β=79.480(12)°,γ=69.727(12)°,V=1.0553(13)nm3,Dc=1.543g@cm-3,Z=2,R=0.0443,wR=0.0831.Ⅱ屬正交晶繫,Pbcn空間群,晶胞參數a=1.0153(3)nm,b=1.7543(5)nm,c=1.6860(5)nm,V=3.0031(15)nm3,Dc=1.394g@cm-3,Z=4,R=0.0519,wR=0.1035.Ⅲ屬單斜晶繫,P21/c空間群,晶胞參數a=1.0280(5)nm,b=1.2113(5)nm,c=1.7192(7)nm,β=93.560(7)°,V=2.1366(16)nm3,Dc=1.712g@cm-3,Z=4.Ⅳ屬單斜晶繫,Cc空間群,晶胞參數a=1.5875(7)nm,b=1.0359(5)nm,c=2.1919(9)nm,β=101.266(8)°V=3.535(3)nm3,Dc=1.443g@cm-3,Z=4.Ⅰ和Ⅱ為兩覈鐵簇,其簇骨架Fe2PCl和Fe2P2呈蝶狀.Ⅲ和Ⅳ為三覈鐵簇,其簇骨架Fe3P為含麵橋μ3-PNEt2的三角錐構型.
Fe3(CO)12여배위기전체P(NEt2)2Cl반응,급출4개신적량핵화삼핵철탄기족합연생물:Fe2(CO)6(μ-Cl)[μ-(NEl2)2](I),Fe2(CO)6[μ-P(NEt2)2]2(Ⅱ),Fe3(CO)9(μ-CO)(μ3-PNEt2)(Ⅲ)화Fe3(CO)9(μ3-PNEt2)[P(NEt2)3](Ⅳ).재반응기간,배전체분자중적P-Cl화P-N건벽개,형성적분자편Cl、PNEt2、P(NEt2)2화P(NEt2)3작위배체여철탄합물중신조건성상술족합물.이용X사선연사법측정료타문적정체결구.I속삼사정계,P1공간군,정포삼수a=0.8745(6)nm,b=0.9601(7)nm,c=1.3996(10)nm,α=74.131(11)°,β=79.480(12)°,γ=69.727(12)°,V=1.0553(13)nm3,Dc=1.543g@cm-3,Z=2,R=0.0443,wR=0.0831.Ⅱ속정교정계,Pbcn공간군,정포삼수a=1.0153(3)nm,b=1.7543(5)nm,c=1.6860(5)nm,V=3.0031(15)nm3,Dc=1.394g@cm-3,Z=4,R=0.0519,wR=0.1035.Ⅲ속단사정계,P21/c공간군,정포삼수a=1.0280(5)nm,b=1.2113(5)nm,c=1.7192(7)nm,β=93.560(7)°,V=2.1366(16)nm3,Dc=1.712g@cm-3,Z=4.Ⅳ속단사정계,Cc공간군,정포삼수a=1.5875(7)nm,b=1.0359(5)nm,c=2.1919(9)nm,β=101.266(8)°V=3.535(3)nm3,Dc=1.443g@cm-3,Z=4.Ⅰ화Ⅱ위량핵철족,기족골가Fe2PCl화Fe2P2정접상.Ⅲ화Ⅳ위삼핵철족,기족골가Fe3P위함면교μ3-PNEt2적삼각추구형.