| 含偶磷氮烷配体的三核钌羰基簇合物的合成和晶体结构 |
| Synthesis and Crystal Strrctures of Trinuclear Ruthenium Carbonyl Clusters Containing Cyclodiphosphazane Ligand |
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| 摘要: 用Ru3(CO)12与顺-2,4二(叔丁基胺基)-1,3,-二(叔丁基)-1,3,2,4-环偶磷氮烷cis-[P(NHBut)NBut]2反应,得到两个新的含偶磷氮环的三核钌羰基簇合物:Ru3(CO)11[{P(NHBut)NBut}2] Ⅰ和Ru3(CO)11[P(NHBut)(NBut)2P(O)H] Ⅱ。对它们进行了元素分析,IR和1H NMR谱表征,并用X-ray单晶衍射法测定了晶体结构。Ⅰ:正交晶系,Pna2(1)空间群,a=2.7574(9) nm,b=0.8981(3) nm,c=1.5272(5) nm, V=3.782(2) nm3,Dc=1.686 g·cm-3,Z=4;Ⅱ:三斜晶系,P1空间群,a=0.96384(19) nm,b=1.1705(2) nm,c=1.5589(3) nm,α=101.72(3) °,β=91.54(3) °,γ=108.20(3) °,V=1.6282(6)nm3,Dc=1.845g·cm-3,Z=2;两个簇合物均为Ru3(CO)12的单取代衍生物,配位基环偶磷氮烷以单齿P原子配位在一个Ru原子的赤道位置上。Ⅱ中,偶磷氮环上未配位P(Ⅲ)被氧化成具有膦酰基结构(=P(O)H)的P(Ⅴ)。 |
| 关键词: 钌羰基簇合物 环偶磷氮烷配体 合成 晶体结构 |
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| Abstract: Reaction of Ru3(CO)12 with cis-2,4-di(tert-butylamino)-1,3-di(tert-butyl)-1,3,2,4-cyclodiphosph-(Ⅲ) azane,yielded two novel trinuclear ruthenium carbonyl clusters containing cyclodiphosphazane ligand: Ru3(CO)11[{P(NHBut)NBut}2] (Ⅰ) and Ru3(CO)11[P(NHBut)(NBut)2P(O)H] (Ⅱ). These complexes have been characterized by elementary analysis, IR and 1H NMR spectra and X-ray single crystal diffraction.Ⅰ: Orthorhombic, Pna21, a=2.7574(9) nm, b=0.8981(3) nm, c=1.5272(5) nm, V= 3.782(2) nm3, Dc=1.686 g·cm-3, Z=4; Ⅱ: triclinic, P1, a=0.96384(19) nm, b=1.1705(2) nm, c=1.5589(3) nm, α=101.72(3) °, β=91.54(3) °, γ=108.20(3) °, V=1.6282(6) nm3, Dc=1.845 g·cm-3, Z=2; In two complexes, the phosphorus-nitrogen heterocycle is not cleaved during the reactions, and one P atom of them is coordinated to Ru atom. In the complex Ⅱ, the uncoordinated P(Ⅲ) atom was oxidized to the P(Ⅴ), phosphonic amide =P(O)H, in which process the bond between P and NHBut group was cleaved and one P-H bond was formed. CCDC: Ⅰ, 217283; Ⅱ, 217282. |
| Keywords: ruthenium carbonyl derivative cyclodiphosphazane ligand synthesis crystal structure |
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| 宫培军,吴秉芳,刘树堂,王丁泽.含偶磷氮烷配体的三核钌羰基簇合物的合成和晶体结构[J].无机化学学报,2004,20(1):37-40. |
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