| 簇合物Co3(CO)7(μ3-S)[μ,η2-CNP(S)(C6H4OCH3)OC(Ph)CH]和Co3(CO)7(μ3-S)[μ,η2-SCNC(CH3)2P(S)(Cl)N(Ph)]的合成与晶体结构 |
| Syntheses and Crystalline Structures of Co3(CO)7(μ3-S)[μ,η2-CNP(S)(C6H4OCH3)OC(Ph)CH](Ⅰ) and Co3(CO)7(μ3-S)[μ,η2-SCNC(CH3)< |
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| 摘要: 用Co2(CO)8分别与两个杂环配体C(S)NHP(S)(C6H4OCH3)OC(Ph)CH (L1)和C(S)NHC(CH3)2P(S)(Cl)N(Ph) (L2)反应,合成两个新的三核钴羰基硫簇合物Co3(CO)7(μ3-S)[μ,η2-CNP(S)(C6H4OCH3)OC(Ph)CH](Ⅰ)和Co3(CO)7(μ3-S)[μ,η2-SCNC(CH3)2P(S)(Cl)N(Ph)](Ⅱ)。用元素分析,IR, 1H NMR, 31P NMR及MS谱表征了它们的结构,同时用X射线衍射法测定了它们的晶体分子结构,二者属于三斜晶系,空间群P1,Ⅰ的晶胞参数为:a=0.84768(1)nm,b=1.19049(3)nm,c=1.43639(1)nm,α=86.926(1)°,β=81.601(3)°,γ=88.535(2)°,V=1.4318(5)nm3,Z=2,Dc=1.641g·cm-3,F(000)=716,μ=1.893mm-1,R=0.0602,Rw=0.1515。Ⅱ的晶胞参数为:a=1.2050(2)nm,b=1.2448(2)nm,c=0.8951(2)nm,α=97.49(1)°,β=93.552(4)°,γ=108.432(3)°,V=1.2554(3)nm3,Z=2,Dc=1.841g·cm-3,F(000)=690,μ=2.419mm-1,R=0.0423,Rw=0.1075。Ⅰ和Ⅱ的分子骨架Co3S为三角锥构型,S作为面桥基配体,所有CO作为端基配体与三个Co原子成键。Ⅰ中含有CoCoCN四元环组件,Ⅱ中含有CoCoSCN五元环组件。 |
| 关键词: 钴羰基硫簇合物 合成 晶体结构 |
| 基金项目: |
| Abstract: Through the reaction of Co2(CO)8 with two heterocyclic ligands of C(S)NHP(S)(C6H4OCH3)OC(Ph)CH (L1) and C(S)NHC(CH)P(S)(Cl)N(Ph) (L2),the two trinuclear cobalt carbonyl sulfur clusters, Co3(CO)7(μ3-S)[μ,η2-CNP(S)(C6H4OCH3)OC(Ph)CH](Ⅰ) and Co3(CO)7(μ3-S)[μ,η2-SCNC(CH3)2P(S)(Cl)N(Ph)](Ⅱ), were prepared and characterized by IR, 1H NMR, 31P NMR , MS spectroscopy and X-ray crystal diffraction.The crystals of Ⅰ and Ⅱ are triclinic,belonging to space group P1,a=0.84768(1)nm,b=1.19043(3)nm,c=1.43639(1)nm,α=86.926(1)°,β=81.603(3)°,γ=88.535(2)°,V=1.4318(5)nm3, Z=2, Dc=1.641g·cm-3,F(000)=716,μ=1.893mm-1,R=0.0602, Rw=0.1515 for complex Ⅰ;a=1.2050(2)nm,b=1.2448(2)nm,c=0.8951(2)nm, α=97.49(1)°,β=93.552(4)°,γ=108.432(3)°, V=1.2554(3)nm3, Z=2, Dc=1.841g·cm-3, F(000)=690,μ=2.419mm-1,R=0.0423, Rw=0.1075 for complex Ⅱ. The structure analyses show that the Co3S frameworks of Ⅰ and Ⅱ are a triangular pyramid, respectively, and for which the sulfur atom as face bridging ligand and all carbonyls as terminal ligand link up with three cobalts in the cluster framework. Ⅰ contains a four-member ring of CoCoCN and Ⅱ has a five-member of CoCoSCN. |
| Keywords: cobalt carbonyl sulfur cluster synthesis crystal structure |
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| 关敏,刘树堂,吴秉芳,于世泳.簇合物Co3(CO)7(μ3-S)[μ,η2-CNP(S)(C6H4OCH3)OC(Ph)CH]和Co3(CO)7(μ3-S)[μ,η2-SCNC(CH3)2P(S)(Cl)N(Ph)]的合成与晶体结构[J].无机化学学报,2002,18(4):351-356. |
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