C l2M eS iS iM eC l2与环戊二烯基锂及对甲苯基溴化镁反应,生成C5H5(p-Tol)M eS iS iM e(p-Tol)C5H5.后者再与五羰基铁反应,得到标题化合物[η5,η5-C5H4(p-Tol)M eS iS iM e(p-Tol)C5H4]Fe2(CO)2(μ-CO)2(3);同时还得到两个单硅桥连...C l2M eS iS iM eC l2与环戊二烯基锂及对甲苯基溴化镁反应,生成C5H5(p-Tol)M eS iS iM e(p-Tol)C5H5.后者再与五羰基铁反应,得到标题化合物[η5,η5-C5H4(p-Tol)M eS iS iM e(p-Tol)C5H4]Fe2(CO)2(μ-CO)2(3);同时还得到两个单硅桥连副产物[η5,η5-(p-Tol)2M eS iS iM e(C5H4)2]Fe2(CO)2(μ-CO)2(4)和[η5,η5-(p-Tol)M e2S iS iM e(C5H4)2]Fe2(CO)2(μ-CO)2(5).化合物3中顺式异构体(3a)占绝对优势,可通过简单重结晶分离出纯品.化合物3a在加热条件下发生分子内的硅硅键和铁铁键之间的复分解重排反应,生成[η5-(p-Tol)M eS iC5H4Fe(CO)2]2(6).该产物为顺反异构体的混合物(顺反异构体的摩尔比为4∶3),表明重排反应不涉及协同历程.利用X射线衍射法测定了化合物4的分子结构.展开更多
The complex(C5Me4iBu)2Ru2(CO)4 has been synthesized by the reaction of C5Me4iBuH with Ru3(CO)12 in refluxing xylene and its molecular structure was characterized by elemental analysis,IR spectra,1H NMR and X-ray cryst...The complex(C5Me4iBu)2Ru2(CO)4 has been synthesized by the reaction of C5Me4iBuH with Ru3(CO)12 in refluxing xylene and its molecular structure was characterized by elemental analysis,IR spectra,1H NMR and X-ray crystal structure determination.Crystal data for this compound:Triclinic,space group P1,Mr=668.78,a=0.865 96(17)nm,b=0.892 90(18)nm,c=0.975 7(2)nm,α=88.39(3)°,β=71.64(3)°,γ=84.99(3)°,V=0.713 3(2)nm3,Z=1,Dc=1.557 g.cm-3,μ(Mo Kα)=1.091mm-1,F(000)=342,R1=0.025 3,wR2=0.067 6(observed reflections with I>2σ(I))and R1= 0.026 9,wR2=0.068 2(all reflections).The structure of the dimer confirms the structure with bridging and terminal CO groups,and the Ru-Ru bond distance is 0.275 19(8)nm.CCDC:693389.展开更多
文摘C l2M eS iS iM eC l2与环戊二烯基锂及对甲苯基溴化镁反应,生成C5H5(p-Tol)M eS iS iM e(p-Tol)C5H5.后者再与五羰基铁反应,得到标题化合物[η5,η5-C5H4(p-Tol)M eS iS iM e(p-Tol)C5H4]Fe2(CO)2(μ-CO)2(3);同时还得到两个单硅桥连副产物[η5,η5-(p-Tol)2M eS iS iM e(C5H4)2]Fe2(CO)2(μ-CO)2(4)和[η5,η5-(p-Tol)M e2S iS iM e(C5H4)2]Fe2(CO)2(μ-CO)2(5).化合物3中顺式异构体(3a)占绝对优势,可通过简单重结晶分离出纯品.化合物3a在加热条件下发生分子内的硅硅键和铁铁键之间的复分解重排反应,生成[η5-(p-Tol)M eS iC5H4Fe(CO)2]2(6).该产物为顺反异构体的混合物(顺反异构体的摩尔比为4∶3),表明重排反应不涉及协同历程.利用X射线衍射法测定了化合物4的分子结构.
文摘The complex(C5Me4iBu)2Ru2(CO)4 has been synthesized by the reaction of C5Me4iBuH with Ru3(CO)12 in refluxing xylene and its molecular structure was characterized by elemental analysis,IR spectra,1H NMR and X-ray crystal structure determination.Crystal data for this compound:Triclinic,space group P1,Mr=668.78,a=0.865 96(17)nm,b=0.892 90(18)nm,c=0.975 7(2)nm,α=88.39(3)°,β=71.64(3)°,γ=84.99(3)°,V=0.713 3(2)nm3,Z=1,Dc=1.557 g.cm-3,μ(Mo Kα)=1.091mm-1,F(000)=342,R1=0.025 3,wR2=0.067 6(observed reflections with I>2σ(I))and R1= 0.026 9,wR2=0.068 2(all reflections).The structure of the dimer confirms the structure with bridging and terminal CO groups,and the Ru-Ru bond distance is 0.275 19(8)nm.CCDC:693389.
