含硫磷桥基的两核铁羰基簇合物的合成和晶体结构
Synthesis and Crystal Structure of D inuclear Iron Carbonyl Clusters Containing a Phosphido-Thiolato Bridging Ligand
作者单位
宫培军 内蒙古大学化学化工学院, 呼和浩特010021 
吴秉芳 内蒙古大学化学化工学院, 呼和浩特010021 
胡其图 内蒙古大学化学化工学院, 呼和浩特010021 
刘树堂 内蒙古大学化学化工学院, 呼和浩特010021 
摘要: Fe3(CO)12与杂环二硫代次膦酸盐SP(C6H4OR)(S)N(C6H5)NC(Me)(R=Me,Et)反应,得到两个新的含硫磷桥基的双核铁羰基簇合物Fe2(CO)6[μ-η2-SC(Me)NN(C6H5)P(C6H4O
关键词: 双核铁羰基簇合物  硫磷桥基配体  合成  晶体结构
基金项目: 国家自然科学基金资助项目(No.29861001);内蒙古自然科学基金资助项目No.980201
Abstract: The reaction of Fe3(CO)12with two cyclic dithiophosphinate SP(S)(C6H4OR)N(C6H5)NC(Me )(R =Me,Et ),yields two novel dinuclear iron carbonyl clusters contining a phosphi do-thiolato bridging μ-η2-SCNNP ligand Fe2(CO)6[μ-η2-SC(Me )NN(C6 H5)P(C6H4 OMe )](Ⅰ),Fe2(CO)6[μ-η2-SC(Me)NN(C6H5)P(C6H4OEt)](Ⅱ) and cluster Fe3(CO)93-S)2(known).We suggest that during the reaction ,the ligand precursor has been cleaved in its P =Sand P-Sbonds and opened its ring to give the fragments as ligands μ3-S,μ-η2-SC(Me)NN(C6H5)P(C6H4OR)that coordinated to the iron atoms of the decarbonyl fragmental Fe3(CO)12to form the clusters as listed above.The clusters were characterized by elemental analysis,IR,1H NMR and Ms spectrometric methods ,and the molecular structure of cluster?has been determined by X-ray diffrac tion method,it belongs to monoclini c with space group P2(1)/n,a=11.192(2)Å,b=14.272(3)Å,c=16.281(3)Å,V=2470.2(8)Å3,β=108.22(3)°,Dc=1.565g·cm-3,Z =4,F(000)=1176,R=0.0460,Rw=0.1196.The din-uclear cluster has two bridges Fe-S-Fe and Fe-P-Fe,and the chain C (7)-N(2)-N(1)link the sul-phur atom and the phosphorus atom ,th at contains two six-membered chelate rings Fe(1)SCNNP and Fe(2)PNNCS in the cluster,they enhanced t he stability of the cluster.
Keywords: dinuclear iron carbonyl cluster  phosphido-thiolato bridging ligand  synthesis  crystal structure
投稿时间:2001-04-06 修订日期:2001-05-22
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宫培军,吴秉芳,胡其图,刘树堂.含硫磷桥基的两核铁羰基簇合物的合成和晶体结构[J].无机化学学报,2001,17(6):794-798.
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