摘要
含氮宾的两个三核羰基铁簇合物是由[Et_3NH][HFe_3(CO)_(11)]与C_6H_5NCO在苯中反应获得。应用四园衍射仪测定了H_2Fe_3(N-C_6H_5)(CO)_9(Ⅰ)和Fe_3(N-C_6H_5)(μ_3-CO)(CO)_9(Ⅱ)的晶体结构。晶体数据为:C_(15)H_7NO_9Fe_3(Ⅰ),空间群P2_1/a,a=18.343(2),b=9.072(1),c=11.451(1)(?),β=102.03(1)°,V=1863.7(?)~3,Z=4,D_c=2.143g/cm^3;C_(16)H_5NO_(10)Fe_3(Ⅱ),空间群P2_1/c,a=8.634(1),b=13.026(1),c=17.642(2)(?),β=97.68(1)°,V=1966.3(?)~3,Z=4,D_c=1.820g/cm结构系用直接法解出,最后R_(Ⅰ)因子为0.033,R_(Ⅱ)因子为0.027。测定结果表明,(Ⅰ)和(Ⅱ)分子均具有C_s对称性,且三个Fe原子共面,呈近似等边三角形结构。(Ⅰ)中面桥N原子以不对称方式与三个Fe原子成键;(Ⅱ)中面桥羰基以不对称方式与三个Fe原子键连。Fe-N和Fe-C键长分别在1.896-1.938(?)和2.006-2.110(?)之间。
The nitrene containing trinuclear iron carbaonyl clusters were prepared by reacting (Et3NH)(HFe3(CO)11) with C6H5NCO in benzene.
The crystal structure of H2Fe3(CO)9(μ3-NC6H5) and Fe3(CO)9(μ3-CO)(μ3-NC6H5) have been determined by single crystal diffractometry. Crystal data:(Ⅰ) C15H7NO9Fe3, space group P2,/a, a= 18.343(2), b = 9.072(1), c= 11.451(1)A,β = 102.03(1), V= 1863.7 A3,Z=4,Dc = 2.143gcm-3; (Ⅱ)C16H5NO10Fe3 ,space group P21/c,a = 8.634(1), b=13.026(1), c=17.642(2)A, β = 97.68(1), V=1966.3A3, Z = 4, Dc= 1.820gcm-3. Based on observed MoKx data, the structures were solved by direct method and refined to R(Ⅰ) =0.033 for 1796 reflections, and R(Ⅱ) =0.027 for 2679 reflections. All three iron interactions are bonding ((Ⅰ )2.577, 2.573, 2.510A;(Ⅱ)2.571, 2.553, 2.510A) and define a nearly equilateral triangle. The molecular configurations and Fe-N, Fe-Fe distances are discussed together with the electron distribution relationships.
出处
《无机化学学报》
SCIE
CAS
CSCD
北大核心
1991年第2期202-207,共6页
Chinese Journal of Inorganic Chemistry
关键词
铁
羰基簇合物
氮宾
卡宾
合成
iron carbonyl cluster, nitrene containing complex, crystal structure
