含氮宾或卡宾的金属羰基簇合物的结构化学研究Ⅱ——Fe_2(CO)_6(PhNCONPh)的合成和结构

Structural Chemistry of Nitrene or Carbene Containing Transitionmetal Carbonyl Cluster——Ⅱ.Synthesis and Crystal Structure of Fe_2(CO)_6(PhNCONPh)

Fe_2(CO)_6(PhNCONPh)簇合物是由[Et_3NH][HFe_3(CO)_(11)]和C_6H_5NCO在苯中反应获得。应用四园衍射仪测定了该簇合物的晶体结构。晶体学数据:C_(19)H_(10)O_7N_2Fe_2,空间群P2_1/n,a=8.5062(1),b=13.2752(1),c=18.9038(2)(?),β=98.96(2)°,Z=4和D_c=1.643gcm^(-3)。结构系用直接法解出,最后R 因子为0.031.结果表明,题目簇合物分子是由苯代脲基C_6H_6—N—C(O)—N—C_6H_5中的N 原子,分别和(OC)_3Fe—Fe(CO)_3中的两个Fe 原子键合而成。使各两Fe 与N 原子和一个C 原子形成变形的双三角锥构型。

The nitrene containing trinuclearironcarbonyl clusters were prepared byreacting(Et_3NH)(HFe_3(CO)_(11))and C_6H_5NCO in benzene.The crystal andmoleculer structure of the title compound was determined by x-ray analysis.Crystal data:C_(19)H_(10)O_7N_2Fe_2,space group P2_1/n,a=8.5062(1),b=13.2752(1),c=18.9038(2)(?),β=98.96(2)。,Z=4,Dc=1.643g/cm^3.The diffracted intensitieswere colleted on a CAD-4 diffractometer with MoKα radiation in the rage ofθ°<2θ<50°.The structure was solved by direct method and difference Fouriersynthesis,refined by full-matrix least-squares procedure to the discrepencyfactor R=0.031.The molecular configuration and Fe-N,Fe-C,Fe-Fe distancesalso the electron distribution relationships are discussed.