本文合成了簇合物〔（Ｐｈ３Ｐ）２Ｎ〕〔ＦｅＣｏ３（ＣＯ）１２〕并测定了其晶体结构。单晶结构数据如下：Ｍ＝１１０７．３６，单斜晶系，空间群Ｐ２１／ｎ：ａ＝１３．８５７（３），ｂ＝１０．９０６（５），ｃ＝３２．１５５（６），β＝１００．０９（２）°，Ｖ＝４７８４（２）３，ｚ＝４，μ（ＭｏＫα）＝１４．４８ｃｍ－１，Ｄｃ＝１．５３７ｇ／ｃｍ３，Ｆ（０００）＝２２３２。用３０８２个可观测衍射点（Ⅰ＞３．００σ（Ⅰ））对结构进行精修，最终偏离因子Ｒ＝０．１３６，Ｒｗ＝０．１６８。在该簇合物中，ＦｅＣｏ３骨架是一个四面体构型，其中阴离子〔ＦｅＣｏ３（ＣＯ）１２〕－的负电荷集中在簇骨架的Ｆｅ原子上。 In this paper, the cluster complex [(Ph3P) 2N] [FeCo3 (CO) 12] was synthesized and its crystal structure was determined. The single crystal structure data are as follows: M = 1107.36, monoclinic, space group P21 / n: a = 13.857 (3), b = 10.906 (5), c = 32.155 , Β = 100.09 (2) °, V = 4784 (2) 3, z = 4, μ (MoKα) = 14.48 cm -1, Dc = 1.537 g / cm 3, F (000) = 2232. The structure was refined using 3082 observable diffraction points (Ⅰ> 3.00σ (Ⅰ)) with a final deviation factor of R = 0.136 and Rw = 0.168. In this cluster, the FeCo3 framework is a tetrahedral structure in which the negative charge of the anion [FeCo3 (CO) 12] - is concentrated on the Fe atoms of the cluster skeleton.