新颍ＭｏＣｕＳｅ簇合物｛ＭｏＣｕ３Ｓｅ３Ｉ｝（ＰＰｈ３）３Ｏ·０．５ＣＨ２Ｃｌ２是由［Ｅｔ４Ｎ］２ＭｏＳｅ４、Ｃｕ（ＰＰｈ３）２ＮＯ３和ＫＩ在乙腈和二氯甲烷１∶１的混合溶剂中反应所得。晶体属单斜晶系，空间群Ｐ２１／ｃ；晶胞参数：ａ＝１１．９９４（２），ｂ＝２８．３５８（８），ｃ＝１９．５００（３）；β＝１０２．０４（１）°；Ｖ＝６４８６．７（４）３；Ｚ＝４；Ｄｃ＝１５８ｇ／ｃｍ３；Ｆ（０００）＝２９９２。晶体结构用直接法解出，经全矩阵最小二乘法修正，用４０５７个Ｉ＞３．０σ（Ｉ）的独立衍射点，最终偏离因子Ｒ＝０．０７３，ＲＷ＝０．０７９。标题化合物的核心｛ＭｏＣｕ３Ｓｅ３Ｉ｝是一个崎变的立方烷构型。ＭｏＣｕ和ＭｏＳｅ的平均间距分别是２７８２和２３８５；三个ＣｕＩ的间距为２８０３（４），２９０５（３），３０１５（４）。 New Ying Mo-Cu-Se cluster {MoCu3Se3I} (PPh3) 3O0.5CH2Cl2 is obtained by the reaction of [Et4N] 2MoSe4, Cu (PPh3) 2NO3 and KI in a mixed solvent of acetonitrile and dichloromethane 1: 1 . The crystal is monoclinic with space group P21 / c; unit cell parameters are a = 11.994 (2), b = 28.358 (8) and c = 19.500 (3) (1) °; V = 6486.7 (4) 3; Z = 4; Dc = 158g / cm3; F (000) = 2992. The crystal structure was solved by the direct method and corrected by full matrix least square method. The final deviation factor R = 0.073 and RW = 0.079 were obtained with 4057 independent diffraction points with I> 3.0σ (I). The core of the title compound {MoCu3Se3I} is a Kawasaki-like alkane configuration. The average spacing between MoCu and MoSe is 2782 and 2385, respectively. The spacings of three CuI are 2803 (4), 2905 (3), 3015 (4)  .