新颍Mo-Cu-Se簇合物｛MoCu_3Se_3I｝(PPh_3)_3O·0.5CH_2Cl_2的合成及晶体结构

SYNTHESIS AND CRYSTAL STRUCTURE OF A NOVEL Mo Cu Se CLUSTER COMPOUND {MoCu 3Se 3I}(PPh 3) 3O·0.5CH 2Cl 2

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）。

The new novel Mo Cu Se cluster compound {MoCu 3Se 3I}(PPh 3) 3O·0.5CH 2Cl 2 has been synthesized by 2MoSe 4 , Cu(PPh 3) 2NO 3, KI in CH 3CN/CH 2Cl 2 (1∶1) solvent. Its crystal is monoclinic, space group P2 1/c with unit cell parameters: a =11.994(2), b =28.358(8), c =19.500(3); β =102.04(1)°; V =6486.7(4) 3; Z=4; D c=1.58 g/cm 3; F (000)=2992. The final R=0.073 and R W=0.079 for 4057 (I>3.0 (σ)) observed reflections. The core {MoCu 3Se 3I} of the title compound is a distorted cubic configuration. The average values of Mo Cu and Mo Se bond length are 2.782 and 2.385, respectively. The Cu I bond lengths vary from 2.803(4) to 3.015(4).