一价铜配合物〔Cu（C_8H_4F_3O_2S）（PPh_3）_2〕的合成和晶体

Synthesis and Structure of [Cu(C_8H_4O_2F_3S) (PPh_3)_2]

室温下，铜粉和２－噻吩甲酰三氟丙酮、三苯基膦在甲醇和四氢呋喃混合溶剂中反应，生成一价铜的配合物［Ｃｕ（Ｃ_８Ｈ_４Ｆ_３Ｏ_２Ｓ）（ＰＰｈ_３）_２］，测定了该配合物的晶体结构，结果表明，晶体属单斜晶系，Ｐ２_１／ｎ空间群，晶胞参数：ａ＝１０．５８４（１），ｂ＝１６．７３８（１），ｃ＝２２．７２８（９）Ａ；β＝９４．２２（２）°，Ｖ＝４０１５．２Ａ３，Ｍｒ＝７８５．２９，Ｚ＝４，Ｄｃ＝１０２９９ｇ／ｃｍ３，μ＝９．８６ｃｍ－１。晶体结构由直接法解出，使用块对角矩阵和全矩阵最小二乘法对原子参数进行修正，最后偏离因子Ｒ＝０．０４８，Ｒｗ＝０．０５４，其中４３９１个Ｉ＞３σ（Ｉ）的可观察衍射点参加了结构修正，结果表明，Ｃｕ原子由２个Ｏ原子和２个Ｐ原子配位，形成畸变四面体构型。

Reaction of Cu (1 mmol) with 2-thenoyltrifluoroacetone( 1mmol) and PPh_3 (2 mmol) gave a Cu (I) complex [Cu(C_8H_4O_2F_3S) (PPh_3)_2]. X-ray crystal structure analysis revealed that Cu (I) ion is coordinated by one 2-thenoyltrifluoroacetone and two PPh_3 to form a tetrahedron. Crystal data: Mr= 785. 29, monoclinic, space group. The structure was solved by direct methods,and refined by block diagonal and full-matrix least-squares method to a final R=0. 0484 and R_w= 0. 0544.