双二硫代吡咯烷基铜的固相合成及其晶体结构

Solid State Sytheses and Crystal Strusture of Bis (Pyrrolidone-carbothioato)Copper (Ⅱ)

标题化合物用低热固相合成．其单晶经ｘ射线结构分析，获得晶体属三斜晶系，空间群Ｐ，ａ＝０．７４８（２），ｂ＝０．８０６（１），ｃ＝０．６３８ｎｍ，α＝１０４．８２（１），β＝９４．１０（２），γ＝７６．５９（２）°，ｖ＝０．３６１７ｎｍ３，ｚ＝１，Ｄｃａｌ＝１．６３ｇ／ｃｍ３．晶体结构用直接法解出，所有非氢原子的座标参数和各向异性热振动参数经全矩阵最小二乘修正，最后偏离因子Ｒ１＝０．０５０，Ｒ２＝０．０６０．考虑到该络合物的分子结构中心部分是属于一个较大范围的共轭体系．因此，四个Ｃｕ－Ｓ键键长为０．２２８和０．２３１ｎｍ，两个Ｃ－Ｓ键长为０．１７１和０．１７２ｎｍ以及Ｃ１－Ｎ键长为０．１３２ｎｍ，是较合理的，且与镍和铜的同类络合物一致．

The title Compound was obtained by solid state syntheses under lower temperature,and the single crystal was determinde by X-ray crystallographic analysis: Triclinic, Space Group P1,a=0. 748(2),b=0.806(1),c=0. 638(l),a=104. 82(1),β=94.10(2),γ=76. 59 (2),v=0.3617nm￣3. The structure was solved by direct methods,and refined by Full Matrix Least-Squars with all non-hydrogen atoms and anisotropic thermal parameters, Finally,R_1= 0. 050, R_2=0. 060. It was expected that considerably conjugated system of center of molecular structure,therefore, four Cu-S bond distance 0. 228 and 0. 231 nm,two C-S bond distance 0.171 and 0.172nm,and C-N bond distance 0.132nm agreed with those parent complexes of Nickel(Ⅱ) and Copper(Ⅱ).