Schiff碱N-氧化吡啶-2-甲醛缩氨基硫脲的晶体结构

Crystal Structure of Schiff-base Picolinaldehyde Thiosemicarbazone N- oxide

合成了标题Ｓｃｈｉｆｆ碱并获得了其单晶，化学式为Ｃ７Ｈ８Ｎ４ＯＳ，Ｍｒ＝ １９６．２３，经Ｘ射线单晶衍射分析，该晶体属于单斜晶系，空间群为Ｃ２／ｃ，晶胞参数： ａ＝ １３．１９８（２），ｂ＝ ８．０７０（１），ｃ＝ １６．９９９（２），β＝ １０２．７６０（１０）°，Ｖ＝ １７６５．８（４）３，Ｚ＝ ８，Ｄｃ＝１．４７６ｇ／ｃｍ ３，μ＝ ０．３３０ｍ ｍ － １，Ｆ（０００）＝ ８１６，在２．４６°＜ θ＜ ２９．００°范围内以ω扫描方式收得独立衍射点２３４７ 个，其中Ｉ＞ ２σ（Ｉ）的可观测点为１６８７ 个。最终偏离因子Ｒ＝０．０３４４，ｗ Ｒ＝ ０．０８４３，（Δ／σ）ｍ ａｘ＝ ０．００１，Ｓ＝ １．０８２。分子为平面构型。与相应配合物的晶体结构进行了比较并讨论了配位前后标题化合物主要的键性质的变化。

The title Schiff base (C 7H 8N 4OS, M r =196.23) was prepared by condensation reaction between picolinaldehyde \$N\$ oxide and thiosemicarbazone, and its single crystal was obtained. The crystal belongs to monoclinic system, space group C 2/c with cell parameters: \$a=13.198(2),b=8.070(1),c=16.999(2),β=102.760(10)°,V=1765.8(4) 3,Z=8,D c\$=1.476g/cm 3, μ =0.330mm -1 ,\$F\$(000)=816。2437 independent reflections were collected with \$ω\$ scans within the range of \$θ\$=2.46 to 29.00°, in which 1687 [\$I>2σ(I)]\$ reflections can be observed. \$R=0\^0344,wR\$=0.0843. (Δ/σ ) max =0.001,S=1.082.The structure of the compound is a plane. The changes of bonding of the title Schiff base were discussed and compared with the known crystal structure of its coordination compounds.