2-甲酰吡啶缩氨基硫脲合成和分子结构测定

Synthesis and Molecular Structure Determination of 2-Formylpyridine Thiosemi arbazone

用α-皮考啉,硫磺和氨基硫脉合成的C_7H_5N_4S·2H_2O为橙黄针状晶体,四方晶系,空间群14_I/a.a=1.367 1(1),c=2.217 6(3)nm.V=4.144nm^2,Z=16,D_(cal)=1.360g/cm^3.D_(oba)=1.350g/cm^3.经石墨单色化的Moka辐射,以ω/2θ方式扫描收集1885个独立反射,其中1253个可观察反射参加结构解析和精修.最终残差指数R=0.041,位移/误差=0.09,单位权重观察值最大误差为1.550.晶体结构分析揭示化合物属于E型结构.每一不对称单位统计上包含二个结晶水,而且观察到明显的O…H-N类型的氢键的存在.

The title compound C7H8N4S (HPAT) has been synthesized by thereation of α-picoline, sulphur with thiosemicarbazide, Which crystalizes as needle-like habit with an orangesh red colour. It belons to tetragonal system, space goup I41/a, a = l. 3671 (1), c=2. 2176(3)nm, v=4. 144 7(nm)3, z=16, Dcal=1. 360g/cm3, Dobs=l. 350g/cm3, Moka( = 0. 071069nm) radiation was used to collect intensity data by ω-2θ scan mode. U-nique reflections of 1885 have been measured, of which 1253 reflections were participated in structure determination and refinement, The final residual index R=0.041, shift/error=0. 09, and maximum error of an observation value of unit weight is 1. 550. The crystal structure reveals that this compound possesses the configuration of E-isomer; and contains two water molecules in asymmetric unit statistically; furthermore, Hydrosen bond of O…H-N type is found in the crystal.