呋喃醛双缩二氨基硫脲腙的合成和结构测定

由ＣＳ＿２，Ｎ＿２Ｈ＿４和Ｃ＿４Ｈ＿３ＯＣＨＯ合成Ｃ＿（１１）Ｈ＿（１０）Ｎ＿４Ｏ＿２Ｓ·１／２ＤＭＦ，Ｍ＿ｒ＝２９８．７９，橙黄针状晶体，三斜晶系，空间群Ｐ１，ａ＝８．９１２（３），ｂ＝９．９８９（３），ｃ＝１６．１０７（４），ａ＝８３．６１８（６），β＝８７．１０５（５），γ＝８６．１１５（３）°，Ｖ＝１４２０．４，Ｚ＝４，Ｄ＿ｘ＝１．３９７ｇ／ｃｍ￣３，λ（ＭｏＫα）＝０．７１０７３，μ＝２．１７０ｃｍ￣（－１），Ｆ（０００）＝６１６。３２２６个可观察的独立反射（Ｉ＞３σ（Ｉ）使结构顺利解出，并精修到Ｒ＝０．０４８，△ρ＿（ｍａｘ）＝０．２８６。单晶体结构分析表明不对称单位含有二个非结晶学对称相关的独立分子和一个溶剂分子ＤＭＦ，通过ＤＭＦ中的ｏ原子和亚胺Ｈ形成Ｎ－Ｈ…Ｏ…Ｈ－Ｎ类型双氢键，使两个分立分子缔合一起而自成独立的结构单元。

Synthesis and Structure of Bis-Furfural Thiocarbazone

This paper reports the synthesis of the title compound C_(11)H_(10)N_4O_2S·1/2 DMF, from CS_2, N_2H_4·H_2O and 2-furfural. M_r = 298. 79,orangeyellow needle-like crystal, triclinic system , spqce group P1, a = 8. 912(3). b=9. 989(3) , c=16. 107(4) ,α=83. 618(6i),β=87. 105(5), γ=86. 115(3)°,V= 1420. 4 , Z=4, D_x=1. 397 g/cm￣3 .λ(MoKα) = 0.71073,μ= 2. 170 cm￣(-1) , F(000) = 616. The structure was solved satisfactorily by direct methods and Fourier technique using 3226 observable independent reflections with I>3σ(I) ,and refined to final R=0. 048, R_w = 0. 049 (W=1) . △/σ= 0. 001 , maximum error of an observable value of unit weight is 1. 078 , △ρ_(max)= 0. 286 e/ by means of normal refinement procedure. The structure analysis revealed that an asymmetry unit consists of two non-crystallography symmetry related independent molecules and one solvent DMF molecule. Because the network of double hydrogen bonds as N-H…O…H-N was formed between two molecules and DMF bridged by oxygen atom in DMF and hydrogen atoms in imido-group, two discrete molecules was associated with each other more closely and became an independent structure unit.