摘要
合成了2-环己氧羰基乙基三氯化锡及其N,N-二乙基二硫代氨基甲酸配合物,通过元素分析、IR、1H和13CNMR及X-射线单晶衍射对其结构进行了表征。化合物2属于单斜晶系,C2/c空间群,晶胞参数为a=1.90867(17)nm,b=0.67885(8)nm,c=3.1902(3)nm,β=97.311(7)°,Z=8,μ=1.715mm-1,R=0.0334。中心锡原子为含有分子内羰基氧原子和N,N-二乙基二硫代氨基甲酸配体的两个硫原子配位的畸变八面体构型。波谱数据表明化合物1和2存在着分子内羰基氧原子对锡原子的配位,而在化合物3和4中这一配位则被两个或三个双齿二硫代氨基甲酸配体所替代。化合物2的理论研究表明AM1半经验计算可以成功预测这类有机锡化合物的几何构型。
2-Cyclohexyloxycarbonylethyltin trichloride and its complexes with N, N-diethyldithiocarbamate, (CH2)(5)CHO COCH2CH2SnCl3-x[S2CN(Et)(2)](x) (x = 0, 1; 1, 2; 2, 3; 3, 4), were synthesized and characterized by the means of elemental analysis, IR, H-1 and C-13 NMR and X-ray single crystal diffraction. The crystal structure of complex 2 (monoclinic space group C2/c with unit cell parameters a = 1.90867 (17) nm, b = 0.67885 (8) nm, c = 3.1902 (3) nm, beta = 97.311 (7)degrees, Z = 8, mu = 1.715mm(-1), R = 0.0334) shows that the tin atom adopts a distorted octahedral geometry via the N, N-diethyldithiocarbamate ligand and intramolecular carbonyl oxygen to tin coordination. The spectral data suggest that intramolecular carbonyl oxygen to tin coordination in 1 is existent and is not allowed in order to accommodate two and three bidentate dithiocarbamate ligands in 3 and 4 respectively. Theoretical study for 2 indicates that AM1 semi-empirical calculations successfully predict the molecular geometries for these organotin compounds in the solid.
出处
《无机化学学报》
SCIE
CAS
CSCD
北大核心
2003年第7期685-690,共6页
Chinese Journal of Inorganic Chemistry
基金
国家自然科学基金资助项目(No.20173050)
晶体材料国家重点实验室资助项目。
