摘要
本文采用微波固相反应、液相反应和固液相反应的方法共制备了九种新的生物无机配合物,对新制备的配合物分别采用元素分析、XRD分析与计算、红外、拉曼和扫描电镜等手段进行了表征,研究其组成和结构。结果分别为甘氨酰谷氨酰胺硫酸铜属于单斜晶,其分子式为(C7H13O4N3)2(CuSO4)·4.5H2O,晶胞参数为：a=11.6037 nm,b=8.3963 nm,c=5.6518 nm,α=90.0°,β=99.1°,γ=90.0°；N-乙酰-L-谷氨酰胺硫酸铜属于正交晶系,其分子式为(NH2COCH2CH2C(COOH)NHCOOH)2(CuSO4)·2.5H2O,晶胞参数为：a=16.4671nm,b=9.1700nm,c=7.6919nm,α=90.0°,β=90.0°,γ=90.0°；L-精氨酸α-酮戊二酸铜属于三斜晶形,其分子式为C17H38N8O11Cu·H2O,空间群为P-1,晶胞参数为：a=9.0478nm,b=7.3516 nm,c=6.5809nm,α=111.6°,β=103.4°,γ=102.6°；L-精氨酸焦谷氨酸铜属于三斜晶形,其分子式为5C6H17N4O7·2Cu,空间群为P1,晶胞参数为：a=14.5805nm,b=11.8571 nm,c=13.8994 nm,α=81.7°,β=117.4°,γ=199.4°;L-精氨酸谷氨锌属于正交晶形,其分子式为C11H24N2O16·Zn,空间群为P 21 21 21,晶胞参数为：a=11,1780nm,b=10.4598nm,c=7.2161nm,α=90.0°,β=90.0°,γ=90.0°;L-赖氨酸L-天门冬氨酸铜属于正交晶形,其分子式为C30H57N7O18·Cu12·20H2O,空间群为P 222,晶胞参数为：a=10.2930nm,b=16.1275nm,c=9.2356nm,α=90.0°,β=90.0°,γ=90.0°；二巯基丁二酸氯化铋产物属于单斜晶系,晶胞参数为：a=1.4616nm,b=1.3629nm, c=1.3919nm,α=90.0°,β=130.5°,γ=90.0°；二巯基丁二酸硫酸亚铁属于三斜晶系,其分子式为FeSO43.5H2O(C4H6O4S2),晶胞参数为：a=0.8044nm,b=0.9813nm,c= 2.1612 nm,α=90.8°,β=120.8°,γ=121.8°；氨三乙酸硫酸铜属于单斜晶系,分子式为(CuSO4)2(C6H9O6N)7H2O,其晶胞a=15.9552nm,b=7.6721nm,c=14.3311nm,β=98.0°。
通过MS Modeling软件对L-精氨酸α-酮戊二酸铜配合物的XRD谱图进行从头计算,通过对数据进行预处理、指标化、Pawley精修、空间群确定、结构测定以及Rietveld精修,最终得到了其具体的分子结构的信息。
In this paper, we used microwave solid reaction, liquid reaction and solid-liquid reaction to synthetize nine new bioinorganic complexes. In order to study the characterization, composition and structure information of the new complexes respectively, means of analysis methods have been used here, including elemental analysis, XRD analysis and calculation, IR, Raman spectra and the scanning electron microscope (SEM). The results are showed below: The complex of glycylglutamine and blue vitriol belongs to monoclinic system, and its molecular formula is (C7H13O4N3)2(CuSO4)·4.5H2O, with lattice parameters:a=11.6037 nm. b=8.3963 nm, c=5.6518nm,α=90.0°,β=99.1°,γ=90.0°; The complex of N-Acetyl-L-Glutamine and blue vitriol belongs to orthogonal system, and its molecular formula is (NH2COCH2CH2C(COOH)NHCOOH)2(CuSO4)·2.5H2O, with lattice parameters:a =16.4671nm, b=9.1700nm, c=7.6919nm,α=90.0°,β=90.0°,γ=90.0°; The complex of L-Arginine-α-ketoglutarate and copper hydroxide belongs to clinorhomboidal system, and its molecular formula is C17H38N8O11Cu·H2O, space group P-1, with lattice parameters:a= 9.0478nm, b=7.3516nm, c= 6.5809nm,α=111.6°,β=103.4°,γ=102.6°; The complex of L-Arginine-L-pyroglutamate and blue vitriol belongs to clinorhomboidal system, and its molecular formula is 5C6H17N4O7·2Cu, space group P1, with lattice parameters:a= 14.5805nm, b=11.8571 nm, c= 13.8994 nm,α=81.7°,β=117.4°,γ=199.4°; The complex of L-Arginine L-glutamate and zinc acetate belongs to orthogonal system, and its molecular formula is C11H24N2O16·Zn, space group P 21 21 21, with lattice parameters:a=11,1780nm, b=10.4598nm, c= 7.2161nm,α=90.0°,β=90.0°,γ=90.0°; The complex of L-lysine-L-apatate and copper hydroxide belongs to orthogonal system, and its molecular formula is C30H57N7O18·Cu12·20H2O, space group P 2 2 2, with lattice parameters:a=10.2930nm, b=16.1275nm, c= 9.2356nm,α=90.0°,β=90.0°,γ=90.0°; The complex of dimercaptosuccinic acid and bismuth trichloride belongs to monoclinic system, with lattice parameters:a= 1.4616nm, b=1.3629nm, c=1.3919nm,α=90.0°,β=130.5°,γ=90.0°; The complex of the complex of bismuth trichloride and ferrous sulphate belongs to orthogonal system, and its molecular formula is FeSO43.5H2O(C4H6O4S2), with lattice parameters:a=0.8044nm, b= 0.9813nm, c=2.1612 nm,α=90.8°,β=120.8°,γ=121.8°; The complex of nitrilotriacetic acid and blue vitriol belongs to monoclinic system, and its molecular formula is (CuSO4)2(C6H9O6N)7H2O, with lattice parameters:a=15.9552nm, b=7.6721nm, c=14.3311nm,α=90.0°,β=98.0°,γ=90.0°.
We used the MS Modeling software to get the ab initio structure solution from the XRD pattern of the complex of L-Arginine-a-ketoglutarate and copper hydroxide. The whole procedure contains pretreatment, indexing, Pawley refinement, identification of space group, structure solution and Rietveld refinement, and finally getting the accurate crystal structure.
引文
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