The title compound [Zn(Py) 2L] n(L=1,2′-ferrocenedicarboxylate) was synthesized under mild conditions and its crystal structure was characterized. It crystallizes in a monoclinic system, space group C2/c with the cel...The title compound [Zn(Py) 2L] n(L=1,2′-ferrocenedicarboxylate) was synthesized under mild conditions and its crystal structure was characterized. It crystallizes in a monoclinic system, space group C2/c with the cell parameters a=1.683 0(5) nm, b=1.380 4(3) nm, c=1.746 2(3) nm, β=108.78(2)°, V=3.840 8(15) nm 3, Z=8, M r=485.52, T=293(2) K, D c=3.359 Mg/m 3, μ= 4.073 mm -1, F(000)=3 872, R 1=0.040 1, wR 2=0.113 2. The compound exhibits an unusual one-dimensional chain consisting of two zigzag chains.展开更多
目的:建立一种分离苯磺酸氨氯地平外消旋体的方法。方法:先合成手性金属-有机骨架材料[Zn_2(D-Cam)_2(4,4′-bpy)]_n(简称为Zn-MOF)并对其进行X射线粉末衍射表征,由其与GF254硅胶混合制备薄层色谱固定相后用于分离苯磺酸氨氯地平外消旋...目的:建立一种分离苯磺酸氨氯地平外消旋体的方法。方法:先合成手性金属-有机骨架材料[Zn_2(D-Cam)_2(4,4′-bpy)]_n(简称为Zn-MOF)并对其进行X射线粉末衍射表征,由其与GF254硅胶混合制备薄层色谱固定相后用于分离苯磺酸氨氯地平外消旋体;以两个对映体的比移值和分离度为指标优选分离条件(展开剂组成及比例、手性Zn-MOF的用量等)并进行方法的重现性试验。结果:成功合成了手性Zn-MOF材料并经表征证实;优选的分离条件为取0.10 g手性Zn-MOF混合1.5 g GF254硅胶制备薄层色谱板、展开剂为乙腈-仲丁醇(30∶70,V/V)。在此条件下,苯磺酸氨氯地平外消旋体实现了有效分离,所得斑点大小均一,比移值>0.27,分离度约为2(RSD=3.8%,n=3)。结论:由手性Zn-MOF制备的薄层色谱固定相对苯磺酸氨氯地平外消旋体具有较好的手性识别能力,且其分离方法操作简单,结果直观、准确、重现性好。展开更多
A new zinc hydrogen phosphite C4H8N2H4·Zn（HPO3）2 was prepared by hydrothermal method in the presence of piperazine as a structure-directing agent and the crystal structure was determined by single-crystal X-ray...A new zinc hydrogen phosphite C4H8N2H4·Zn（HPO3）2 was prepared by hydrothermal method in the presence of piperazine as a structure-directing agent and the crystal structure was determined by single-crystal X-ray diffraction analysis and further characterized by X-ray powder diffraction, IR, ICP, elemental analysis and TG analysis. This compound has one-dimensional anionic chains containing four-membered rings built from corner-sharing linked alternating ZnO4 tetrahedra and HPO3 pseudo pyramids. The zinc hydrogen phosphite chains are interacted with the templates of diprotonated piperazine by N—H…O hydrogen bond. Crystal data for C4H8N2H4·Zn（HPO3）2∶monoclinic, space group C2/c. a=1.774 8（2） nm, b=0.724 28（9） nm, c=0.880 87（11） nm, β= 105.345（3）°, V=1.091 9（2） nm 3, Z=4, Dc=1^907 Mg/m 3, R1=0.022 9, wR2=0.058 8.展开更多
文摘The title compound [Zn(Py) 2L] n(L=1,2′-ferrocenedicarboxylate) was synthesized under mild conditions and its crystal structure was characterized. It crystallizes in a monoclinic system, space group C2/c with the cell parameters a=1.683 0(5) nm, b=1.380 4(3) nm, c=1.746 2(3) nm, β=108.78(2)°, V=3.840 8(15) nm 3, Z=8, M r=485.52, T=293(2) K, D c=3.359 Mg/m 3, μ= 4.073 mm -1, F(000)=3 872, R 1=0.040 1, wR 2=0.113 2. The compound exhibits an unusual one-dimensional chain consisting of two zigzag chains.
文摘目的:建立一种分离苯磺酸氨氯地平外消旋体的方法。方法:先合成手性金属-有机骨架材料[Zn_2(D-Cam)_2(4,4′-bpy)]_n(简称为Zn-MOF)并对其进行X射线粉末衍射表征,由其与GF254硅胶混合制备薄层色谱固定相后用于分离苯磺酸氨氯地平外消旋体;以两个对映体的比移值和分离度为指标优选分离条件(展开剂组成及比例、手性Zn-MOF的用量等)并进行方法的重现性试验。结果:成功合成了手性Zn-MOF材料并经表征证实;优选的分离条件为取0.10 g手性Zn-MOF混合1.5 g GF254硅胶制备薄层色谱板、展开剂为乙腈-仲丁醇(30∶70,V/V)。在此条件下,苯磺酸氨氯地平外消旋体实现了有效分离,所得斑点大小均一,比移值>0.27,分离度约为2(RSD=3.8%,n=3)。结论:由手性Zn-MOF制备的薄层色谱固定相对苯磺酸氨氯地平外消旋体具有较好的手性识别能力,且其分离方法操作简单,结果直观、准确、重现性好。
文摘A new zinc hydrogen phosphite C4H8N2H4·Zn（HPO3）2 was prepared by hydrothermal method in the presence of piperazine as a structure-directing agent and the crystal structure was determined by single-crystal X-ray diffraction analysis and further characterized by X-ray powder diffraction, IR, ICP, elemental analysis and TG analysis. This compound has one-dimensional anionic chains containing four-membered rings built from corner-sharing linked alternating ZnO4 tetrahedra and HPO3 pseudo pyramids. The zinc hydrogen phosphite chains are interacted with the templates of diprotonated piperazine by N—H…O hydrogen bond. Crystal data for C4H8N2H4·Zn（HPO3）2∶monoclinic, space group C2/c. a=1.774 8（2） nm, b=0.724 28（9） nm, c=0.880 87（11） nm, β= 105.345（3）°, V=1.091 9（2） nm 3, Z=4, Dc=1^907 Mg/m 3, R1=0.022 9, wR2=0.058 8.
