A Cd(Ⅱ) seven-coordinate dimmer [Cd(3,5-Me2PhCO2)2(phen)]2 has been synthesized with 3,5-dimethyl-benzoic acid and 1,10-phenanthroline.The crystal structure was determined by single-crystal X-ray diffraction.The crys...A Cd(Ⅱ) seven-coordinate dimmer [Cd(3,5-Me2PhCO2)2(phen)]2 has been synthesized with 3,5-dimethyl-benzoic acid and 1,10-phenanthroline.The crystal structure was determined by single-crystal X-ray diffraction.The crystal belongs to monoclinic system,space group C2/c with a=2.939 8(6) nm,b=1.032 9(2) nm,c=2.106 6(4) nm,β=125.423(3) °.The crystal structure shows that the cadmium ion is coordinated with five oxygen atoms and two nitrogen atoms,forming a distorted capped octahedral coordination geometry.There exist two types of coordinated 3,5-dimethylbenzoic carboxylic anions:the tridentate-chelating-bridging ones and the bidentate-chelating ones.The Cd(Ⅱ) …Cd(Ⅱ) distance is 0.395 7 nm.The result of TG analysis shows that the title complex was stable under 300.0 ℃.CCDC:694570.展开更多
本文通过X-射线粉末衍射仪(PXRD)对利伐沙班混晶中的晶型Ⅰ和晶型Ⅱ进行了定性与定量分析,利用差示扫描量热仪(DSC)结合X射线粉末衍射仪原位高温附件(in situ high temperature)测定了晶型Ⅱ的热稳定性.定量分析采用X射线粉末衍射K值法...本文通过X-射线粉末衍射仪(PXRD)对利伐沙班混晶中的晶型Ⅰ和晶型Ⅱ进行了定性与定量分析,利用差示扫描量热仪(DSC)结合X射线粉末衍射仪原位高温附件(in situ high temperature)测定了晶型Ⅱ的热稳定性.定量分析采用X射线粉末衍射K值法,结果表明:该方法具有方便快速,简单实用的优点;热分析表明晶型Ⅱ在190℃左右发生相转变,逐步转变为晶型Ⅰ.展开更多
The binuclear Zn(Ⅱ) complex [Zn2(L)2(Mf)2] with 2-hydroxyacetophenone benzoylhydrazone(H2L) and monodentate N-heterocycle,morphine(Mf) has been synthesized and characterized by elemental analysis,IR,UV,molar conducti...The binuclear Zn(Ⅱ) complex [Zn2(L)2(Mf)2] with 2-hydroxyacetophenone benzoylhydrazone(H2L) and monodentate N-heterocycle,morphine(Mf) has been synthesized and characterized by elemental analysis,IR,UV,molar conductivity,TG and X-ray diffraction structural analysis.Crystal data: monoclinic,space group P21/n with a=1.263 9(6) nm,b=1.085 2(4) nm,c=1.313 4(5) nm,β=92.16(2)°,V=1.800(1) nm3,Z=2,Dc=1.493 g.cm-3,μ= 1.388 mm-1,F(000) =840,and final R =0.038 4,wR =0.087 9.The two Zn (Ⅱ) centers in the centrosymmetric binuclear complex are bridged by phenolic oxygen atoms with Zn…Zn separation of 0.315 0(1) nm.The coordina-tion geometry of each Zn(Ⅱ) atom is trigonal bipyramidal.The fluorescence activities of ligand and the complex were also studied.展开更多
为开发高温释放型烟用香料添加剂,本研究以2,3-吡嗪二羧酸和薄荷醇为原料,N,N′-二环己基碳酰亚胺（DCC）为缩合剂,4-二甲氨基吡啶（DMAP）为催化剂,经酯化反应制备了新型潜香目标化合物2,3-吡嗪二羧酸薄荷醇酯。该化合物经X射线单晶衍...为开发高温释放型烟用香料添加剂,本研究以2,3-吡嗪二羧酸和薄荷醇为原料,N,N′-二环己基碳酰亚胺（DCC）为缩合剂,4-二甲氨基吡啶（DMAP）为催化剂,经酯化反应制备了新型潜香目标化合物2,3-吡嗪二羧酸薄荷醇酯。该化合物经X射线单晶衍射、核磁共振波谱（1 H NMR,13 C NMR）、红外光谱（IR）和高分辨质谱（HRMS）表征后,结合同步热稳定性分析,采用在线热裂解-气相色谱/质谱（Py-GC/MS）法对裂解产物进行定性和半定量分析,并初步推测了其可能的裂解机理。结果表明：在主要热失重区间268.5~334.9℃范围内,目标化合物基本分解完全,熔融温度为140.9℃,裂解温度为315.9℃;共鉴定出目标化合物的46种裂解产物,主要有薄荷烯、薄荷醇和吡嗪等多种对烟草香味有重要作用的致香成分。该方法能够方便、快速地分离鉴定高温食品香料添加剂的热裂解产物,可为该添加剂在烟草中的加香应用提供理论参考。展开更多
文摘A Cd(Ⅱ) seven-coordinate dimmer [Cd(3,5-Me2PhCO2)2(phen)]2 has been synthesized with 3,5-dimethyl-benzoic acid and 1,10-phenanthroline.The crystal structure was determined by single-crystal X-ray diffraction.The crystal belongs to monoclinic system,space group C2/c with a=2.939 8(6) nm,b=1.032 9(2) nm,c=2.106 6(4) nm,β=125.423(3) °.The crystal structure shows that the cadmium ion is coordinated with five oxygen atoms and two nitrogen atoms,forming a distorted capped octahedral coordination geometry.There exist two types of coordinated 3,5-dimethylbenzoic carboxylic anions:the tridentate-chelating-bridging ones and the bidentate-chelating ones.The Cd(Ⅱ) …Cd(Ⅱ) distance is 0.395 7 nm.The result of TG analysis shows that the title complex was stable under 300.0 ℃.CCDC:694570.
文摘本文通过X-射线粉末衍射仪(PXRD)对利伐沙班混晶中的晶型Ⅰ和晶型Ⅱ进行了定性与定量分析,利用差示扫描量热仪(DSC)结合X射线粉末衍射仪原位高温附件(in situ high temperature)测定了晶型Ⅱ的热稳定性.定量分析采用X射线粉末衍射K值法,结果表明:该方法具有方便快速,简单实用的优点;热分析表明晶型Ⅱ在190℃左右发生相转变,逐步转变为晶型Ⅰ.
文摘The binuclear Zn(Ⅱ) complex [Zn2(L)2(Mf)2] with 2-hydroxyacetophenone benzoylhydrazone(H2L) and monodentate N-heterocycle,morphine(Mf) has been synthesized and characterized by elemental analysis,IR,UV,molar conductivity,TG and X-ray diffraction structural analysis.Crystal data: monoclinic,space group P21/n with a=1.263 9(6) nm,b=1.085 2(4) nm,c=1.313 4(5) nm,β=92.16(2)°,V=1.800(1) nm3,Z=2,Dc=1.493 g.cm-3,μ= 1.388 mm-1,F(000) =840,and final R =0.038 4,wR =0.087 9.The two Zn (Ⅱ) centers in the centrosymmetric binuclear complex are bridged by phenolic oxygen atoms with Zn…Zn separation of 0.315 0(1) nm.The coordina-tion geometry of each Zn(Ⅱ) atom is trigonal bipyramidal.The fluorescence activities of ligand and the complex were also studied.
文摘为开发高温释放型烟用香料添加剂,本研究以2,3-吡嗪二羧酸和薄荷醇为原料,N,N′-二环己基碳酰亚胺（DCC）为缩合剂,4-二甲氨基吡啶（DMAP）为催化剂,经酯化反应制备了新型潜香目标化合物2,3-吡嗪二羧酸薄荷醇酯。该化合物经X射线单晶衍射、核磁共振波谱（1 H NMR,13 C NMR）、红外光谱（IR）和高分辨质谱（HRMS）表征后,结合同步热稳定性分析,采用在线热裂解-气相色谱/质谱（Py-GC/MS）法对裂解产物进行定性和半定量分析,并初步推测了其可能的裂解机理。结果表明：在主要热失重区间268.5~334.9℃范围内,目标化合物基本分解完全,熔融温度为140.9℃,裂解温度为315.9℃;共鉴定出目标化合物的46种裂解产物,主要有薄荷烯、薄荷醇和吡嗪等多种对烟草香味有重要作用的致香成分。该方法能够方便、快速地分离鉴定高温食品香料添加剂的热裂解产物,可为该添加剂在烟草中的加香应用提供理论参考。
