4′-acetylbenzo-15-crown-5thiosemicarbazone was synthesized with high yield (94%)via the reaction of 4′-acetylbenzo-15-crown-5 and thiosemicarbazide under the microwave irradiation and hydrochloric acid as the cataly...4′-acetylbenzo-15-crown-5thiosemicarbazone was synthesized with high yield (94%)via the reaction of 4′-acetylbenzo-15-crown-5 and thiosemicarbazide under the microwave irradiation and hydrochloric acid as the catalyst.Its structure was determined by single-crystal X-ray diffraction.The crystal belongs to triclinic crystal system,P-1 space group,a=9.5470(19)?,b=13.637(3)?,c=16.029(3)?,α=75.33(3)°,β=83.62(3)°,γ=70.99(3)°,V=1097.8(7)s assembled into supramolecule structure by intermolecular hydrogen bonds.展开更多
以丙酸和硝基苯为混合溶剂,苯甲醛、对羟基苯甲醛和吡咯为原料合成了5-对羟基苯基-10,15,20-三苯基卟啉(HPTPP).然后以HPTPP和环氧氯丙烷为原料,在NaOH催化条件下合成了5-[4-(2,3-环氧丙氧基)苯基]-10,15,20-三苯基卟啉(EPPTPP).利用傅...以丙酸和硝基苯为混合溶剂,苯甲醛、对羟基苯甲醛和吡咯为原料合成了5-对羟基苯基-10,15,20-三苯基卟啉(HPTPP).然后以HPTPP和环氧氯丙烷为原料,在NaOH催化条件下合成了5-[4-(2,3-环氧丙氧基)苯基]-10,15,20-三苯基卟啉(EPPTPP).利用傅里叶变换红外光谱仪(FTIR)、核磁共振波谱仪(NMR)、紫外可见分光光度计(UV-Vis)和荧光分光光度计分别对HPTPP和EPPTPP的化学结构和光学性质进行了表征与测试.结果表明:FTIR谱图中,1 347cm-1和917cm-1处为EPPTPP卟啉环中C N键伸缩振动吸收峰和环氧化物环的(C—OC键)不对称伸缩振动吸收峰.EPPTPP的1 H NMR谱图中,在δ2.94～4.56内5个位移峰峰面积比为1∶1∶1∶1∶1,与EPPTPP中环氧基团的不同氢原子数比完全一致.UV-Vis谱图中,具有与卟啉结构相符合的吸收峰,表明成功合成了EPPTPP.通过荧光光谱分析了HPTPP和EPPTPP的荧光性质,并计算得到了二者的荧光量子产率分别为0.140和0.143.展开更多
The solid complex of lithium perchlorate with 4 tert butylbenzo 15 crown 5（4 t BB15C5） has been prepared in iodobenzene. The composition of the solid was determined as Li（4 t BB15C5）ClO 4 and its melting point was...The solid complex of lithium perchlorate with 4 tert butylbenzo 15 crown 5（4 t BB15C5） has been prepared in iodobenzene. The composition of the solid was determined as Li（4 t BB15C5）ClO 4 and its melting point was 119121 ℃. The far IR shift of the complex is obvious. The far IR absorption band of the complex containing 100% 6Li can be found by extrapolation, resolving the difficulty in obtaining a sample of 100% 6Li up to now. A relative reduced partition function ratio, [（ s/s′）f ] org , being 1.045 is calculated. Since the [ （s/s′）f ] aq of lithium perchlorate in solid state had been obtained as 1.025 and may act as that in aqueous phase, the phase equilibrium separation factor α may be obtained as 1.019 by the quotient of 1.045/1.025 for the extractive system of （4 t BB15C5） C 6H 5I/LiClO 4 H 2O. The value of α is just equal to the value of intrinsic separation factor （1+ ε p） described previously. [WT5HZ]展开更多
A new molybdophosphate, (NH3CH2CH2NH3)2Mo5O15(HPO4)2 has been synthesized under hydrothermal conditions and structurally characterized by single crystal X ray diffractions. The compound crystallizes in the monoclinic,...A new molybdophosphate, (NH3CH2CH2NH3)2Mo5O15(HPO4)2 has been synthesized under hydrothermal conditions and structurally characterized by single crystal X ray diffractions. The compound crystallizes in the monoclinic, space group C2/c, a=1.7633(2)nm, b=1.00122(11) nm, c=1.37624(13)nm, β=96.974(5)°, V=2.4117(5)nm3, Z=4, Dc=2.853g·cm-3, μ(MoKα)=2.766mm-1, F(000)=1992. The structure contains the isolated polyanions of [Mo5O15(HPO4)2]4- units around which the portonated ethylenediamine ions are pos itioned. By hydrogen bond interactions the polyanions are interconnected to form a three dimensional network. Other characterizations by powder XRD, IR and thermal analysis are also described. CCDC: 206321.展开更多
采用固相烧结法制备铋层结构Na 0.5 Bi 4.5 Ta x Ti 4-x O 15+0.5 x(NBT-Ta-x)(x=0~0.20)压电陶瓷。采用X射线衍射、扫描电镜和自动控温测试系统研究Ta 5+的B位掺杂对NBT-Ta-x陶瓷的微观结构、电导、介电和压电性能的影响。结果表明:随T...采用固相烧结法制备铋层结构Na 0.5 Bi 4.5 Ta x Ti 4-x O 15+0.5 x(NBT-Ta-x)(x=0~0.20)压电陶瓷。采用X射线衍射、扫描电镜和自动控温测试系统研究Ta 5+的B位掺杂对NBT-Ta-x陶瓷的微观结构、电导、介电和压电性能的影响。结果表明:随Ta掺杂量的增加,晶粒尺寸和长径比逐渐减小,表现出沿c轴的取向生长,同时,陶瓷的理论密度和体积密度增加,在掺杂量x=0.05时达到最高的相对密度96.1%,Ta在NBT晶格中的固溶极限在0.10附近。随Ta 5+掺杂量x增加到0.20,陶瓷的居里温度从680℃降至658℃。Ta 5+掺杂使NBT-Ta-x陶瓷的电阻率增加了两个数量级,压电常数d 33从13.8 pC/N增加到23 pC/N。当x=0.04~0.05时,NBT-Ta-x陶瓷的综合电性能良好:T c=670~672℃,d 33=21.8~23 pC/N,k p=7.9%~8.3%。展开更多
The complex dimethylgallium- [4-nitro-2- (N-benzo- 15-crown-5 ) - 1 -phenoxide ] (C23H31 N2O7Ga) has been synthesized by the method reported. The crystal X-ray diffraction analysis shows that the crystal belongs to th...The complex dimethylgallium- [4-nitro-2- (N-benzo- 15-crown-5 ) - 1 -phenoxide ] (C23H31 N2O7Ga) has been synthesized by the method reported. The crystal X-ray diffraction analysis shows that the crystal belongs to the triclinic with space group P1, M = 517. 23 and the unit cell parameters: a = 1. 4501 (2), b = 1. 5090(2), c = 1. 3865 (6)nm, a = 105. 58(1 ), β = 117. 26(2), γ = 66. 812(8)°, V= 2. 464546nm3, Z =4, Dc = 1. 39g· cm-3, u = 11. 6cm-1, F(000) = 1080, R = 0. 051, Rw = 0. 064. The coordination number of Ga is four and the gallium atom is located in a distorted tetrahedron structure.展开更多
文摘4′-acetylbenzo-15-crown-5thiosemicarbazone was synthesized with high yield (94%)via the reaction of 4′-acetylbenzo-15-crown-5 and thiosemicarbazide under the microwave irradiation and hydrochloric acid as the catalyst.Its structure was determined by single-crystal X-ray diffraction.The crystal belongs to triclinic crystal system,P-1 space group,a=9.5470(19)?,b=13.637(3)?,c=16.029(3)?,α=75.33(3)°,β=83.62(3)°,γ=70.99(3)°,V=1097.8(7)s assembled into supramolecule structure by intermolecular hydrogen bonds.
文摘以丙酸和硝基苯为混合溶剂,苯甲醛、对羟基苯甲醛和吡咯为原料合成了5-对羟基苯基-10,15,20-三苯基卟啉(HPTPP).然后以HPTPP和环氧氯丙烷为原料,在NaOH催化条件下合成了5-[4-(2,3-环氧丙氧基)苯基]-10,15,20-三苯基卟啉(EPPTPP).利用傅里叶变换红外光谱仪(FTIR)、核磁共振波谱仪(NMR)、紫外可见分光光度计(UV-Vis)和荧光分光光度计分别对HPTPP和EPPTPP的化学结构和光学性质进行了表征与测试.结果表明:FTIR谱图中,1 347cm-1和917cm-1处为EPPTPP卟啉环中C N键伸缩振动吸收峰和环氧化物环的(C—OC键)不对称伸缩振动吸收峰.EPPTPP的1 H NMR谱图中,在δ2.94～4.56内5个位移峰峰面积比为1∶1∶1∶1∶1,与EPPTPP中环氧基团的不同氢原子数比完全一致.UV-Vis谱图中,具有与卟啉结构相符合的吸收峰,表明成功合成了EPPTPP.通过荧光光谱分析了HPTPP和EPPTPP的荧光性质,并计算得到了二者的荧光量子产率分别为0.140和0.143.
文摘The solid complex of lithium perchlorate with 4 tert butylbenzo 15 crown 5（4 t BB15C5） has been prepared in iodobenzene. The composition of the solid was determined as Li（4 t BB15C5）ClO 4 and its melting point was 119121 ℃. The far IR shift of the complex is obvious. The far IR absorption band of the complex containing 100% 6Li can be found by extrapolation, resolving the difficulty in obtaining a sample of 100% 6Li up to now. A relative reduced partition function ratio, [（ s/s′）f ] org , being 1.045 is calculated. Since the [ （s/s′）f ] aq of lithium perchlorate in solid state had been obtained as 1.025 and may act as that in aqueous phase, the phase equilibrium separation factor α may be obtained as 1.019 by the quotient of 1.045/1.025 for the extractive system of （4 t BB15C5） C 6H 5I/LiClO 4 H 2O. The value of α is just equal to the value of intrinsic separation factor （1+ ε p） described previously. [WT5HZ]
文摘A new molybdophosphate, (NH3CH2CH2NH3)2Mo5O15(HPO4)2 has been synthesized under hydrothermal conditions and structurally characterized by single crystal X ray diffractions. The compound crystallizes in the monoclinic, space group C2/c, a=1.7633(2)nm, b=1.00122(11) nm, c=1.37624(13)nm, β=96.974(5)°, V=2.4117(5)nm3, Z=4, Dc=2.853g·cm-3, μ(MoKα)=2.766mm-1, F(000)=1992. The structure contains the isolated polyanions of [Mo5O15(HPO4)2]4- units around which the portonated ethylenediamine ions are pos itioned. By hydrogen bond interactions the polyanions are interconnected to form a three dimensional network. Other characterizations by powder XRD, IR and thermal analysis are also described. CCDC: 206321.
文摘采用固相烧结法制备铋层结构Na 0.5 Bi 4.5 Ta x Ti 4-x O 15+0.5 x(NBT-Ta-x)(x=0~0.20)压电陶瓷。采用X射线衍射、扫描电镜和自动控温测试系统研究Ta 5+的B位掺杂对NBT-Ta-x陶瓷的微观结构、电导、介电和压电性能的影响。结果表明:随Ta掺杂量的增加,晶粒尺寸和长径比逐渐减小,表现出沿c轴的取向生长,同时,陶瓷的理论密度和体积密度增加,在掺杂量x=0.05时达到最高的相对密度96.1%,Ta在NBT晶格中的固溶极限在0.10附近。随Ta 5+掺杂量x增加到0.20,陶瓷的居里温度从680℃降至658℃。Ta 5+掺杂使NBT-Ta-x陶瓷的电阻率增加了两个数量级,压电常数d 33从13.8 pC/N增加到23 pC/N。当x=0.04~0.05时,NBT-Ta-x陶瓷的综合电性能良好:T c=670~672℃,d 33=21.8~23 pC/N,k p=7.9%~8.3%。
文摘The complex dimethylgallium- [4-nitro-2- (N-benzo- 15-crown-5 ) - 1 -phenoxide ] (C23H31 N2O7Ga) has been synthesized by the method reported. The crystal X-ray diffraction analysis shows that the crystal belongs to the triclinic with space group P1, M = 517. 23 and the unit cell parameters: a = 1. 4501 (2), b = 1. 5090(2), c = 1. 3865 (6)nm, a = 105. 58(1 ), β = 117. 26(2), γ = 66. 812(8)°, V= 2. 464546nm3, Z =4, Dc = 1. 39g· cm-3, u = 11. 6cm-1, F(000) = 1080, R = 0. 051, Rw = 0. 064. The coordination number of Ga is four and the gallium atom is located in a distorted tetrahedron structure.
