The title compound ethyl 1-（2-bromoethyl）-3-（4-methoxyphenyl）-1H-pyrazole-5-carboxylate 1 has been synthesized and structurally characterized by single-crystal X-ray diffraction.The crystal is of monoclinic（C15H1...The title compound ethyl 1-（2-bromoethyl）-3-（4-methoxyphenyl）-1H-pyrazole-5-carboxylate 1 has been synthesized and structurally characterized by single-crystal X-ray diffraction.The crystal is of monoclinic（C15H17BrN2O3,Mr = 353.22）,space group C21 with a = 24.691（7）,b = 6.7678（17）,c = 17.884（5） ,β = 97.184（5）o,V = 2965.1（13） 3,Z = 8,Dc = 1.583 g.cm-3,F（000） = 1440,μ = 2.784 mm-1,the final R = 0.0260 and wR = 0.0596 for 2684 observed reflections with I 2σ（I）.All the carbon atoms in the molecule are nearly coplanar except C（15）,with a large conjugated system among the carbonyl group,pyrazole ring and the benzene ring.Three non-classical intermolecular hydrogen bonds help to stabilize the crystal lattice.The regioselectivity was rationalized based on the coordination of potassium ion with the N-anion and the carbonyl oxygen atom.展开更多
A novel molecule tetra-N-alkylation of cyclen （1,4,7,10-tetraazacyclododecane）, 1,4,7,10-tetrakis（2-（（4-hydroxy）phenoxy）ethyl）-1,4,7,10-tetraazacyclododecane 2, was synthesized and structurally characterized b...A novel molecule tetra-N-alkylation of cyclen （1,4,7,10-tetraazacyclododecane）, 1,4,7,10-tetrakis（2-（（4-hydroxy）phenoxy）ethyl）-1,4,7,10-tetraazacyclododecane 2, was synthesized and structurally characterized by single-crystal X-ray diffraction. The molecule turned into chiral helical compound crystals grown from EtOH by slow diffusion at room temperature and three of the four hydroquinone groups of the benzene ring formed a g-electron-rich cavity by C-H…π stacking interaction. The crystal belongs to the monoclinic system, space group P21/C with a = 13.9192（9）, b = 13.2871（6）, c = 22.1894（15）A^°, β = 91.4600（10）°, V = 4102.5（4）A^°3, Z = 4, Dc = 1.219 g/cm^3, C40H52N4O8, Mr = 752.89, F（000） = 1616,μ = 0.088 mm^-1, MoKa radiation （λ = 0.71073）, R = 0.0578 and wR = 0.1389 for 5588 observed reflections with I 〉 2σ（I）. Moreover, compound 2 was characterized with ^1H NMR, ^13C NMR, IR spectra and MS.展开更多
The new compound 1,4,7,10-tetrakis-（2-（2,3-difluorophenyl） ethyl） -1,4,7,10-tetra-zacyclododecane 2 has been synthesized and structurally characterized by single-crystal X-ray diffraction. The molecule turned into...The new compound 1,4,7,10-tetrakis-（2-（2,3-difluorophenyl） ethyl） -1,4,7,10-tetra-zacyclododecane 2 has been synthesized and structurally characterized by single-crystal X-ray diffraction. The molecule turned into diamond crystals grown from CH3CN by slow diffusion at room temperature. It crystallizes in the triclinic system,space group P1^- with a = 9.543（2） ,b = 10.507（3） ,c = 10.734（3） A,α = 60.979（3） ,β = 81.870（4） ,γ = 84.279（4） o,V = 931.1（4） 3,Z = 1,Dc = 1.307 g/cm^3,C40H44F8N4,Mr = 732.79,F（000） = 384,μ = 0.105 mm^-1,T = 296（2） K,MoKa radiation（λ = 0.71073） ,R = 0.0494 and wR = 0.0989 for 1589 observed reflections with I 〉 2σ（I） . Hydrogen bonds and C-H···π stacking interactions in 2 contribute to a supramolecular structure. Moreover,compound 2 has been determined by ^1H NMR,^13C NMR,MS,IR spectra and elemental analysis.展开更多
A new pendant arms macrocyclic ligand, N, N'-bis(2-cyanoethyl)-3,4: 9, 10-dibenzo-1, 12-diaza-5, 8-dioxacyclopentadecane (L), was synthesized in goodyield (93% ) by alkylating 3, 4: 9, 10-dibenzo-1, 12-diaza-5, 8-...A new pendant arms macrocyclic ligand, N, N'-bis(2-cyanoethyl)-3,4: 9, 10-dibenzo-1, 12-diaza-5, 8-dioxacyclopentadecane (L), was synthesized in goodyield (93% ) by alkylating 3, 4: 9, 10-dibenzo-1, 12-diaza-5, 8-dioxacyclopentadecane(L') with acrylonitrile. Its crystal structure has been determined by X-ray diffraction.The ligand crystallizes in the orthorhombic system, space group Pbca, a=18. 143 (3),b=11. 206(2), c=22. 274(5)A, V=4528(2)A3, Mr=418. 55, Z= 8, F(000)=1792, Dc= 1. 228 gcm-3, T= 293K, μ= 7. 9 cm-1, final R=0.044 and Rw=0.067(w=1/(σ2 (F) + 0. 0005F2 ) ) based on 2291 independent reflections with F> 4. 0σ(F). The two benzene rings of the macrocyclic ligand are not in the same plane, andthe dihedral angle between them is 73. 6°, the molecule is in a folded state.展开更多
A series of rotenone O-alkyl oxime derivatives was designed and synthesized. Their structures were confirmed by elemental analyses, Fourier transform infrared（FTIR） and 1H NMR spectral studies, and the typical cryst...A series of rotenone O-alkyl oxime derivatives was designed and synthesized. Their structures were confirmed by elemental analyses, Fourier transform infrared（FTIR） and 1H NMR spectral studies, and the typical crystal structure of rotenone O-ethyl oxime（3b） was determined by X-ray diffraction. The preliminary biological activities of the new compounds were evaluated. The results of bioassays indicate that the title compounds exhibit moderate insecticidal and bactericidal activities. Among the synthesized compounds, compound 3q exhibited 90.0% mortality against M. separata at 1000 μg/mL. Compounds 3b and 3g exhibited both 90.0% inhibition rate against R. solani at 500 μg/mL, respectively.展开更多
A novel 1-D iodoplumbate hybrid, 2（Pb3I9）^3＊·3（C14H18N2）^2＋ 1, has been hydrothermally synthesized and characterized by IR spectra, TGA and single-crystal X-ray diffraction. Complex 1 crystallizes in monocl...A novel 1-D iodoplumbate hybrid, 2（Pb3I9）^3＊·3（C14H18N2）^2＋ 1, has been hydrothermally synthesized and characterized by IR spectra, TGA and single-crystal X-ray diffraction. Complex 1 crystallizes in monoclinic, space group P21/c, with a = 12.057（2）, b = 14.024（3）, c = 24.742（5） A, β = 90.48（3）°, V = 4183.6（14） A^3, Z = 4, R= 0.0477 and wR = 0.0800. The title compound consists of 1-D chains （Pb3I9）n^3n＊ parallel to the [100] direction and stacks of alkylated 4,4＇-bipyridium cations running along the [011] direction. Each anionic chain is surrounded by six arrays of alkylated 4,4＇-bipyridium cations through extensive C-H…I atypical hydrogen-bonding interactions to afford an interesting 3-D supramolecular network. Significant fluorescent property of the compound was observed at room temperature.展开更多
Reaction of (ArO)2Sm(THF)4 (ArO = 2,6-di- tert-butyl-4-methylphenolate) with Et2AlCl in THF gives SmCl2 (1) and (ArO)AlEt2(THF) (2) via ligand exchange. Complex 1 reacts with cyclooctatetraene (C8H8) to give [(C8H8)Sm...Reaction of (ArO)2Sm(THF)4 (ArO = 2,6-di- tert-butyl-4-methylphenolate) with Et2AlCl in THF gives SmCl2 (1) and (ArO)AlEt2(THF) (2) via ligand exchange. Complex 1 reacts with cyclooctatetraene (C8H8) to give [(C8H8)SmCl(THF)2]2(3).Crystal structural determinations show that compl 2 has a monomeric structure,the aluminum atom is coordinated by two carbon atoms and two oxygen atoms,to form a distorted tetrahedron. Complex 3 has a dimeric structure,the samarium atom is coordinated by a cyclooctatetraenyl ring,two chorine atoms and two oxygen atoms,the coordination number of the central metal is 9.展开更多
基金Supported by Scientific Technological project (2009GG20002027) in Shandong Province
文摘The title compound ethyl 1-（2-bromoethyl）-3-（4-methoxyphenyl）-1H-pyrazole-5-carboxylate 1 has been synthesized and structurally characterized by single-crystal X-ray diffraction.The crystal is of monoclinic（C15H17BrN2O3,Mr = 353.22）,space group C21 with a = 24.691（7）,b = 6.7678（17）,c = 17.884（5） ,β = 97.184（5）o,V = 2965.1（13） 3,Z = 8,Dc = 1.583 g.cm-3,F（000） = 1440,μ = 2.784 mm-1,the final R = 0.0260 and wR = 0.0596 for 2684 observed reflections with I 2σ（I）.All the carbon atoms in the molecule are nearly coplanar except C（15）,with a large conjugated system among the carbonyl group,pyrazole ring and the benzene ring.Three non-classical intermolecular hydrogen bonds help to stabilize the crystal lattice.The regioselectivity was rationalized based on the coordination of potassium ion with the N-anion and the carbonyl oxygen atom.
基金supported by the National Natural Science Foundation of China (20872051)
文摘A novel molecule tetra-N-alkylation of cyclen （1,4,7,10-tetraazacyclododecane）, 1,4,7,10-tetrakis（2-（（4-hydroxy）phenoxy）ethyl）-1,4,7,10-tetraazacyclododecane 2, was synthesized and structurally characterized by single-crystal X-ray diffraction. The molecule turned into chiral helical compound crystals grown from EtOH by slow diffusion at room temperature and three of the four hydroquinone groups of the benzene ring formed a g-electron-rich cavity by C-H…π stacking interaction. The crystal belongs to the monoclinic system, space group P21/C with a = 13.9192（9）, b = 13.2871（6）, c = 22.1894（15）A^°, β = 91.4600（10）°, V = 4102.5（4）A^°3, Z = 4, Dc = 1.219 g/cm^3, C40H52N4O8, Mr = 752.89, F（000） = 1616,μ = 0.088 mm^-1, MoKa radiation （λ = 0.71073）, R = 0.0578 and wR = 0.1389 for 5588 observed reflections with I 〉 2σ（I）. Moreover, compound 2 was characterized with ^1H NMR, ^13C NMR, IR spectra and MS.
基金supported by the National Natural Science Foundation of China (20872051)
文摘The new compound 1,4,7,10-tetrakis-（2-（2,3-difluorophenyl） ethyl） -1,4,7,10-tetra-zacyclododecane 2 has been synthesized and structurally characterized by single-crystal X-ray diffraction. The molecule turned into diamond crystals grown from CH3CN by slow diffusion at room temperature. It crystallizes in the triclinic system,space group P1^- with a = 9.543（2） ,b = 10.507（3） ,c = 10.734（3） A,α = 60.979（3） ,β = 81.870（4） ,γ = 84.279（4） o,V = 931.1（4） 3,Z = 1,Dc = 1.307 g/cm^3,C40H44F8N4,Mr = 732.79,F（000） = 384,μ = 0.105 mm^-1,T = 296（2） K,MoKa radiation（λ = 0.71073） ,R = 0.0494 and wR = 0.0989 for 1589 observed reflections with I 〉 2σ（I） . Hydrogen bonds and C-H···π stacking interactions in 2 contribute to a supramolecular structure. Moreover,compound 2 has been determined by ^1H NMR,^13C NMR,MS,IR spectra and elemental analysis.
文摘A new pendant arms macrocyclic ligand, N, N'-bis(2-cyanoethyl)-3,4: 9, 10-dibenzo-1, 12-diaza-5, 8-dioxacyclopentadecane (L), was synthesized in goodyield (93% ) by alkylating 3, 4: 9, 10-dibenzo-1, 12-diaza-5, 8-dioxacyclopentadecane(L') with acrylonitrile. Its crystal structure has been determined by X-ray diffraction.The ligand crystallizes in the orthorhombic system, space group Pbca, a=18. 143 (3),b=11. 206(2), c=22. 274(5)A, V=4528(2)A3, Mr=418. 55, Z= 8, F(000)=1792, Dc= 1. 228 gcm-3, T= 293K, μ= 7. 9 cm-1, final R=0.044 and Rw=0.067(w=1/(σ2 (F) + 0. 0005F2 ) ) based on 2291 independent reflections with F> 4. 0σ(F). The two benzene rings of the macrocyclic ligand are not in the same plane, andthe dihedral angle between them is 73. 6°, the molecule is in a folded state.
基金Supported by the National Science and Technology Pillar Program of China(No.2011BAE06B01)
文摘A series of rotenone O-alkyl oxime derivatives was designed and synthesized. Their structures were confirmed by elemental analyses, Fourier transform infrared（FTIR） and 1H NMR spectral studies, and the typical crystal structure of rotenone O-ethyl oxime（3b） was determined by X-ray diffraction. The preliminary biological activities of the new compounds were evaluated. The results of bioassays indicate that the title compounds exhibit moderate insecticidal and bactericidal activities. Among the synthesized compounds, compound 3q exhibited 90.0% mortality against M. separata at 1000 μg/mL. Compounds 3b and 3g exhibited both 90.0% inhibition rate against R. solani at 500 μg/mL, respectively.
基金supported by the Natural Science Foundation of Fujian Province (008 J0172)Innovation Project of Fujian Province (2007F3107)National Natural Science Foundation of China (20705031)
文摘A novel 1-D iodoplumbate hybrid, 2（Pb3I9）^3＊·3（C14H18N2）^2＋ 1, has been hydrothermally synthesized and characterized by IR spectra, TGA and single-crystal X-ray diffraction. Complex 1 crystallizes in monoclinic, space group P21/c, with a = 12.057（2）, b = 14.024（3）, c = 24.742（5） A, β = 90.48（3）°, V = 4183.6（14） A^3, Z = 4, R= 0.0477 and wR = 0.0800. The title compound consists of 1-D chains （Pb3I9）n^3n＊ parallel to the [100] direction and stacks of alkylated 4,4＇-bipyridium cations running along the [011] direction. Each anionic chain is surrounded by six arrays of alkylated 4,4＇-bipyridium cations through extensive C-H…I atypical hydrogen-bonding interactions to afford an interesting 3-D supramolecular network. Significant fluorescent property of the compound was observed at room temperature.
基金supported by the National Natural Science Foundation of China(Grant No.20072027).
文摘Reaction of (ArO)2Sm(THF)4 (ArO = 2,6-di- tert-butyl-4-methylphenolate) with Et2AlCl in THF gives SmCl2 (1) and (ArO)AlEt2(THF) (2) via ligand exchange. Complex 1 reacts with cyclooctatetraene (C8H8) to give [(C8H8)SmCl(THF)2]2(3).Crystal structural determinations show that compl 2 has a monomeric structure,the aluminum atom is coordinated by two carbon atoms and two oxygen atoms,to form a distorted tetrahedron. Complex 3 has a dimeric structure,the samarium atom is coordinated by a cyclooctatetraenyl ring,two chorine atoms and two oxygen atoms,the coordination number of the central metal is 9.
