Two new macrocyclic compounds, [Cu2（L）2]（ClO4）4·2CH3OH （1） and [Cu（L）]（ClO4）2·2H2O （2） （L = 1,3,10,12,15,18-hexaazatetracyclodocosane） were synthesized by condensation reactions involving amine...Two new macrocyclic compounds, [Cu2（L）2]（ClO4）4·2CH3OH （1） and [Cu（L）]（ClO4）2·2H2O （2） （L = 1,3,10,12,15,18-hexaazatetracyclodocosane） were synthesized by condensation reactions involving amines and formaldehyde in the presence of copper anion. Compound 1 crystallizes in triclinic, space group Pí with a = 10.442（2）, b = 14.197（3）, c = 17.388（4）, α = 91.218（4）, β = 90.69（3）, γ = 93.756（4）o, V = 2520.4（9）3, Z = 2, F（000） = 1260, Dc = 1.589 Mg/m3, Mr = 1205.92, μ = 1.137 mm-1, λ = 0.71073, the final R = 0.0668 and wR = 0.1573 for 9703 observed reflections with I 2σ（I）. Compound 2 crystallizes in monoclinic, space group C2/c with a = 16.911（2）, b = 11.4172（15）, c = 27.059（4）, β = 107.787（2）o, V = 4974.7（12）3, Z = 8, F（000） = 2504, Dc = 1.610 Mg/m3, Mr = 602.92, μ = 1.155 mm-1, λ = 0.71073, the final R = 0.0419 and wR = 0.1131 for 4374 observed reflections with I 2σ（I）.展开更多
The crystal structure of copper(Ⅱ) complex with a new 14-membered tetraazamacrocyclic ligand 5,5,7,12,12,14-hexamethy1-1,4,8,11-tetraazacyclotetradecane-N'N'-diacetic acid,[CuC16N4H34(CH2COO)(CH2COOH)]·C...The crystal structure of copper(Ⅱ) complex with a new 14-membered tetraazamacrocyclic ligand 5,5,7,12,12,14-hexamethy1-1,4,8,11-tetraazacyclotetradecane-N'N'-diacetic acid,[CuC16N4H34(CH2COO)(CH2COOH)]·ClO4·0. 5HCIO4·1. 5H2O was determined. Crystallographic data: Mr = 639.22,orthorhombic, space group Pcnb with a=11.743(4),b=16.446(2),c=29.611 (4) A,Z=8,V=5726(3) A3, Dc=1.482 g·cm-3, F(000)=1344,μ=9. 64 cm-1,R=0.063,and Rw=0.067 for 2386 reflections with I≥3σ(I). The structure shows an unusual configuration in which two carboxyl groups were bonded to two neighboring nitrogen atoms of the macrocycle, N1 and N4, and six methyl substituents occur on one side of the macrocycle, while two carboxyl groups on the other side, and central copper(Ⅱ) ion forms a five-coordinated geometry.展开更多
The title compound 1,4,23,26,29,48-hexaaza-6,9:16,19:31,34:41,44-tetrabenzo-12, 15,37,40-tetraoxa-cyclodotetracontane-4,5,18,19,25,26,39,40-octaene 1 (C40H46N6O4) was synthe- sized by [2+2] condensation of diethylenet...The title compound 1,4,23,26,29,48-hexaaza-6,9:16,19:31,34:41,44-tetrabenzo-12, 15,37,40-tetraoxa-cyclodotetracontane-4,5,18,19,25,26,39,40-octaene 1 (C40H46N6O4) was synthe- sized by [2+2] condensation of diethylenetriamine with 4,4?diformyl-diphenoxyethane (dialdehyde) in a mixed solvent of ethanol and tetrahydrofuran. The crystal data are: Mr = 674.83, triclinic, P, a = 5.8249(1), b = 9.4114(8), c = 17.649(2) ? a = 79.310(7), b = 85.397(4), g = 78.970(8), V = 932.1(1) ?, Z = 1, Dc = 1.202 g/cm3, F(000) = 360, m(MoKa) = 0.079 mm-1, R = 0.0486 and wR = 0.1439. The title molecule has a crystallographic center symmetry. The distance between the two secondary amine nitrogen atoms is 18.890(3) ?展开更多
A mixed-valence dinuclear manganese complex, [Mn ⅡMn ⅢL](ClO 4)·1/2MeOH, where L is a macrocyclic ligand derived from the cyclocondensation of sodium 2,6-diformyl-4-methylphenolate with N,N-bis(2-aminoethyl)...A mixed-valence dinuclear manganese complex, [Mn ⅡMn ⅢL](ClO 4)·1/2MeOH, where L is a macrocyclic ligand derived from the cyclocondensation of sodium 2,6-diformyl-4-methylphenolate with N,N-bis(2-aminoethyl)-2-hydroxybenzyl amine, was obtained and its structure was determined by X-ray diffraction. The orange crystal is a monoclinic system with space group P2 1/c and lattice parameters a=1.1617(4), b=1.4005(3), c=1.4641(3) nm, β=113.03(2)°, and Z=2. The crystal structure shows that each pendant-arm is bonded in a bidentate fashion to the adjacent metal atom and that both the arms are on the same side of the macrocycle. The two Mn atoms are bridged by two μ 2-phenoxy oxygen atoms of the tetra-imine macrocycle, and each Mn atom, locating in a trigonal prismatic coordination environment(N 3O 3), is six-coordinated by the two imine nitrogen atoms, one tertiary nitrogen atom and a pendant phenol moiety apart from the two oxygen atoms.展开更多
The title compound, (C 34 H 54 N 2O 10 )[Eu(NO 3) 5](C 34 H 52 N 2O 10 =1,2 bis(2,3 benzo 10 aza 15 crown 5 N ethyleneoxy)ethane), was synthesized in acetonitrile solution and its ...The title compound, (C 34 H 54 N 2O 10 )[Eu(NO 3) 5](C 34 H 52 N 2O 10 =1,2 bis(2,3 benzo 10 aza 15 crown 5 N ethyleneoxy)ethane), was synthesized in acetonitrile solution and its crystal structure was determined by X ray analysis. The crystal crystallizes in monoclinic, space group P21/c with cell parameters a =1 1801(2) nm, b =2 3560(5) nm, c =1 7025(3) nm, β =99 67(3)°, V =4 6662(16) nm 3, Z =4, D c=1 581 g/cm 3. The europium ion is coordinated with ten oxygen atoms from five nitrato groups, and neither O atoms nor N atoms of the macrocyclic compound are bonded to the europium ion.展开更多
Crystal structure of nickel（II） complex with a new 14 membered tetraazamacrocyclic ligand 5,12-diphenyl-7,14-dimethyl-1,4,8,11-tetraazacyclotetradecane-N’,N-diacetic acid,Ni[N<sub>4</sub>C<sub>10&...Crystal structure of nickel（II） complex with a new 14 membered tetraazamacrocyclic ligand 5,12-diphenyl-7,14-dimethyl-1,4,8,11-tetraazacyclotetradecane-N’,N-diacetic acid,Ni[N<sub>4</sub>C<sub>10</sub>（CH<sub>2</sub>COO）<sub>2</sub>（C<sub>6</sub>H<sub>5</sub>）<sub>2</sub>]·2H<sub>2</sub>O, M<sub>r</sub>= 589. 38 is reported.It crystallizes in monoclinic P2<sub>1</sub>/c space group with a=12.949（6）,b=16.373（3）,c=14.232（16）,β=98.68（6）°,V=2982.9（7）,Z=4,D<sub>c</sub>=1.312 gcm-3,μ=6.953 cm-1,F（000）=1256.0.Finally,the structure was refined to R=0.080,R<sub>w</sub>=0.065 for 2952 reflections.The central nickel ion of the complex forms an octahedron with four nitrogen atoms of the macrocycle and two oxygen atoms of the appended carboxylate groups.Two phenyl planes of the ligand are almost parallel to each other.展开更多
The title compound C（15）H（14）N4OS·H<sub>2</sub>O crystallizes in the monoclinic system, space group P21/a, with a=8. 733（3） , b= 16. 731 （4） , c=10. 476（4） A,β= 95. 41（3） °, V = 1523...The title compound C（15）H（14）N4OS·H<sub>2</sub>O crystallizes in the monoclinic system, space group P21/a, with a=8. 733（3） , b= 16. 731 （4） , c=10. 476（4） A,β= 95. 41（3） °, V = 1523. 7（8） A￣3, D<sub>c</sub>=1. 38 g/cm￣3, Z = 4,Mr= 316. 38,λ（MoKα） = 0. 71069 A, F（000） = 664,μ= 2.14 cm-1, T= 296K. Final R=0. 054,and Rω=0.063 for 1279 reflections with I≥3σ（I）. The parent structure of the molecule is a distorted six-membered ring. The effect of the steric hindrance between the two phenyls on the conjugate interactions in the heterocyclic ring has been discussed.展开更多
The title compound （E）-ethyl 2-fluoro-2-（3-oxoisobenzofuran-1（3H）-ylidene） aceta- te was synthesized as an unexpected product by the reaction ofphthalyl dichloride with bis-silylenol ether, which is not in accor...The title compound （E）-ethyl 2-fluoro-2-（3-oxoisobenzofuran-1（3H）-ylidene） aceta- te was synthesized as an unexpected product by the reaction ofphthalyl dichloride with bis-silylenol ether, which is not in accordance with our previous studies. The title compound was characterized by single-crystal X-ray diffraction, 1H NMR, 13C NMR, 19F NMR, GCMS, HRMS and IR. The crystal （C12HgFO4, Mr = 236.19） belongs to the monoclinic system, space group P21/c, a = 19.1609（8）, b = 7.9831（3）, c = 13.7715（6） A, V= 2106.13（15） A3, Z= 8, Dx = 1.490 Mg m-3, MoKa radiation, 2 = 0.71073 A,μ = 0.12 mm-1, F（000） = 976, the final R = 0.025 and wR = 0.1300 for 4505 observed reflections with I〉 2σ（I）.展开更多
文摘Two new macrocyclic compounds, [Cu2（L）2]（ClO4）4·2CH3OH （1） and [Cu（L）]（ClO4）2·2H2O （2） （L = 1,3,10,12,15,18-hexaazatetracyclodocosane） were synthesized by condensation reactions involving amines and formaldehyde in the presence of copper anion. Compound 1 crystallizes in triclinic, space group Pí with a = 10.442（2）, b = 14.197（3）, c = 17.388（4）, α = 91.218（4）, β = 90.69（3）, γ = 93.756（4）o, V = 2520.4（9）3, Z = 2, F（000） = 1260, Dc = 1.589 Mg/m3, Mr = 1205.92, μ = 1.137 mm-1, λ = 0.71073, the final R = 0.0668 and wR = 0.1573 for 9703 observed reflections with I 2σ（I）. Compound 2 crystallizes in monoclinic, space group C2/c with a = 16.911（2）, b = 11.4172（15）, c = 27.059（4）, β = 107.787（2）o, V = 4974.7（12）3, Z = 8, F（000） = 2504, Dc = 1.610 Mg/m3, Mr = 602.92, μ = 1.155 mm-1, λ = 0.71073, the final R = 0.0419 and wR = 0.1131 for 4374 observed reflections with I 2σ（I）.
文摘The crystal structure of copper(Ⅱ) complex with a new 14-membered tetraazamacrocyclic ligand 5,5,7,12,12,14-hexamethy1-1,4,8,11-tetraazacyclotetradecane-N'N'-diacetic acid,[CuC16N4H34(CH2COO)(CH2COOH)]·ClO4·0. 5HCIO4·1. 5H2O was determined. Crystallographic data: Mr = 639.22,orthorhombic, space group Pcnb with a=11.743(4),b=16.446(2),c=29.611 (4) A,Z=8,V=5726(3) A3, Dc=1.482 g·cm-3, F(000)=1344,μ=9. 64 cm-1,R=0.063,and Rw=0.067 for 2386 reflections with I≥3σ(I). The structure shows an unusual configuration in which two carboxyl groups were bonded to two neighboring nitrogen atoms of the macrocycle, N1 and N4, and six methyl substituents occur on one side of the macrocycle, while two carboxyl groups on the other side, and central copper(Ⅱ) ion forms a five-coordinated geometry.
基金The project was financially supported from the National Natural Science Foundation of China (No. 20171012)+5 种基金 and the Natural Science Foundation of Fujian province (No.E0110010)
文摘The title compound 1,4,23,26,29,48-hexaaza-6,9:16,19:31,34:41,44-tetrabenzo-12, 15,37,40-tetraoxa-cyclodotetracontane-4,5,18,19,25,26,39,40-octaene 1 (C40H46N6O4) was synthe- sized by [2+2] condensation of diethylenetriamine with 4,4?diformyl-diphenoxyethane (dialdehyde) in a mixed solvent of ethanol and tetrahydrofuran. The crystal data are: Mr = 674.83, triclinic, P, a = 5.8249(1), b = 9.4114(8), c = 17.649(2) ? a = 79.310(7), b = 85.397(4), g = 78.970(8), V = 932.1(1) ?, Z = 1, Dc = 1.202 g/cm3, F(000) = 360, m(MoKa) = 0.079 mm-1, R = 0.0486 and wR = 0.1439. The title molecule has a crystallographic center symmetry. The distance between the two secondary amine nitrogen atoms is 18.890(3) ?
基金the Natural Science Foundation of Shandong Province(No.Y2 0 0 2 B0 6 )
文摘A mixed-valence dinuclear manganese complex, [Mn ⅡMn ⅢL](ClO 4)·1/2MeOH, where L is a macrocyclic ligand derived from the cyclocondensation of sodium 2,6-diformyl-4-methylphenolate with N,N-bis(2-aminoethyl)-2-hydroxybenzyl amine, was obtained and its structure was determined by X-ray diffraction. The orange crystal is a monoclinic system with space group P2 1/c and lattice parameters a=1.1617(4), b=1.4005(3), c=1.4641(3) nm, β=113.03(2)°, and Z=2. The crystal structure shows that each pendant-arm is bonded in a bidentate fashion to the adjacent metal atom and that both the arms are on the same side of the macrocycle. The two Mn atoms are bridged by two μ 2-phenoxy oxygen atoms of the tetra-imine macrocycle, and each Mn atom, locating in a trigonal prismatic coordination environment(N 3O 3), is six-coordinated by the two imine nitrogen atoms, one tertiary nitrogen atom and a pendant phenol moiety apart from the two oxygen atoms.
文摘The title compound, (C 34 H 54 N 2O 10 )[Eu(NO 3) 5](C 34 H 52 N 2O 10 =1,2 bis(2,3 benzo 10 aza 15 crown 5 N ethyleneoxy)ethane), was synthesized in acetonitrile solution and its crystal structure was determined by X ray analysis. The crystal crystallizes in monoclinic, space group P21/c with cell parameters a =1 1801(2) nm, b =2 3560(5) nm, c =1 7025(3) nm, β =99 67(3)°, V =4 6662(16) nm 3, Z =4, D c=1 581 g/cm 3. The europium ion is coordinated with ten oxygen atoms from five nitrato groups, and neither O atoms nor N atoms of the macrocyclic compound are bonded to the europium ion.
文摘Crystal structure of nickel（II） complex with a new 14 membered tetraazamacrocyclic ligand 5,12-diphenyl-7,14-dimethyl-1,4,8,11-tetraazacyclotetradecane-N’,N-diacetic acid,Ni[N<sub>4</sub>C<sub>10</sub>（CH<sub>2</sub>COO）<sub>2</sub>（C<sub>6</sub>H<sub>5</sub>）<sub>2</sub>]·2H<sub>2</sub>O, M<sub>r</sub>= 589. 38 is reported.It crystallizes in monoclinic P2<sub>1</sub>/c space group with a=12.949（6）,b=16.373（3）,c=14.232（16）,β=98.68（6）°,V=2982.9（7）,Z=4,D<sub>c</sub>=1.312 gcm-3,μ=6.953 cm-1,F（000）=1256.0.Finally,the structure was refined to R=0.080,R<sub>w</sub>=0.065 for 2952 reflections.The central nickel ion of the complex forms an octahedron with four nitrogen atoms of the macrocycle and two oxygen atoms of the appended carboxylate groups.Two phenyl planes of the ligand are almost parallel to each other.
文摘The title compound C（15）H（14）N4OS·H<sub>2</sub>O crystallizes in the monoclinic system, space group P21/a, with a=8. 733（3） , b= 16. 731 （4） , c=10. 476（4） A,β= 95. 41（3） °, V = 1523. 7（8） A￣3, D<sub>c</sub>=1. 38 g/cm￣3, Z = 4,Mr= 316. 38,λ（MoKα） = 0. 71069 A, F（000） = 664,μ= 2.14 cm-1, T= 296K. Final R=0. 054,and Rω=0.063 for 1279 reflections with I≥3σ（I）. The parent structure of the molecule is a distorted six-membered ring. The effect of the steric hindrance between the two phenyls on the conjugate interactions in the heterocyclic ring has been discussed.
文摘The title compound （E）-ethyl 2-fluoro-2-（3-oxoisobenzofuran-1（3H）-ylidene） aceta- te was synthesized as an unexpected product by the reaction ofphthalyl dichloride with bis-silylenol ether, which is not in accordance with our previous studies. The title compound was characterized by single-crystal X-ray diffraction, 1H NMR, 13C NMR, 19F NMR, GCMS, HRMS and IR. The crystal （C12HgFO4, Mr = 236.19） belongs to the monoclinic system, space group P21/c, a = 19.1609（8）, b = 7.9831（3）, c = 13.7715（6） A, V= 2106.13（15） A3, Z= 8, Dx = 1.490 Mg m-3, MoKa radiation, 2 = 0.71073 A,μ = 0.12 mm-1, F（000） = 976, the final R = 0.025 and wR = 0.1300 for 4505 observed reflections with I〉 2σ（I）.
