A new bicadmium(??) complex [Cd2L](ClO4)2?1.25H2O (C28H35Cd2Cl4N6O13.25) was synthesized and characterized by X-ray diffraction and ES mass spectral analyses. It crystallizes in the triclinic system, space gro...A new bicadmium(??) complex [Cd2L](ClO4)2?1.25H2O (C28H35Cd2Cl4N6O13.25) was synthesized and characterized by X-ray diffraction and ES mass spectral analyses. It crystallizes in the triclinic system, space group P1 with a = 15.630(3), b = 15.990(3), c = 16.330(3) ?, α = 89.90(3), β = 68.87(3), γ = 87.94(3)o, V = 3804.1(13) ?3, Mr = 1034.22, Z = 4, F(000) = 2060, Dc = 1.806 g/cm3, T = 293(2) K, μ = 1.468 mm-1 and λ = 0.71073 ?. The structure was refined to R = 0.0779 and wR = 0.1960 for 7034 observed reflections with I > 2σ(I).展开更多
An unsymmetrical macrocyclic dinuclear Zn(II) complex, [Zn2(H0.5L)(OAc)](ClO4)1.5(1, H2 L is the condensation product between 2, 6-diformyl-4-methylphenol and diethylenetriamine), was obtained and characteri...An unsymmetrical macrocyclic dinuclear Zn(II) complex, [Zn2(H0.5L)(OAc)](ClO4)1.5(1, H2 L is the condensation product between 2, 6-diformyl-4-methylphenol and diethylenetriamine), was obtained and characterized by IR spectrum, elemental analysis and X-ray single-crystal diffraction. The complex crystallizes in monoclinic, space group P21/c with a = 16.784(2), b = 19.474(3), c = 10.3364(13)A, β = 92.923(2)°, V = 3374.1(7) A3, Z = 4, Dc = 1.672 g/cm^3, F(000) = 1740, μ = 1.651 mm^-1, the R = 0.0609 and wR = 0.1696 for 4745 observed reflections(I 〉 2σ(I)). The interactions of the complex with DNA have been measured by electrochemical studies, UV spectroscopy and viscosity experiment. The interactions of the complex with calf thymus DNA were studied by UV-vis spectra and the binding constant is 1.58 × 10^4 mol·L^-1. The phosphate hydrolysis catalyzed by the complex was investigated using 4-nitrophenyl phosphate(NPP) as the substrate; the observed first order rate constant value is 3.0 × 10^–4 s^-1.展开更多
Two novel diethyltin(IV) complexes of N-salicylidenevaline (H2L1) and N-Sali- cylidenetryptophan (H2L^2), Et2SrtL^1 1 and Et2SnL^2 2, were synthesized and characterized by elemental analysis, IR, ^1H NMR and X-r...Two novel diethyltin(IV) complexes of N-salicylidenevaline (H2L1) and N-Sali- cylidenetryptophan (H2L^2), Et2SrtL^1 1 and Et2SnL^2 2, were synthesized and characterized by elemental analysis, IR, ^1H NMR and X-ray single-crystal diffraction analysis. Complex 1 belongs to the trigonal system, space group R-3 with a = b = 19.2730(5), c = 23.6890(13)A^°, V= 7620.4(5) A^°^3, Z = 6, Dc= 1.553 g/cm^3,μ= 1.518 mm^-1, F(000) = 3600, R = 0.0238 and wR = 0.0636. Complex 2 is of monoelinie system, space group P21/c with a = 13.7550(8), b = 11.5425(7), c = 12.7876(7)A^°, β= 93.585(1)°, V = 2026.3(2) A^°^3, Z = 4, Dc= 1.548 g/cm^3,μ = 1.286 mm^-1, F(000) = 976, R = 0.0298 and wR = 0.0722. Complex 1 is a cyclic trimer with a macrocyclic 12-membered ring structure formed by the bidentate bridging coordination of carboxylate group to tin atoms. The tin atom is six-coordinated in a distorted octahedral geometry. In complex 2, the distorted trigonal bipyramidal Et2SnL2 units are linked into polymeric chains by the weak Sn…O interaction involving Sn and the earbonyl O of an adjacent ligand, and the chains are further connected by intermolecular N-H…O hydrogen bonds to form a two-dimensional supramolecular structure.展开更多
A new macrocycle based on diethoxycarbonyl glycoluril 3,C26H30N6O10,has been synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic,space group P21/c with a = 12.7291(10),b ...A new macrocycle based on diethoxycarbonyl glycoluril 3,C26H30N6O10,has been synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic,space group P21/c with a = 12.7291(10),b = 25.157(2),c = 8.5489(7) A,β = 104.4760(10)°,V = 2650.7(4) A^3,Z = 4,C26H30N6O10,Mr = 586.56,F(000) = 1232,T = 292(2) K,Dc = 1.470 g/cm^3,μ = 0.115 mm^-1,the final R = 0.0590 and wR = 0.1299 for 4918 observed reflections with I 〉 2σ(I). In the structure of the title compound,a three-dimensional microporous architecture is formed via intermolecular hydrogen bonding interactions.展开更多
metol-free Robson -type macrocycle was synthesized for first time by proton-templation and from that the metal complexes were prepared.By X-ray study the structure of Ni(Ⅱ)-complex was characterized.
A novel [2+4+2]-macrocyclic compound 3(C52H69N16O12, Mr = 1109.53) con- taining bis(ethoxycarbonyl)glycoluril groups was synthesized via the Mannich three-component reaction in one pot and its structure was char...A novel [2+4+2]-macrocyclic compound 3(C52H69N16O12, Mr = 1109.53) con- taining bis(ethoxycarbonyl)glycoluril groups was synthesized via the Mannich three-component reaction in one pot and its structure was characterized by single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1 with a = 10.077(3), b = 10.642(3), c = 15.324(5) , α = 96.704(5), β = 102.304(5), γ = 104.546(5)°, Z = 2, V = 1528.7(8)3, Dc = 1.283 g/cm3, μ = 0.097 mm-1, F(000) = 628, R = 0.0818 and wR(I 〉 2σ(I)) = 0.2346 for 3034 observed reflections.展开更多
A novel [1+1] Schiff-base macrocyclic compound 3 has been synthesized from precursor 1, 1,3-bis(2'- formylphenoxy)-2-propanol, and precursor 2, resorcinol-bis(4-aminophenyl)ether, via condensation and cyclizacti...A novel [1+1] Schiff-base macrocyclic compound 3 has been synthesized from precursor 1, 1,3-bis(2'- formylphenoxy)-2-propanol, and precursor 2, resorcinol-bis(4-aminophenyl)ether, via condensation and cyclizaction using Ba2+ as template. The macrocycle 3 was further reduced giving saturated macrocycle 4. The structures of 3 and 4 were characterized by elemental analysis, ~H NMR, IR, and MS spectra, and their structures were determined via single crystal X-ray diffraction studies. X-ray diffraction analysis revealed that the macrocyclic compound 3 has a folded conformation, and the corresponding reduced product 4 adopts a twisted and folded conformation due to its flexible nature. ~ 2013 Bi-Xue Zhu. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.展开更多
The functionalized calix[4]pyrrole meso-substituted Schiff bases were conveniently prepared by four- step synthetic route. Furthermore, the nickel and copper complexes of calix[4]pyrrole meso-substituted Schiff base w...The functionalized calix[4]pyrrole meso-substituted Schiff bases were conveniently prepared by four- step synthetic route. Furthermore, the nickel and copper complexes of calix[4]pyrrole meso-substituted Schiff base with 1:2 stoichiometry were obtained. The crystal structures of the calix[4]pyrroles and their metal complexes were determined by X-ray diffraction.展开更多
We describe the design and execution of a novel synthetic route to the tricyclic core of haliclonin A,a tetracyclic marine natural product.The approach features Bachi's thiol-medicated free radical cyclization of alk...We describe the design and execution of a novel synthetic route to the tricyclic core of haliclonin A,a tetracyclic marine natural product.The approach features Bachi's thiol-medicated free radical cyclization of alkenyl isocyanide to build the bridged ring system,and ring-closing metathesis(RCM) reaction to form the macrocycle.Execution of the synthetic plan ultimately resulted in a diazatricyclic compound.By means of 2D NMR techniques,the structure of this compound was revealed to an unexpected product 8.Analysis of the synthetic pathways allowed concluding that the unexpected product is a result of an "unexpected" migration of olefinic bond during dioxolanation of the 2-cyclohexenone derivative 7.This investigation also resulted in a concise construction of the functionalized hexahydro-1H-isoindole-1,5(4H)-dione 12 and the macrocyclic tricyclic ring system 8.展开更多
New [1+1] and 62-membered [2+2] Schiff base macrocycles containing a 2,6-diamidopyridine subunit have been synthesized by condensation reaction of the precursors pyridine-2,6-dicarboxamide and 1,10- bis(2'-formylp...New [1+1] and 62-membered [2+2] Schiff base macrocycles containing a 2,6-diamidopyridine subunit have been synthesized by condensation reaction of the precursors pyridine-2,6-dicarboxamide and 1,10- bis(2'-formylphenyloxy)decane in the presence of phosphoric acid via a one-pot process. The cyclo- condensed products were effectively isolated by gel column chromatography and characterized by 1H NMR, FTIR, mass spectrometry and X-ray analysis. The two macrocycles have a twisted structure, and not an open 'circular' conformation in the solid state.展开更多
基金This project was supported by the National Natural Science Foundation of China(No.50372028)
文摘A new bicadmium(??) complex [Cd2L](ClO4)2?1.25H2O (C28H35Cd2Cl4N6O13.25) was synthesized and characterized by X-ray diffraction and ES mass spectral analyses. It crystallizes in the triclinic system, space group P1 with a = 15.630(3), b = 15.990(3), c = 16.330(3) ?, α = 89.90(3), β = 68.87(3), γ = 87.94(3)o, V = 3804.1(13) ?3, Mr = 1034.22, Z = 4, F(000) = 2060, Dc = 1.806 g/cm3, T = 293(2) K, μ = 1.468 mm-1 and λ = 0.71073 ?. The structure was refined to R = 0.0779 and wR = 0.1960 for 7034 observed reflections with I > 2σ(I).
基金Supported by National Natural Science Foundation of China(21201136)Wuhan Youth Chenguang Program of Science and Technology(201271031374)
文摘An unsymmetrical macrocyclic dinuclear Zn(II) complex, [Zn2(H0.5L)(OAc)](ClO4)1.5(1, H2 L is the condensation product between 2, 6-diformyl-4-methylphenol and diethylenetriamine), was obtained and characterized by IR spectrum, elemental analysis and X-ray single-crystal diffraction. The complex crystallizes in monoclinic, space group P21/c with a = 16.784(2), b = 19.474(3), c = 10.3364(13)A, β = 92.923(2)°, V = 3374.1(7) A3, Z = 4, Dc = 1.672 g/cm^3, F(000) = 1740, μ = 1.651 mm^-1, the R = 0.0609 and wR = 0.1696 for 4745 observed reflections(I 〉 2σ(I)). The interactions of the complex with DNA have been measured by electrochemical studies, UV spectroscopy and viscosity experiment. The interactions of the complex with calf thymus DNA were studied by UV-vis spectra and the binding constant is 1.58 × 10^4 mol·L^-1. The phosphate hydrolysis catalyzed by the complex was investigated using 4-nitrophenyl phosphate(NPP) as the substrate; the observed first order rate constant value is 3.0 × 10^–4 s^-1.
基金supported by the NNSFC (20701027)the Post-Doctor Innovation Project of Shandong Province (200702021) the Key Laboratory of Colloid Interface Chemistry of Ministry of Education (200707)
文摘Two novel diethyltin(IV) complexes of N-salicylidenevaline (H2L1) and N-Sali- cylidenetryptophan (H2L^2), Et2SrtL^1 1 and Et2SnL^2 2, were synthesized and characterized by elemental analysis, IR, ^1H NMR and X-ray single-crystal diffraction analysis. Complex 1 belongs to the trigonal system, space group R-3 with a = b = 19.2730(5), c = 23.6890(13)A^°, V= 7620.4(5) A^°^3, Z = 6, Dc= 1.553 g/cm^3,μ= 1.518 mm^-1, F(000) = 3600, R = 0.0238 and wR = 0.0636. Complex 2 is of monoelinie system, space group P21/c with a = 13.7550(8), b = 11.5425(7), c = 12.7876(7)A^°, β= 93.585(1)°, V = 2026.3(2) A^°^3, Z = 4, Dc= 1.548 g/cm^3,μ = 1.286 mm^-1, F(000) = 976, R = 0.0298 and wR = 0.0722. Complex 1 is a cyclic trimer with a macrocyclic 12-membered ring structure formed by the bidentate bridging coordination of carboxylate group to tin atoms. The tin atom is six-coordinated in a distorted octahedral geometry. In complex 2, the distorted trigonal bipyramidal Et2SnL2 units are linked into polymeric chains by the weak Sn…O interaction involving Sn and the earbonyl O of an adjacent ligand, and the chains are further connected by intermolecular N-H…O hydrogen bonds to form a two-dimensional supramolecular structure.
基金supported by Central China Normal University and the National Natural Science Foundation of China (20472022 and 20672042)
文摘A new macrocycle based on diethoxycarbonyl glycoluril 3,C26H30N6O10,has been synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic,space group P21/c with a = 12.7291(10),b = 25.157(2),c = 8.5489(7) A,β = 104.4760(10)°,V = 2650.7(4) A^3,Z = 4,C26H30N6O10,Mr = 586.56,F(000) = 1232,T = 292(2) K,Dc = 1.470 g/cm^3,μ = 0.115 mm^-1,the final R = 0.0590 and wR = 0.1299 for 4918 observed reflections with I 〉 2σ(I). In the structure of the title compound,a three-dimensional microporous architecture is formed via intermolecular hydrogen bonding interactions.
文摘metol-free Robson -type macrocycle was synthesized for first time by proton-templation and from that the metal complexes were prepared.By X-ray study the structure of Ni(Ⅱ)-complex was characterized.
基金supported by Central China Normal University and the National Science Foundation of China(No.21272085)
文摘A novel [2+4+2]-macrocyclic compound 3(C52H69N16O12, Mr = 1109.53) con- taining bis(ethoxycarbonyl)glycoluril groups was synthesized via the Mannich three-component reaction in one pot and its structure was characterized by single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1 with a = 10.077(3), b = 10.642(3), c = 15.324(5) , α = 96.704(5), β = 102.304(5), γ = 104.546(5)°, Z = 2, V = 1528.7(8)3, Dc = 1.283 g/cm3, μ = 0.097 mm-1, F(000) = 628, R = 0.0818 and wR(I 〉 2σ(I)) = 0.2346 for 3034 observed reflections.
基金supported by the National Natural Science Foundation of China(No.21061003)he International Collaborative Project of Guizhou Province(No.[2009]700104)the Natural Science Foundation of the Guizhou Province(No.(2012)2151)
文摘A novel [1+1] Schiff-base macrocyclic compound 3 has been synthesized from precursor 1, 1,3-bis(2'- formylphenoxy)-2-propanol, and precursor 2, resorcinol-bis(4-aminophenyl)ether, via condensation and cyclizaction using Ba2+ as template. The macrocycle 3 was further reduced giving saturated macrocycle 4. The structures of 3 and 4 were characterized by elemental analysis, ~H NMR, IR, and MS spectra, and their structures were determined via single crystal X-ray diffraction studies. X-ray diffraction analysis revealed that the macrocyclic compound 3 has a folded conformation, and the corresponding reduced product 4 adopts a twisted and folded conformation due to its flexible nature. ~ 2013 Bi-Xue Zhu. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.
基金financially supported by the National Natural Science Foundation of China (No.21172190)the Priority Academic Program Development of Jiangsu Higher Education Institutions
文摘The functionalized calix[4]pyrrole meso-substituted Schiff bases were conveniently prepared by four- step synthetic route. Furthermore, the nickel and copper complexes of calix[4]pyrrole meso-substituted Schiff base with 1:2 stoichiometry were obtained. The crystal structures of the calix[4]pyrroles and their metal complexes were determined by X-ray diffraction.
基金the National Natural Science Foundation of China(No.21472153)the National Basic Research Program(973 Program)of China(No.2010CB833200)+1 种基金the SKL of Xiamen University(No.201509)the Program for Changjiang Scholars and Innovative Research Team in University of Ministry of Education,China,for financial support
文摘We describe the design and execution of a novel synthetic route to the tricyclic core of haliclonin A,a tetracyclic marine natural product.The approach features Bachi's thiol-medicated free radical cyclization of alkenyl isocyanide to build the bridged ring system,and ring-closing metathesis(RCM) reaction to form the macrocycle.Execution of the synthetic plan ultimately resulted in a diazatricyclic compound.By means of 2D NMR techniques,the structure of this compound was revealed to an unexpected product 8.Analysis of the synthetic pathways allowed concluding that the unexpected product is a result of an "unexpected" migration of olefinic bond during dioxolanation of the 2-cyclohexenone derivative 7.This investigation also resulted in a concise construction of the functionalized hexahydro-1H-isoindole-1,5(4H)-dione 12 and the macrocyclic tricyclic ring system 8.
基金supported by the National Natural Science Foundation of China (No. 21061003)the ‘Chun-Hui’ Fund of Chinese Ministry of Education (No. Z2012054)
文摘New [1+1] and 62-membered [2+2] Schiff base macrocycles containing a 2,6-diamidopyridine subunit have been synthesized by condensation reaction of the precursors pyridine-2,6-dicarboxamide and 1,10- bis(2'-formylphenyloxy)decane in the presence of phosphoric acid via a one-pot process. The cyclo- condensed products were effectively isolated by gel column chromatography and characterized by 1H NMR, FTIR, mass spectrometry and X-ray analysis. The two macrocycles have a twisted structure, and not an open 'circular' conformation in the solid state.