A new complex Mn(Htpc)2(H2O)2(1, Htpc = 5-(trifluoromethyl)pyridine-2-carboxylic acid) has been synthesized and characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. 1 belongs to triclinic ...A new complex Mn(Htpc)2(H2O)2(1, Htpc = 5-(trifluoromethyl)pyridine-2-carboxylic acid) has been synthesized and characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. 1 belongs to triclinic system, space group P■ with a = 5.0885(10), b = 6.5574(13), c = 14.016(3) ?, β = 90.67(3)o, V = 436.34(17) ?3, Z = 1, Dc = 1.793 g·cm-3, μ = 0.855 mm-1, Mr = 471.18, F(000) = 235, the final R = 0.0454 and wR = 0.1134 for 1998 observed reflections with I > 2σ(I). The Mn(Ⅱ) ion is coordinated by two N and two O atoms from two Htpc as well as two O atoms from two coordinated water molecules, forming a 0D motif with distorted octahedral coordinate geometry. The adjacent 0D units are linked into 1D chains through hydrogen bond O(1W)–H(1 WB)···O(2), and via the O(1 W)–H(1 WA)···O(1) hydrogen bond the neighboring 1D chains are connected into a 2D supramolecular layer. Moreover, the interactions between the ligand and its complex with CT-DNA were studied by EtBr fluorescence probe, which suggested that these compounds bind to CT-DNA through an intercalation mode. The binding constants were 0.41 and 0.64 for Htpc and complex 1, respectively. It indicates that the interaction between complex 1 and CT-DNA is stronger than Htpc.展开更多
The title compound 4-（4,6-dimethoxylpyrimidin-2-yl）-3-thiourea carboxylic acid methyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in eth...The title compound 4-（4,6-dimethoxylpyrimidin-2-yl）-3-thiourea carboxylic acid methyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at the room temperature. The structure was characterized by elemental analysis and IR and determined by X-ray diffraction analysis＇ Crystallographic data： C9H12N4O4S, Mr = 272.29, monoclinic, space group C2/m with a = 1.6672（3）, b = 0.66383（12）, c = 1.1617（2） nm, β = 109.275（2）°, V = 1.2136（4） nm^3, Dc = 1.490 g/cm^3,μ = 0.281 mm^-1, F（000） = 568, Z = 4, R1 = 0.0341and wR2 = 0.1042.展开更多
4-（4,6-Dimethoxyl-pyrimidin-2-yl）-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single ...4-（4,6-Dimethoxyl-pyrimidin-2-yl）-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at room temperature. The crystal structure was determined by X-ray diffraction analysis. Crystallographic data： C10H14N4O4S, M, = 286.31, monoclinic, space group C2/c with a = 2.5309（3）, b = 0.67682（6）, c = 1.74237（19） nm, β = 114.744（3）°, V= 2.7106（5） nm3, Dc = 1.403 g/cm3, p = 0.225 mm-1, F（000） = 1200, Z= 8, R= 0.0514 and wR= 0.1529.展开更多
The title Mn（Ⅱ） coordination polymer,poly{[heptaaqua-（μ4-bi-phenyl-3,3？,5,5？-tetracarboxylate）-bimanganese（Ⅱ）] pentahydrate},[Mn_2（bpta）（H_2O）_7]_n·5n H_2O（I）,is crystallized from a mixture of bi...The title Mn（Ⅱ） coordination polymer,poly{[heptaaqua-（μ4-bi-phenyl-3,3？,5,5？-tetracarboxylate）-bimanganese（Ⅱ）] pentahydrate},[Mn_2（bpta）（H_2O）_7]_n·5n H_2O（I）,is crystallized from a mixture of biphenyl-3,3？,5,5？-tetracarboxylic acid（H_4bpta） and MnCl_2·4H_2O in waterethanol under room temperature. Its asymmetric unit consists of one and two halves of crystallographically independent Mn（Ⅱ） cations,one fully deprotonated H4 bpta ligand,seven coordinated water molecules and five solvent water as guest molecules. In I,each Mn（Ⅱ） atom is octahedrally coordinated by six oxygen atoms from bpta^（4-） anions and coordinated water molecules. In the Mn（Ⅱ） cations,one half Mn（Ⅱ） ion of them located at a 2-fold axis generating a trinuclear [Mn_3（H_2O）_2（RCOO）_2] linker by μ1,1-O（water） and μ1,3-O,O？（carboxylate） bridges and another half Mn（Ⅱ） ion with an inversion is a mononuclear linker. These neighbouring trinuclear and mononuclear Mn（Ⅱ） cations are linked together by biphenyl-3,3？,5,5？-tetracarboxylates to form a three-dimensional framework with a（42.84） topology of a（4,4）-connected net,in which the positions of the trinuclear [Mn_3（H_2O）_2（R-COO）_2] linker as a 4-connector linking four bpta^（4-） ligands in I reproduce an eagle-shaped arrangement. The polymeric structure exhibits a water channel with an accessible void of 797.1 ？~3,amounting to 15.7% of the total unit-cell volume. Each of the cavities in the network is occupied by solvent water molecules.展开更多
The title compound, acetic acid-3,5-diacetoxy-2-acetoxymethyl-6-（4-quinoxalin- 2-yl-phenoxy）-tetrahydro-pyran-4-yl-ester 8 （C28H28N2O10, Mr = 552.54）, has been synthesized and its crystal structure was determined ...The title compound, acetic acid-3,5-diacetoxy-2-acetoxymethyl-6-（4-quinoxalin- 2-yl-phenoxy）-tetrahydro-pyran-4-yl-ester 8 （C28H28N2O10, Mr = 552.54）, has been synthesized and its crystal structure was determined by X-ray diffraction analysis. It crystallizes in monoclinic, space group P21, a = 10.060（8）, b = 5.648（4）, c = 24.11（2）A, β = 91.078（10）°, Z = 2, V= 1369.9（19）A^3, Dc = 1.339 g/cm^3,μ（MoKa） = 1.03 cm^-1, F（000） = 580.00, T =. 193.1 Kx-9 θmax = 25.03, （△/σ）max = 0.0000, Flack = -0.0（24）, the final R = 0.0680 and wR = 0.140 （w = 1/[0.0016Fo^2 ＋ 1.00000（Fo^2）]/（4Fo^2）） for 3126 observed reflections （1 〉 20（/））. The pyranoid ring adopts chair conformation in the sugar moiety, and all of the acetyl groups are in the e bond of the pyranoid ring, so the sugar moiety is very stable.展开更多
基金Supported by the Scientific Research Foundation of Higher Education Institutions of Ningxia(No.NGY2017004)the National Natural Science Foundation of China(Nos.21763022 and 50564043)the Major Innovation Projects for Building First-class Universities in China’s Western Region(No.ZKZD2017003)
文摘A new complex Mn(Htpc)2(H2O)2(1, Htpc = 5-(trifluoromethyl)pyridine-2-carboxylic acid) has been synthesized and characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. 1 belongs to triclinic system, space group P■ with a = 5.0885(10), b = 6.5574(13), c = 14.016(3) ?, β = 90.67(3)o, V = 436.34(17) ?3, Z = 1, Dc = 1.793 g·cm-3, μ = 0.855 mm-1, Mr = 471.18, F(000) = 235, the final R = 0.0454 and wR = 0.1134 for 1998 observed reflections with I > 2σ(I). The Mn(Ⅱ) ion is coordinated by two N and two O atoms from two Htpc as well as two O atoms from two coordinated water molecules, forming a 0D motif with distorted octahedral coordinate geometry. The adjacent 0D units are linked into 1D chains through hydrogen bond O(1W)–H(1 WB)···O(2), and via the O(1 W)–H(1 WA)···O(1) hydrogen bond the neighboring 1D chains are connected into a 2D supramolecular layer. Moreover, the interactions between the ligand and its complex with CT-DNA were studied by EtBr fluorescence probe, which suggested that these compounds bind to CT-DNA through an intercalation mode. The binding constants were 0.41 and 0.64 for Htpc and complex 1, respectively. It indicates that the interaction between complex 1 and CT-DNA is stronger than Htpc.
基金This work was supported by the National Natural Science Foundation of China (20571060) and Education Committee of Shaan Xi Province (05JK294)
文摘The title compound 4-（4,6-dimethoxylpyrimidin-2-yl）-3-thiourea carboxylic acid methyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at the room temperature. The structure was characterized by elemental analysis and IR and determined by X-ray diffraction analysis＇ Crystallographic data： C9H12N4O4S, Mr = 272.29, monoclinic, space group C2/m with a = 1.6672（3）, b = 0.66383（12）, c = 1.1617（2） nm, β = 109.275（2）°, V = 1.2136（4） nm^3, Dc = 1.490 g/cm^3,μ = 0.281 mm^-1, F（000） = 568, Z = 4, R1 = 0.0341and wR2 = 0.1042.
基金supported by the National Natural Science Foundation of China (20571060)Natural Science Foundation of Shaanxi Province (2007B08)Education Committee of Shaanxi Province (05JK294)
文摘4-（4,6-Dimethoxyl-pyrimidin-2-yl）-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at room temperature. The crystal structure was determined by X-ray diffraction analysis. Crystallographic data： C10H14N4O4S, M, = 286.31, monoclinic, space group C2/c with a = 2.5309（3）, b = 0.67682（6）, c = 1.74237（19） nm, β = 114.744（3）°, V= 2.7106（5） nm3, Dc = 1.403 g/cm3, p = 0.225 mm-1, F（000） = 1200, Z= 8, R= 0.0514 and wR= 0.1529.
基金supported by the National Natural Science Foundation of China(No.21571118)
文摘The title Mn（Ⅱ） coordination polymer,poly{[heptaaqua-（μ4-bi-phenyl-3,3？,5,5？-tetracarboxylate）-bimanganese（Ⅱ）] pentahydrate},[Mn_2（bpta）（H_2O）_7]_n·5n H_2O（I）,is crystallized from a mixture of biphenyl-3,3？,5,5？-tetracarboxylic acid（H_4bpta） and MnCl_2·4H_2O in waterethanol under room temperature. Its asymmetric unit consists of one and two halves of crystallographically independent Mn（Ⅱ） cations,one fully deprotonated H4 bpta ligand,seven coordinated water molecules and five solvent water as guest molecules. In I,each Mn（Ⅱ） atom is octahedrally coordinated by six oxygen atoms from bpta^（4-） anions and coordinated water molecules. In the Mn（Ⅱ） cations,one half Mn（Ⅱ） ion of them located at a 2-fold axis generating a trinuclear [Mn_3（H_2O）_2（RCOO）_2] linker by μ1,1-O（water） and μ1,3-O,O？（carboxylate） bridges and another half Mn（Ⅱ） ion with an inversion is a mononuclear linker. These neighbouring trinuclear and mononuclear Mn（Ⅱ） cations are linked together by biphenyl-3,3？,5,5？-tetracarboxylates to form a three-dimensional framework with a（42.84） topology of a（4,4）-connected net,in which the positions of the trinuclear [Mn_3（H_2O）_2（R-COO）_2] linker as a 4-connector linking four bpta^（4-） ligands in I reproduce an eagle-shaped arrangement. The polymeric structure exhibits a water channel with an accessible void of 797.1 ？~3,amounting to 15.7% of the total unit-cell volume. Each of the cavities in the network is occupied by solvent water molecules.
基金This project was supported by the Key Laboratory of Organic Synthesis of Jiangsu Province
文摘The title compound, acetic acid-3,5-diacetoxy-2-acetoxymethyl-6-（4-quinoxalin- 2-yl-phenoxy）-tetrahydro-pyran-4-yl-ester 8 （C28H28N2O10, Mr = 552.54）, has been synthesized and its crystal structure was determined by X-ray diffraction analysis. It crystallizes in monoclinic, space group P21, a = 10.060（8）, b = 5.648（4）, c = 24.11（2）A, β = 91.078（10）°, Z = 2, V= 1369.9（19）A^3, Dc = 1.339 g/cm^3,μ（MoKa） = 1.03 cm^-1, F（000） = 580.00, T =. 193.1 Kx-9 θmax = 25.03, （△/σ）max = 0.0000, Flack = -0.0（24）, the final R = 0.0680 and wR = 0.140 （w = 1/[0.0016Fo^2 ＋ 1.00000（Fo^2）]/（4Fo^2）） for 3126 observed reflections （1 〉 20（/））. The pyranoid ring adopts chair conformation in the sugar moiety, and all of the acetyl groups are in the e bond of the pyranoid ring, so the sugar moiety is very stable.
