A new hexanuclear silver (I) compound 2 containing thiosemicarbazone with the group of benzene was synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analysis and fluorescence ...A new hexanuclear silver (I) compound 2 containing thiosemicarbazone with the group of benzene was synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analysis and fluorescence spectrum. The title compound crystallizes in triclinic, space group P with a = 11.611(3), b = 15.610(5), c = 15.624(7) , α = 113.942(6), β = 104.520(6), γ = 104.230(4)°, V = 2304.1(14) 3, C60H77Ag6N22O4.5S6, Mr = 2018.02, Dc = 1.454 g/cm3, μ(MoKα) = 1.435 mm-1, F(000) = 1005, Z = 1, the final R = 0.0468 and wR = 0.1474 for 6608 observed reflections (I 2σ(I)). In the structure, the S atom of the ligand L2 (L2 = benzaldehyde thiosemicarbazone) served as a triply bridged chelator to connect the six silver atoms into a Ag6L26 cluster. The luminescence property of compound 2 was investigated at room temperature.展开更多
A series of acyls (Ac, Bz and Ts) were introduced regioselectively to the 2-hydroxyl in methyl and ally 3-O-benzyl-α-L-rhamnopyranosides mediated by silver(I) oxide in the presence of a catalytic amount of potass...A series of acyls (Ac, Bz and Ts) were introduced regioselectively to the 2-hydroxyl in methyl and ally 3-O-benzyl-α-L-rhamnopyranosides mediated by silver(I) oxide in the presence of a catalytic amount of potassium iodide in 56-78% yields.展开更多
The title complex,[Ag 2 (L1) 2 (Pyr)·2.5H 2 O] 1 (L1=6-amino-1-naphthalenesulfonate anion,Pyr=pyrazine),has been synthesized and characterized by single-crystal X-ray diffraction analysis.It crystallizes in...The title complex,[Ag 2 (L1) 2 (Pyr)·2.5H 2 O] 1 (L1=6-amino-1-naphthalenesulfonate anion,Pyr=pyrazine),has been synthesized and characterized by single-crystal X-ray diffraction analysis.It crystallizes in triclinic,space group P1,with a=7.339(5),b=13.105(5),c=14.097(5),α=84.377(5),β=76.921(5),γ=79.628(5)°,V=1296.7(11) 3,C 48 H 50 Ag 4 N 8 O 17 S 4,M r=1570.68,Z=1,D c=2.011 g/cm 3,μ=1.732 mm-1,F(000)=782,S=1.148,the final R=0.0436 and wR=0.1181 for 4130 observer reflections (I 2σ(Ⅰ)).Compound 1 shows a rare one-dimensional (1D) double chain,and the chains are further connected through secondary bonding,hydrogen bonds,and π-π interactions to generate a three-dimensional (3D) supramolecular structure.The luminescent property of 1 was also studied in the solid state at room temperture.展开更多
The cyclic voltammetry(CV) and the square wave technique were used for the investigations of thallium(Ⅰ) underpotential deposition(UPD) on the silver electrode. A solution of 10 \{mmol/L\} HClO 4+10 mmol/L NaCl was s...The cyclic voltammetry(CV) and the square wave technique were used for the investigations of thallium(Ⅰ) underpotential deposition(UPD) on the silver electrode. A solution of 10 \{mmol/L\} HClO 4+10 mmol/L NaCl was selected as the supporting electrolyte. The calibration plots for Tl(Ⅰ) concentration in the range of 2×10 -9 -1×10 -7 mol/L were obtained. The detection limit was 5×10 -10 mol/L. For the solutions of 4 0×10 -9 mol/L thallium added before the urine sample pretreatment procedure, the average recovery was 105 6% with a relative standard deviation(RSD) of 15 5%.展开更多
Silver(Ⅰ) oxide was applied to the selective p-tosylation of hydroxyls of saccharide. The reaction of p-methylphenyl-4,6-O-benzylidene-1-thio-β-D-glucopyranoside(A) with a stoichiometric amount of p-toluenesulfo...Silver(Ⅰ) oxide was applied to the selective p-tosylation of hydroxyls of saccharide. The reaction of p-methylphenyl-4,6-O-benzylidene-1-thio-β-D-glucopyranoside(A) with a stoichiometric amount of p-toluenesulfonyl chloride(TsCl) in the presence of silver(Ⅰ) oxide and a catalytic amount of potassium iodide selectively led to the monotosylate derivative:p-methylphenyl 3-O-p-toluenesulfonyl-4,6-O-benzylidene-1-thio-β-D-glucopyranoside(B) in a high yield(97%). A possible mechanism of the reaction is proposed. The rational reaction process is that at n(TsCl)∶n(Ag2O)∶n(A)∶n(KI)=1.2∶1.5∶1.0∶0.2, the mixture is stirred at room temperature for 8 h, 2.74 g(97%)B could be isolated from 2.0 g of compound A.展开更多
The reaction of 2-nitro-(2-pyridylsulfanylmethyl)benzene L with silver nitrate produces a centrosymmetric binuclear complex bis(2-nitro-(2-pyridylsulfanylmethyl)benzene-N,S)- bis(nitrato-O,O)-disilver(Ⅰ), [...The reaction of 2-nitro-(2-pyridylsulfanylmethyl)benzene L with silver nitrate produces a centrosymmetric binuclear complex bis(2-nitro-(2-pyridylsulfanylmethyl)benzene-N,S)- bis(nitrato-O,O)-disilver(Ⅰ), [AgLNO3]2 1. The crystal is of triclinic, space group PI, with a = 7.383 (3), b = 8.340(3), c = 12..003(4) A, a = 95.069(6), β = 93.498(5), γ = 102.734(6)°, C24H20Ag2N6- O10S2, Mr= 832.32, V = 715.6(4) ,A^3, Z = 1, Dc = 1.931 g/cm^3, F(000) = 412,μ = 1.581 mm^-1, R= 0.0351 and wR = 0.0749 Each silver atom is tetrahedrally coordinated by two O atoms from bidentate nitrate, one S atom from a ligand and one N atom from another ligand. Furthermore, Ag- Ag interactions have been observed in the complex.展开更多
基金supported by the Postdoctoral Science Foundation of Central South University
文摘A new hexanuclear silver (I) compound 2 containing thiosemicarbazone with the group of benzene was synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analysis and fluorescence spectrum. The title compound crystallizes in triclinic, space group P with a = 11.611(3), b = 15.610(5), c = 15.624(7) , α = 113.942(6), β = 104.520(6), γ = 104.230(4)°, V = 2304.1(14) 3, C60H77Ag6N22O4.5S6, Mr = 2018.02, Dc = 1.454 g/cm3, μ(MoKα) = 1.435 mm-1, F(000) = 1005, Z = 1, the final R = 0.0468 and wR = 0.1474 for 6608 observed reflections (I 2σ(I)). In the structure, the S atom of the ligand L2 (L2 = benzaldehyde thiosemicarbazone) served as a triply bridged chelator to connect the six silver atoms into a Ag6L26 cluster. The luminescence property of compound 2 was investigated at room temperature.
基金financially supported by the National Natural Science Foundation of China(No.30300434)the 0utstanding Youth Foundation of Sichuan Province(No.04ZQ026-039).
文摘A series of acyls (Ac, Bz and Ts) were introduced regioselectively to the 2-hydroxyl in methyl and ally 3-O-benzyl-α-L-rhamnopyranosides mediated by silver(I) oxide in the presence of a catalytic amount of potassium iodide in 56-78% yields.
基金supported by the Science Foundation of Suihua University (K1001005)
文摘The title complex,[Ag 2 (L1) 2 (Pyr)·2.5H 2 O] 1 (L1=6-amino-1-naphthalenesulfonate anion,Pyr=pyrazine),has been synthesized and characterized by single-crystal X-ray diffraction analysis.It crystallizes in triclinic,space group P1,with a=7.339(5),b=13.105(5),c=14.097(5),α=84.377(5),β=76.921(5),γ=79.628(5)°,V=1296.7(11) 3,C 48 H 50 Ag 4 N 8 O 17 S 4,M r=1570.68,Z=1,D c=2.011 g/cm 3,μ=1.732 mm-1,F(000)=782,S=1.148,the final R=0.0436 and wR=0.1181 for 4130 observer reflections (I 2σ(Ⅰ)).Compound 1 shows a rare one-dimensional (1D) double chain,and the chains are further connected through secondary bonding,hydrogen bonds,and π-π interactions to generate a three-dimensional (3D) supramolecular structure.The luminescent property of 1 was also studied in the solid state at room temperture.
文摘The cyclic voltammetry(CV) and the square wave technique were used for the investigations of thallium(Ⅰ) underpotential deposition(UPD) on the silver electrode. A solution of 10 \{mmol/L\} HClO 4+10 mmol/L NaCl was selected as the supporting electrolyte. The calibration plots for Tl(Ⅰ) concentration in the range of 2×10 -9 -1×10 -7 mol/L were obtained. The detection limit was 5×10 -10 mol/L. For the solutions of 4 0×10 -9 mol/L thallium added before the urine sample pretreatment procedure, the average recovery was 105 6% with a relative standard deviation(RSD) of 15 5%.
文摘Silver(Ⅰ) oxide was applied to the selective p-tosylation of hydroxyls of saccharide. The reaction of p-methylphenyl-4,6-O-benzylidene-1-thio-β-D-glucopyranoside(A) with a stoichiometric amount of p-toluenesulfonyl chloride(TsCl) in the presence of silver(Ⅰ) oxide and a catalytic amount of potassium iodide selectively led to the monotosylate derivative:p-methylphenyl 3-O-p-toluenesulfonyl-4,6-O-benzylidene-1-thio-β-D-glucopyranoside(B) in a high yield(97%). A possible mechanism of the reaction is proposed. The rational reaction process is that at n(TsCl)∶n(Ag2O)∶n(A)∶n(KI)=1.2∶1.5∶1.0∶0.2, the mixture is stirred at room temperature for 8 h, 2.74 g(97%)B could be isolated from 2.0 g of compound A.
基金The Science Foundation of University of Science and Technology of Suzhou
文摘The reaction of 2-nitro-(2-pyridylsulfanylmethyl)benzene L with silver nitrate produces a centrosymmetric binuclear complex bis(2-nitro-(2-pyridylsulfanylmethyl)benzene-N,S)- bis(nitrato-O,O)-disilver(Ⅰ), [AgLNO3]2 1. The crystal is of triclinic, space group PI, with a = 7.383 (3), b = 8.340(3), c = 12..003(4) A, a = 95.069(6), β = 93.498(5), γ = 102.734(6)°, C24H20Ag2N6- O10S2, Mr= 832.32, V = 715.6(4) ,A^3, Z = 1, Dc = 1.931 g/cm^3, F(000) = 412,μ = 1.581 mm^-1, R= 0.0351 and wR = 0.0749 Each silver atom is tetrahedrally coordinated by two O atoms from bidentate nitrate, one S atom from a ligand and one N atom from another ligand. Furthermore, Ag- Ag interactions have been observed in the complex.