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
The bis-benzimidazolium salt bis[2-（N-ethylbenzimidazoliumyl）ethyl]amine hexafluorophosphate（LH2·（PF6）2） and its N-heterocyclic carbene silver（Ⅰ） complex[L2Ag3]（PF6）3（1）have been prepared and charact...The bis-benzimidazolium salt bis[2-（N-ethylbenzimidazoliumyl）ethyl]amine hexafluorophosphate（LH2·（PF6）2） and its N-heterocyclic carbene silver（Ⅰ） complex[L2Ag3]（PF6）3（1）have been prepared and characterized.In complex 1,a trinuclear silver（Ⅰ） architecture is formed by two tridentate ligands and three silver（I） atoms,in which one 12- and two 7-membered rings are contained.In the crystal packing of 1,1D chain and 2D supramolecular layer are formed via intermolecular weak interactions,including π…π interactions and C-H…π contacts.Additionally,the fluorescence emission spectra of LH2-（PF6）2 and 1 are described.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
A new silver complex salt [Ag(N2C11H10)2]NO3 (where N2C11H10 = 4,5-dihydro-1H-benzo[g]indazole), has been synthesized and characterized by elemental and thermal analyses, IR and 1HNMR spectroscopies, single crystal X-...A new silver complex salt [Ag(N2C11H10)2]NO3 (where N2C11H10 = 4,5-dihydro-1H-benzo[g]indazole), has been synthesized and characterized by elemental and thermal analyses, IR and 1HNMR spectroscopies, single crystal X-ray structure determination and DFT studies. Its molecular structure comprises of a silver center coordinated to two nitrogen atoms from two 4,5-dihydro-1H-benzo[g]indazole molecule giving rise to a cationic complex entity, [Ag(N2C11H10)2]+ with as counter ion. The bulk structure is consolidated by N–H…O, C–H…π, Ag…π and Ag…O intermolecular interactions, thus generating a pseudo-helical network. The optimized structure, frontier molecular orbitals (HOMO and LUMO) and global reactivity descriptors were investigated by performing DFT calculations.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
The new salt bis(4,5-dihydro-1H-benzo[g]indazole)silver(I) hexafluorophosphate, [Ag(N2H10C11)2]PF6, has been synthesized in methanol at ambient temperature and characterized by elemental and thermal analyses, FTIR and...The new salt bis(4,5-dihydro-1H-benzo[g]indazole)silver(I) hexafluorophosphate, [Ag(N2H10C11)2]PF6, has been synthesized in methanol at ambient temperature and characterized by elemental and thermal analyses, FTIR and 1HNMR spectroscopies, Rietveld refinement from powder diffraction data and DFT studies. The salt crystallizes in the triclinic space group P-1 with the parameters: a = 7.776 ?, b = 8.676 ?, c = 9.226 ?, α = 69.27° β = 89.86°, γ = 74.50°, V = 558.02 ?3, Z = 1. In the structure, the silver center is coordinated to two nitrogen atoms from two 4,5-dihydro-1H-benzo[g]indazole ligands, forming a centrosymmetric complex cation, [Ag(N2H10C11)2]+, with a linear coordination geometry around the silver center. The hexafluorophosphate ion, , acts as counter anion. The crystal packing is governed by N-H···F and C-H···F hydrogen bonds that interconnect the ionic constituents and Ag···F and Ag···π interactions help for the stabilization of the packing. The optimized structure was obtained at B3LYP/LanL2DZ level in the gas phase. The stability and reactivity of the structure were studied using respectively HOMO-LUMO gap and electronic global quantities (ionization potential (I) and electron affinity (A)) as descriptors.展开更多
Two novel coordination compounds, [Zn（CBPP）2（H2O）2]·3H2O（1） and[Ag（CBPP）·2H2O]（2）（HCBPP = 1-（4？-carboxylatobenzyl）-3-（pyrazin-2-yl）pyrazole）, were hydrothermally synthesized and characterize...Two novel coordination compounds, [Zn（CBPP）2（H2O）2]·3H2O（1） and[Ag（CBPP）·2H2O]（2）（HCBPP = 1-（4？-carboxylatobenzyl）-3-（pyrazin-2-yl）pyrazole）, were hydrothermally synthesized and characterized. Compound 1 crystallizes in monoclinic, space group C2 with a = 26.221（4）, b = 8.4211（7）, c = 14.295（3）A, β = 114.561（8）°, V = 2705.9（2） A3, Dc = 1.587 g/cm3, C28H28Cl2N8O9 Zn, Mr = 685.97 F（000） = 1416, μ（Mo Kα） = 0.926 mm-1, Z = 4, R = 0.0287, w R = 0.1076 for 2818 observed reflections（I 〉 2σ（I））, and R = 0.0300, w R = 0.1110 for all data. In 1, each deprotonated CBPP-ligand with a bidentate coordination mode connects two Zn（II） atoms to generate a 1D helical chain along the b axis. The adjacent chains intersect with each other through hinged Zn（II） ions to build up an interesting two-dimensional network. Compound 2 crystallizes in monoclinic, space group P21/n with a = 6.3544（1）, b = 11.7195（3）, c = 19.3188（4）A, β = 94.297（2）°, V = 1434.64（5） A3, Dc = 1.894 g/cm3, C14H13 Ag N4O4, Mr = 409.15 F（000） = 816, μ（Mo Kα） = 11.536 mm-1, Z = 4, R = 0.0456 and w R = 0.1184 for 2402 observed reflections（I 〉 2σ（I））, and R = 0.0517, w R = 0.1275 for all data. In 2, each ligand binds two Ag（I） atoms in a tridentate coordination mode to form an infinite zigzag chain. Their thermal and photoluminescent properties were also investigated.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
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supported by the National Natural Science Foundation of China(No.21172172)Tianjin Natural Science Foundation(No.11JCZDJC22000)the Program for Innovative Research Team in University of Tianjin(TD12-5038)
文摘The bis-benzimidazolium salt bis[2-（N-ethylbenzimidazoliumyl）ethyl]amine hexafluorophosphate（LH2·（PF6）2） and its N-heterocyclic carbene silver（Ⅰ） complex[L2Ag3]（PF6）3（1）have been prepared and characterized.In complex 1,a trinuclear silver（Ⅰ） architecture is formed by two tridentate ligands and three silver（I） atoms,in which one 12- and two 7-membered rings are contained.In the crystal packing of 1,1D chain and 2D supramolecular layer are formed via intermolecular weak interactions,including π…π interactions and C-H…π contacts.Additionally,the fluorescence emission spectra of LH2-（PF6）2 and 1 are described.
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A new silver complex salt [Ag(N2C11H10)2]NO3 (where N2C11H10 = 4,5-dihydro-1H-benzo[g]indazole), has been synthesized and characterized by elemental and thermal analyses, IR and 1HNMR spectroscopies, single crystal X-ray structure determination and DFT studies. Its molecular structure comprises of a silver center coordinated to two nitrogen atoms from two 4,5-dihydro-1H-benzo[g]indazole molecule giving rise to a cationic complex entity, [Ag(N2C11H10)2]+ with as counter ion. The bulk structure is consolidated by N–H…O, C–H…π, Ag…π and Ag…O intermolecular interactions, thus generating a pseudo-helical network. The optimized structure, frontier molecular orbitals (HOMO and LUMO) and global reactivity descriptors were investigated by performing DFT calculations.
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The new salt bis(4,5-dihydro-1H-benzo[g]indazole)silver(I) hexafluorophosphate, [Ag(N2H10C11)2]PF6, has been synthesized in methanol at ambient temperature and characterized by elemental and thermal analyses, FTIR and 1HNMR spectroscopies, Rietveld refinement from powder diffraction data and DFT studies. The salt crystallizes in the triclinic space group P-1 with the parameters: a = 7.776 ?, b = 8.676 ?, c = 9.226 ?, α = 69.27° β = 89.86°, γ = 74.50°, V = 558.02 ?3, Z = 1. In the structure, the silver center is coordinated to two nitrogen atoms from two 4,5-dihydro-1H-benzo[g]indazole ligands, forming a centrosymmetric complex cation, [Ag(N2H10C11)2]+, with a linear coordination geometry around the silver center. The hexafluorophosphate ion, , acts as counter anion. The crystal packing is governed by N-H···F and C-H···F hydrogen bonds that interconnect the ionic constituents and Ag···F and Ag···π interactions help for the stabilization of the packing. The optimized structure was obtained at B3LYP/LanL2DZ level in the gas phase. The stability and reactivity of the structure were studied using respectively HOMO-LUMO gap and electronic global quantities (ionization potential (I) and electron affinity (A)) as descriptors.
基金financially supported by the National Natural Science Foundation of China(21571034)the Natural Science Foundation of Fujian Province(2014J01033)
文摘Two novel coordination compounds, [Zn（CBPP）2（H2O）2]·3H2O（1） and[Ag（CBPP）·2H2O]（2）（HCBPP = 1-（4？-carboxylatobenzyl）-3-（pyrazin-2-yl）pyrazole）, were hydrothermally synthesized and characterized. Compound 1 crystallizes in monoclinic, space group C2 with a = 26.221（4）, b = 8.4211（7）, c = 14.295（3）A, β = 114.561（8）°, V = 2705.9（2） A3, Dc = 1.587 g/cm3, C28H28Cl2N8O9 Zn, Mr = 685.97 F（000） = 1416, μ（Mo Kα） = 0.926 mm-1, Z = 4, R = 0.0287, w R = 0.1076 for 2818 observed reflections（I 〉 2σ（I））, and R = 0.0300, w R = 0.1110 for all data. In 1, each deprotonated CBPP-ligand with a bidentate coordination mode connects two Zn（II） atoms to generate a 1D helical chain along the b axis. The adjacent chains intersect with each other through hinged Zn（II） ions to build up an interesting two-dimensional network. Compound 2 crystallizes in monoclinic, space group P21/n with a = 6.3544（1）, b = 11.7195（3）, c = 19.3188（4）A, β = 94.297（2）°, V = 1434.64（5） A3, Dc = 1.894 g/cm3, C14H13 Ag N4O4, Mr = 409.15 F（000） = 816, μ（Mo Kα） = 11.536 mm-1, Z = 4, R = 0.0456 and w R = 0.1184 for 2402 observed reflections（I 〉 2σ（I））, and R = 0.0517, w R = 0.1275 for all data. In 2, each ligand binds two Ag（I） atoms in a tridentate coordination mode to form an infinite zigzag chain. Their thermal and photoluminescent properties were also investigated.
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.
