ZHOU Bai-Bin *,1,2 WEI Yong-De 1 LI Zhong-Hua 1 ( 1 Department of Applied Chemistry,Ha rbin Institute of Technology ￡?Harbin￡±￡ì￡°￡°￡°￡±￡(c)( 2 Department of Chemistry,Harbin Norm...ZHOU Bai-Bin *,1,2 WEI Yong-De 1 LI Zhong-Hua 1 ( 1 Department of Applied Chemistry,Ha rbin Institute of Technology ￡?Harbin￡±￡ì￡°￡°￡°￡±￡(c)( 2 Department of Chemistry,Harbin Normal University￡?Harbin￡±￡ì￡°￡°￡?￡°￡(c) The air-solid interface reaction of Ce,Lu with K10 H 3[Gd (SiMo 4 W￡*O￡3￡1￡(c) 2]through chemistry-heated permeation is reported for the fi rst time￡(r)The permeated complex is characterized by ICP and the result shows tha t the mini mum Ce,Lu can permeate into the inner sph ere of K 10 H ￡3 ￡?Gd ￡¨SiMo ￡′ W ￡* O ￡3￡1 ￡(c) 2]The IR ,XRD patterns give the eviden ce that after permeation the comple x still keeps the Keggin structure,howe ver,its crystal structure is different from the complex before permeation￡(r)The cond uctivity of the permeated complex has been measured with the four-electr ode method and the data show that the co nductivity of the complex after permeation is 10 6 times higher than that of the sample before permeation and reaches ￡′￡(r)84 6×10 -1 S·cm -1 ￡(r)These indicate that the permeated c omplex is a good solid electrolyte and further appli cations are also expected￡(r)展开更多
Two new Gd Ⅲ complexes with nitrilotriacetic acid(nta) and trans-1,2-cyclohexanediaminetetraacetic acid(Cydta) ligands were synthesized. Their crystal structures were determined by single-crystal X-ray structure anal...Two new Gd Ⅲ complexes with nitrilotriacetic acid(nta) and trans-1,2-cyclohexanediaminetetraacetic acid(Cydta) ligands were synthesized. Their crystal structures were determined by single-crystal X-ray structure analyses. The crystal data are as follows: K 3[Gd Ⅲ(nta) 2·(H 2O)]·6H 2O, monoclinic system, C2/c space group, a=1.534 81(15) nm, b=1.292 05(12) nm, c=2.610 8(3) nm, β=96.244(2)°, V=5.146 7(9) nm 3, Z=8, M=776.87, D c=2.005 g/cm 3, μ= 3.149 mm -1 and \{F(000)=\}3 080, R=0.024 5, wR=0.064 3 for 4 455 unique reflections and R= 0.028 9, wR=0.067 2 for all 10 305 reflections. The Gd ⅢN 2O 7 part in the [Gd Ⅲ(nta) 2(H 2O)] 3- anion is a pseudo-monocapped square antiprismatic nine-coordination structure.(NH 4)[Gd Ⅲ(Cydta)(H 2O) 2]·5H 2O, triclinic system, P1 space group, a=0.866 2(3) nm, b=1.006 7(3) nm, c= 1.444 8(5) nm, α= 88.282(5)°, β=75\^190(5)°, γ=88.317(4)°, V=1.217 2(7) nm 3, Z=2, M=643.69, D c=1.756 g/cm 3, μ=2.798 mm -1 and F(000)=650, R=0.030 3, wR=0.080 9 for 4 273 unique reflections and R=0.033 2, wR=0.082 5 for all 5 062 reflections. The Gd ⅢN 2O 6 part in the [Gd Ⅲ(Cydta)(H 2O) 2] - anion has a pseudo-square antiprismatic eight-coordination structure.展开更多
A new magnesium borate MgO·3B 2 O 3 ·3.5H 2 O has been synthesized by the method o f phase transformation of 2MgO·2B 2 O 3 ·MgCl 2 ·14H 2 O in boric acid solution and characte rized by XRD,FT-...A new magnesium borate MgO·3B 2 O 3 ·3.5H 2 O has been synthesized by the method o f phase transformation of 2MgO·2B 2 O 3 ·MgCl 2 ·14H 2 O in boric acid solution and characte rized by XRD,FT-IR and Raman spectra as well as by TG.The structural formula of this compound was Mg[B 6 O 9 (OH) 2 ]·2.5H 2 O.The main polyborate anions and their interaction in borate aqueous solution of preparation reactio n have been proposed according to the Raman spectrum of borate solution.The relation between the existing forms of polyborate anions and the crystalliz ing solid phase has been gained.展开更多
A protocol for the synthesis of some 4-Aryl-1,3,4,6,7,8-hexahydroquinazolin-2,5(1H,6H)-diones (HHQs) was developed by means of a three-component condensation reaction of an aromatic aldehyde, 1,3-cylohexadione and ure...A protocol for the synthesis of some 4-Aryl-1,3,4,6,7,8-hexahydroquinazolin-2,5(1H,6H)-diones (HHQs) was developed by means of a three-component condensation reaction of an aromatic aldehyde, 1,3-cylohexadione and urea in the presence of K3AlF6 (Al2O3/KF) as catalyst. This reaction is carried out under different conditions including 1) solvent free;2) reflux in acetonitrile;3) reflux in ethanol;4) reflux in chloroform;and 5) reflux in water. In all conditions, the desired products are obtained in high yields after relatively short reaction times. Nevertheless, the reactions proceed faster and in higher yields when they were carried out in acetonitrile. This adopted protocol for some Biginelli-type products has offered the advantages of reusability of the catalyst, high yields and ease of separation of pure products. Furthermore, the catalyst is easily prepared, stabilized and efficiently used under reaction conditions.展开更多
文摘ZHOU Bai-Bin *,1,2 WEI Yong-De 1 LI Zhong-Hua 1 ( 1 Department of Applied Chemistry,Ha rbin Institute of Technology ￡?Harbin￡±￡ì￡°￡°￡°￡±￡(c)( 2 Department of Chemistry,Harbin Normal University￡?Harbin￡±￡ì￡°￡°￡?￡°￡(c) The air-solid interface reaction of Ce,Lu with K10 H 3[Gd (SiMo 4 W￡*O￡3￡1￡(c) 2]through chemistry-heated permeation is reported for the fi rst time￡(r)The permeated complex is characterized by ICP and the result shows tha t the mini mum Ce,Lu can permeate into the inner sph ere of K 10 H ￡3 ￡?Gd ￡¨SiMo ￡′ W ￡* O ￡3￡1 ￡(c) 2]The IR ,XRD patterns give the eviden ce that after permeation the comple x still keeps the Keggin structure,howe ver,its crystal structure is different from the complex before permeation￡(r)The cond uctivity of the permeated complex has been measured with the four-electr ode method and the data show that the co nductivity of the complex after permeation is 10 6 times higher than that of the sample before permeation and reaches ￡′￡(r)84 6×10 -1 S·cm -1 ￡(r)These indicate that the permeated c omplex is a good solid electrolyte and further appli cations are also expected￡(r)
文摘Two new Gd Ⅲ complexes with nitrilotriacetic acid(nta) and trans-1,2-cyclohexanediaminetetraacetic acid(Cydta) ligands were synthesized. Their crystal structures were determined by single-crystal X-ray structure analyses. The crystal data are as follows: K 3[Gd Ⅲ(nta) 2·(H 2O)]·6H 2O, monoclinic system, C2/c space group, a=1.534 81(15) nm, b=1.292 05(12) nm, c=2.610 8(3) nm, β=96.244(2)°, V=5.146 7(9) nm 3, Z=8, M=776.87, D c=2.005 g/cm 3, μ= 3.149 mm -1 and \{F(000)=\}3 080, R=0.024 5, wR=0.064 3 for 4 455 unique reflections and R= 0.028 9, wR=0.067 2 for all 10 305 reflections. The Gd ⅢN 2O 7 part in the [Gd Ⅲ(nta) 2(H 2O)] 3- anion is a pseudo-monocapped square antiprismatic nine-coordination structure.(NH 4)[Gd Ⅲ(Cydta)(H 2O) 2]·5H 2O, triclinic system, P1 space group, a=0.866 2(3) nm, b=1.006 7(3) nm, c= 1.444 8(5) nm, α= 88.282(5)°, β=75\^190(5)°, γ=88.317(4)°, V=1.217 2(7) nm 3, Z=2, M=643.69, D c=1.756 g/cm 3, μ=2.798 mm -1 and F(000)=650, R=0.030 3, wR=0.080 9 for 4 273 unique reflections and R=0.033 2, wR=0.082 5 for all 5 062 reflections. The Gd ⅢN 2O 6 part in the [Gd Ⅲ(Cydta)(H 2O) 2] - anion has a pseudo-square antiprismatic eight-coordination structure.
文摘A new magnesium borate MgO·3B 2 O 3 ·3.5H 2 O has been synthesized by the method o f phase transformation of 2MgO·2B 2 O 3 ·MgCl 2 ·14H 2 O in boric acid solution and characte rized by XRD,FT-IR and Raman spectra as well as by TG.The structural formula of this compound was Mg[B 6 O 9 (OH) 2 ]·2.5H 2 O.The main polyborate anions and their interaction in borate aqueous solution of preparation reactio n have been proposed according to the Raman spectrum of borate solution.The relation between the existing forms of polyborate anions and the crystalliz ing solid phase has been gained.
文摘A protocol for the synthesis of some 4-Aryl-1,3,4,6,7,8-hexahydroquinazolin-2,5(1H,6H)-diones (HHQs) was developed by means of a three-component condensation reaction of an aromatic aldehyde, 1,3-cylohexadione and urea in the presence of K3AlF6 (Al2O3/KF) as catalyst. This reaction is carried out under different conditions including 1) solvent free;2) reflux in acetonitrile;3) reflux in ethanol;4) reflux in chloroform;and 5) reflux in water. In all conditions, the desired products are obtained in high yields after relatively short reaction times. Nevertheless, the reactions proceed faster and in higher yields when they were carried out in acetonitrile. This adopted protocol for some Biginelli-type products has offered the advantages of reusability of the catalyst, high yields and ease of separation of pure products. Furthermore, the catalyst is easily prepared, stabilized and efficiently used under reaction conditions.
