Rare earth co-permeation of （NH4）3[CrMo6O24H6]·7H2O was reported and the conductivity of （NH4）3[CrMo6O24H6] was improved by 6.734×10^9 times. X-ray fluorescence spectrometry （XRF）, thermogravimetry-dif...Rare earth co-permeation of （NH4）3[CrMo6O24H6]·7H2O was reported and the conductivity of （NH4）3[CrMo6O24H6] was improved by 6.734×10^9 times. X-ray fluorescence spectrometry （XRF）, thermogravimetry-differential thermal analysis （TG-DTA）, X-ray diffraction （XRD） have been used to character （NH4）3[CrMo6O24H6]·7H2O and permeated sample. Experimental results showed that Nd could be permeated into the body of this sample and the XRD patterns showed great difference between （NH4）3[CrMo6O24H6]·7H2O and permeated sample. The structure of （NH4）3[CrMo6O24H6]·7H2O was destroyed and new compound MoN perhaps formed.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
利用水热合成法合成了分子组成为(C6H11NH3)5H(P2Mo5O23)4H2O的杂多化合物, 用单晶X-ray衍射方法测定了它的结构,该晶体属于单斜晶系,空间群P21/c, a = 12.830(3), b = 14.848(3), c = 25.258(5) ? b = 92.95(3), Mr = 1483.62, V = 48...利用水热合成法合成了分子组成为(C6H11NH3)5H(P2Mo5O23)4H2O的杂多化合物, 用单晶X-ray衍射方法测定了它的结构,该晶体属于单斜晶系,空间群P21/c, a = 12.830(3), b = 14.848(3), c = 25.258(5) ? b = 92.95(3), Mr = 1483.62, V = 4805.1(17) 3, Z = 4, Dc = 2.051 g/cm3, m = 1.431 mm-1, F(000) = 3000, I >2s(I) 的可观察衍射点4426个, 最终结构偏差因子R = 0.0464, wR = 0.0801, S = 0.731。在[P2Mo5O23]6-杂多阴离子中5个MoO6八面体通过共边和共角相连, 形成1个近似的五角平面骨架, 2个PO4四面体加在五角平面的两侧。热性质研究表明杂多阴离子骨架在547.4 ℃左右分解。展开更多
The compleo (H 2 O) 4 (3,3’-azpy)(3,3’-azpy) 3 (PF 6 )2 n (3,3’-azpy =3,3’-azobispyridine)has been synthesized and characterized.The crystal(C 40 H 40 F 12 CoN 16 O 4 P 2 ,M r =1157.75)belongs to the triclinic sys...The compleo (H 2 O) 4 (3,3’-azpy)(3,3’-azpy) 3 (PF 6 )2 n (3,3’-azpy =3,3’-azobispyridine)has been synthesized and characterized.The crystal(C 40 H 40 F 12 CoN 16 O 4 P 2 ,M r =1157.75)belongs to the triclinic system,space groupP1with the following crystallographi c parameters:a=10.759(2),b=11.012(2),c=23.207(4)?;α=85.330(10),β=83.470(10),γ=69.770(10)°;V=2560.6(8)? 3 ,D c =1.502g·cm -3 ,μ(Mo Kα)=0.498mm -1 ,F(000)=1178,Z =2,and final R 1 =0.0469,w R 2 =0.1053for observed reflections 5549(I>2.00σ(I)).The X-ray analysis reveals that cob alt?cation coordination environment is a distorted octahedral geometry,the Co 2+ ion is coordinated by four oxygen ato ms of water in the equatorial plane,while the two nitrogen atoms of 3,3’-azpy occupy the axial positions.The complex forms a one-di mensional chain structure via3,3’-azpy bridging ligand.The one-dimension al chain forms three-dimensional network by hydrogen bonds andπ-πinter-actions.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
基金the Key Science and Technology Foundation of Heilongjiang Province(Grant No.GB02A301) National Natural Science Foundation of China(Grant No.2037101)
文摘Rare earth co-permeation of （NH4）3[CrMo6O24H6]·7H2O was reported and the conductivity of （NH4）3[CrMo6O24H6] was improved by 6.734×10^9 times. X-ray fluorescence spectrometry （XRF）, thermogravimetry-differential thermal analysis （TG-DTA）, X-ray diffraction （XRD） have been used to character （NH4）3[CrMo6O24H6]·7H2O and permeated sample. Experimental results showed that Nd could be permeated into the body of this sample and the XRD patterns showed great difference between （NH4）3[CrMo6O24H6]·7H2O and permeated sample. The structure of （NH4）3[CrMo6O24H6]·7H2O was destroyed and new compound MoN perhaps formed.
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The compleo (H 2 O) 4 (3,3’-azpy)(3,3’-azpy) 3 (PF 6 )2 n (3,3’-azpy =3,3’-azobispyridine)has been synthesized and characterized.The crystal(C 40 H 40 F 12 CoN 16 O 4 P 2 ,M r =1157.75)belongs to the triclinic system,space groupP1with the following crystallographi c parameters:a=10.759(2),b=11.012(2),c=23.207(4)?;α=85.330(10),β=83.470(10),γ=69.770(10)°;V=2560.6(8)? 3 ,D c =1.502g·cm -3 ,μ(Mo Kα)=0.498mm -1 ,F(000)=1178,Z =2,and final R 1 =0.0469,w R 2 =0.1053for observed reflections 5549(I>2.00σ(I)).The X-ray analysis reveals that cob alt?cation coordination environment is a distorted octahedral geometry,the Co 2+ ion is coordinated by four oxygen ato ms of water in the equatorial plane,while the two nitrogen atoms of 3,3’-azpy occupy the axial positions.The complex forms a one-di mensional chain structure via3,3’-azpy bridging ligand.The one-dimension al chain forms three-dimensional network by hydrogen bonds andπ-πinter-actions.
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.
