A novel one-dimensional chain complex [Zn(dafo)2(H2O)2](NO3)2 was synthesized. It has been characterized by IR, UV, TGA, Elemental analysis and X-ray diffraction analysis. The crystal belongs to triclinic system, P1 s...A novel one-dimensional chain complex [Zn(dafo)2(H2O)2](NO3)2 was synthesized. It has been characterized by IR, UV, TGA, Elemental analysis and X-ray diffraction analysis. The crystal belongs to triclinic system, P1 space group. The Crystallographic data are: a = 0.702 7(14) nm, b = 0.828 95(17) nm, c = 10.225(2) nm, α = 95.02(3)°, β = 91.45(3)°, γ = 99.85(3)°. The crystal structure data indicate that the Zn(Ⅱ) ion was coordinated with the four nitrogen atoms of two dafo and two oxygen atoms of two coordination water molecules, respectively. The complex has a one-dimensional chain structure, which is formed by hydrogen bonds.展开更多
The novel polyoxometalate, 32[Mo8ⅣMo4ⅤV2ⅣO38(PO4)], was synthesized and characterized by elementary analysis, EPR, IR spectra and X ray diffraction. The compoundcrystallizes in triclinic system, space group with a=...The novel polyoxometalate, 32[Mo8ⅣMo4ⅤV2ⅣO38(PO4)], was synthesized and characterized by elementary analysis, EPR, IR spectra and X ray diffraction. The compoundcrystallizes in triclinic system, space group with a= 1.41999(2)nm, b=1.43467(2)nm, c=1.694610(10)nm, α=95.7250(10)°, β=92.2110(10)°, γ=92.6060(10)°, V=3.42829(7)nm3, Z=2, Dc=2.388g·cm-3, Mr=2465.10g·mol-1, μ=2.489mm-1, F(000)=2388, R1=0.0584, wR2=0.1461, S=1.164. The heteropolyanion is a bi capped pseudo Keggin complex. CCDC: 186645.展开更多
A nanosolid heteropoly acid of H 3PW 12 O 40 /SiO 2 was prepared with the sol-gel method and used to catalyze sythesis of methyl 5-amino-1,2,4,-trazolylformate sulfate.The structure of the nanosolid heteropoly acid H ...A nanosolid heteropoly acid of H 3PW 12 O 40 /SiO 2 was prepared with the sol-gel method and used to catalyze sythesis of methyl 5-amino-1,2,4,-trazolylformate sulfate.The structure of the nanosolid heteropoly acid H 3PW 12 O 40 /SiO 2 was characterized by IR,XRD and TEM.The following optimum condition were that the mole ratio of alcohol to carboxylic acid is 27∶1,the temperature is 75℃,the reaction time is 5 hours,and the catalyst is 2 5% of feedstock.Under the optimum conditions,the yield of esters was above 94%.展开更多
A novel flower-like hydrated magnesium carbonate hydroxide, Mg5 (CO3 )4 (OH)2·4H2O, with micro-structure composed of individual thin nano-sheets was synthesized using a facile solution route without the use o...A novel flower-like hydrated magnesium carbonate hydroxide, Mg5 (CO3 )4 (OH)2·4H2O, with micro-structure composed of individual thin nano-sheets was synthesized using a facile solution route without the use of template or organic surfactant. Reaction time has an important effect on the final morphology of the product. The micro-structure and morphology of Mg5 (CO3)4 (OH)2·4H2O were characterized by means of X-ray diffractometry (XRD), fieldemission scanning electron microscopy(FE-SEM). Brunauer-Emmett-Teller(BET) surface areas of the samples were also measured. The probable formation mechanism of flower-like micro-structure was discussed. It was found that Mg5 (CO3)4( OH)2·4H2O with flower-like micro-structure was a novel and efficient catalyst for the synthesis of diphenyl carbonate (DPC) by transesterification of dimethyl carbonate (DMC) with phenol.展开更多
Both whisker and nanometer MgSO4·5Mg(OH)2·3H2O(MOS) were prepared by hydrothermal method at 140℃for different times, using NaOH and MgSO4·7H2O as raw materials. The MgSO4·5Mg(OH)2·3H2O part i...Both whisker and nanometer MgSO4·5Mg(OH)2·3H2O(MOS) were prepared by hydrothermal method at 140℃for different times, using NaOH and MgSO4·7H2O as raw materials. The MgSO4·5Mg(OH)2·3H2O part icles were characterized by powder X ray diffraction(XRD),thermal analysis(TGA DSC), infrared spectroscopy(FT IR),transmission electron microscopy(SEM) and scanning electron microscopy(TEM). The size distribution in whisker like and nanocrystalline materials arein the range of 10~50μm and 10~20nm respectively. The whisker MOS is metastable phase in MgSO4 NaOH H2O system at 140℃,whereas nanometer MOS is stable phase.展开更多
Compound [Co 3(BTC)(HBTC)(H 2BTC)(C 2H 4O 2) 3]·3(DMF)·6(H 3O) was synthesized under mild conditions and its crystal structure was determined by using single crystal X-ray diffraction. The crystal structure ...Compound [Co 3(BTC)(HBTC)(H 2BTC)(C 2H 4O 2) 3]·3(DMF)·6(H 3O) was synthesized under mild conditions and its crystal structure was determined by using single crystal X-ray diffraction. The crystal structure was solved by direct method and refined by full-matrix least-square method. The crystal is monoclinic and belongs to space group Cc with a=2.645 3(5) nm, b= 1.670 4(3) nm, c=1\^821 6(4) nm, β=128.16(3) °, V=6.329(2) nm 3, Z=2 , D c=20.200 Mg/m 3, M r= 1 314.744, μ=10.274 mm -1, F(000) =38 226, GOF=0.99, R=0.094 1, ωR=0.257 3.展开更多
PhCH2)3Sn·(O2CC5H4N)·(H2O)]n was synthesized by the reaction of 4-pyridine car-boxylic acid with the tribenzyltin o xide and was characterized by IR,1 H NMR and MS.Its crystal structure was determined by X-r...PhCH2)3Sn·(O2CC5H4N)·(H2O)]n was synthesized by the reaction of 4-pyridine car-boxylic acid with the tribenzyltin o xide and was characterized by IR,1 H NMR and MS.Its crystal structure was determined by X-ray single crystal diffraction.The crystal belongs to monoclinic.The space group P21 /c with unit cell parameters a=1.2241(8)nm,b=0.9660(6)nm,c=2.3708(15)nm,β=102.722(12)°,V=2.734(3)nm3,Z =4,Dc=1.298g·cm-3 .In crystal,the tin atom rendered five-coordinate in a trigo nal bipyramidal structure which is b ridged by 4-pyridine carboxy-late into one-dimensional chain polymers.展开更多
Solubilities and properties (density, conductivity and pH value) of solutions in the quaternary system Li +,K +//CO 2- 3,B 4O 2- 7-H 2O at 288 K were experimentally studied with the isothermal equilibrium method. The ...Solubilities and properties (density, conductivity and pH value) of solutions in the quaternary system Li +,K +//CO 2- 3,B 4O 2- 7-H 2O at 288 K were experimentally studied with the isothermal equilibrium method. The phase diagram of the system consisted of two invariant points E and F, five univariant curves, and four crystallization fields that belonged to K 2CO 3·3/2H 2O,Li 2 B 4O 7·3H 2O, K 2 B 4O 7 ·4H 2O and Li 2CO 3. The composition of the solution corresponding to E was w(CO 2- 3)=2.27 %, w(B 4O 2- 7) =6.05 %, w(K + ) =4.30%,w(Li + )=0.30 % and the equilibrium solids were Li 2 B 4O 7· 3H 2O+K 2 B 4O 7·4H 2O+Li 2CO 3;The composition of the solution for F was w(CO 2- 3) =22.45%,w(B 4O 2- 7)=1.88%,w(K + )=29.96%,w(Li + )=0.03% and the equilibrium solids were K 2CO 3·3/2H 2O+ K 2 B 4O 7·4H 2O+Li 2CO 3. K 2CO 3 possesses strong salting-out effect on K 2 B 4O 7,Li 2CO 3 and Li 2 B 4O 7.展开更多
Nanocrystalline MgSO\-4·5Mg(OH)\-2·3H\-2O were prepared by the hydrothermal reaction at 140 ℃ for 24 h. Nanoparticle samples were characterized by FTIR, TG, DSC, XRD and TEM. The size distribution of nano...Nanocrystalline MgSO\-4·5Mg(OH)\-2·3H\-2O were prepared by the hydrothermal reaction at 140 ℃ for 24 h. Nanoparticle samples were characterized by FTIR, TG, DSC, XRD and TEM. The size distribution of nanocrystalline is in the range of 10\20 nm, the mean size is 16 nm.展开更多
文摘A novel one-dimensional chain complex [Zn(dafo)2(H2O)2](NO3)2 was synthesized. It has been characterized by IR, UV, TGA, Elemental analysis and X-ray diffraction analysis. The crystal belongs to triclinic system, P1 space group. The Crystallographic data are: a = 0.702 7(14) nm, b = 0.828 95(17) nm, c = 10.225(2) nm, α = 95.02(3)°, β = 91.45(3)°, γ = 99.85(3)°. The crystal structure data indicate that the Zn(Ⅱ) ion was coordinated with the four nitrogen atoms of two dafo and two oxygen atoms of two coordination water molecules, respectively. The complex has a one-dimensional chain structure, which is formed by hydrogen bonds.
文摘The novel polyoxometalate, 32[Mo8ⅣMo4ⅤV2ⅣO38(PO4)], was synthesized and characterized by elementary analysis, EPR, IR spectra and X ray diffraction. The compoundcrystallizes in triclinic system, space group with a= 1.41999(2)nm, b=1.43467(2)nm, c=1.694610(10)nm, α=95.7250(10)°, β=92.2110(10)°, γ=92.6060(10)°, V=3.42829(7)nm3, Z=2, Dc=2.388g·cm-3, Mr=2465.10g·mol-1, μ=2.489mm-1, F(000)=2388, R1=0.0584, wR2=0.1461, S=1.164. The heteropolyanion is a bi capped pseudo Keggin complex. CCDC: 186645.
文摘A nanosolid heteropoly acid of H 3PW 12 O 40 /SiO 2 was prepared with the sol-gel method and used to catalyze sythesis of methyl 5-amino-1,2,4,-trazolylformate sulfate.The structure of the nanosolid heteropoly acid H 3PW 12 O 40 /SiO 2 was characterized by IR,XRD and TEM.The following optimum condition were that the mole ratio of alcohol to carboxylic acid is 27∶1,the temperature is 75℃,the reaction time is 5 hours,and the catalyst is 2 5% of feedstock.Under the optimum conditions,the yield of esters was above 94%.
基金2013年国家级大学生创新创业训练计划项目(201313256001)湖北师范学院硕士研究生创新科研基金项目(1051320130216)+1 种基金National Undergraduate Training Programs for Innovation and Entrepreneurship(201313256001)Postgraduate Innovation Scientific Research Foundation of Hubei Normal University(1051320130216)
基金Supported by the National Natural Science Foundation of China(Nos.20671011,20331010,90406002and90406024)the 111 Project(No.B07012)the Key Laboratory of Structural Chemistry Foundation(No.060017).
文摘A novel flower-like hydrated magnesium carbonate hydroxide, Mg5 (CO3 )4 (OH)2·4H2O, with micro-structure composed of individual thin nano-sheets was synthesized using a facile solution route without the use of template or organic surfactant. Reaction time has an important effect on the final morphology of the product. The micro-structure and morphology of Mg5 (CO3)4 (OH)2·4H2O were characterized by means of X-ray diffractometry (XRD), fieldemission scanning electron microscopy(FE-SEM). Brunauer-Emmett-Teller(BET) surface areas of the samples were also measured. The probable formation mechanism of flower-like micro-structure was discussed. It was found that Mg5 (CO3)4( OH)2·4H2O with flower-like micro-structure was a novel and efficient catalyst for the synthesis of diphenyl carbonate (DPC) by transesterification of dimethyl carbonate (DMC) with phenol.
文摘Both whisker and nanometer MgSO4·5Mg(OH)2·3H2O(MOS) were prepared by hydrothermal method at 140℃for different times, using NaOH and MgSO4·7H2O as raw materials. The MgSO4·5Mg(OH)2·3H2O part icles were characterized by powder X ray diffraction(XRD),thermal analysis(TGA DSC), infrared spectroscopy(FT IR),transmission electron microscopy(SEM) and scanning electron microscopy(TEM). The size distribution in whisker like and nanocrystalline materials arein the range of 10~50μm and 10~20nm respectively. The whisker MOS is metastable phase in MgSO4 NaOH H2O system at 140℃,whereas nanometer MOS is stable phase.
文摘Compound [Co 3(BTC)(HBTC)(H 2BTC)(C 2H 4O 2) 3]·3(DMF)·6(H 3O) was synthesized under mild conditions and its crystal structure was determined by using single crystal X-ray diffraction. The crystal structure was solved by direct method and refined by full-matrix least-square method. The crystal is monoclinic and belongs to space group Cc with a=2.645 3(5) nm, b= 1.670 4(3) nm, c=1\^821 6(4) nm, β=128.16(3) °, V=6.329(2) nm 3, Z=2 , D c=20.200 Mg/m 3, M r= 1 314.744, μ=10.274 mm -1, F(000) =38 226, GOF=0.99, R=0.094 1, ωR=0.257 3.
文摘PhCH2)3Sn·(O2CC5H4N)·(H2O)]n was synthesized by the reaction of 4-pyridine car-boxylic acid with the tribenzyltin o xide and was characterized by IR,1 H NMR and MS.Its crystal structure was determined by X-ray single crystal diffraction.The crystal belongs to monoclinic.The space group P21 /c with unit cell parameters a=1.2241(8)nm,b=0.9660(6)nm,c=2.3708(15)nm,β=102.722(12)°,V=2.734(3)nm3,Z =4,Dc=1.298g·cm-3 .In crystal,the tin atom rendered five-coordinate in a trigo nal bipyramidal structure which is b ridged by 4-pyridine carboxy-late into one-dimensional chain polymers.
文摘Solubilities and properties (density, conductivity and pH value) of solutions in the quaternary system Li +,K +//CO 2- 3,B 4O 2- 7-H 2O at 288 K were experimentally studied with the isothermal equilibrium method. The phase diagram of the system consisted of two invariant points E and F, five univariant curves, and four crystallization fields that belonged to K 2CO 3·3/2H 2O,Li 2 B 4O 7·3H 2O, K 2 B 4O 7 ·4H 2O and Li 2CO 3. The composition of the solution corresponding to E was w(CO 2- 3)=2.27 %, w(B 4O 2- 7) =6.05 %, w(K + ) =4.30%,w(Li + )=0.30 % and the equilibrium solids were Li 2 B 4O 7· 3H 2O+K 2 B 4O 7·4H 2O+Li 2CO 3;The composition of the solution for F was w(CO 2- 3) =22.45%,w(B 4O 2- 7)=1.88%,w(K + )=29.96%,w(Li + )=0.03% and the equilibrium solids were K 2CO 3·3/2H 2O+ K 2 B 4O 7·4H 2O+Li 2CO 3. K 2CO 3 possesses strong salting-out effect on K 2 B 4O 7,Li 2CO 3 and Li 2 B 4O 7.
文摘Nanocrystalline MgSO\-4·5Mg(OH)\-2·3H\-2O were prepared by the hydrothermal reaction at 140 ℃ for 24 h. Nanoparticle samples were characterized by FTIR, TG, DSC, XRD and TEM. The size distribution of nanocrystalline is in the range of 10\20 nm, the mean size is 16 nm.