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
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
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 new compound 2 6[Co(H 2O) 2(VO) 8(OH) 4(PO 4) 8] has been hydrothermally synthesized. Single crystal X-ray analysis indicates that this compound crystallizes in a monoclinic system, space group P2 1/n with a=1.438 5...A new compound 2 6[Co(H 2O) 2(VO) 8(OH) 4(PO 4) 8] has been hydrothermally synthesized. Single crystal X-ray analysis indicates that this compound crystallizes in a monoclinic system, space group P2 1/n with a=1.438 5(3) nm, b=1.012 2(2) nm, c=1.832 5(4) nm, β=90.21°, V=2\^668 2(9) nm 3, Z=2, D c=2.112 g/cm 3, R=0.055, wR=0.149 7, S=1.037. The structure of 2 6[Co(H 2O) 2(VO) 8(OH) 4(PO 4) 8] is characterized by P-V-O layers constructed by [(VO) 4(OH) 2(PO 4) 4] 6- non-symmetric units. The P-V-O layers are pillared by [Co(H 2O) 2] 2+ group, resulting in the channels within which the protonated diaminoethane and H 3O + are located.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
A novel three dimensional fluorinated gallium phosphate has been hydrothermally synthesized by using diethylenetriamine as an organic structure directing agent. X ray single crystal structure analysis indicates this c...A novel three dimensional fluorinated gallium phosphate has been hydrothermally synthesized by using diethylenetriamine as an organic structure directing agent. X ray single crystal structure analysis indicates this compound crystallizes in the orthorhombic space group Pbca, a =1.605 6(7) nm, b = 1 011 4 (4) nm, c =1.854 6(5) nm, V =3.011 6(19) nm 3, Z =4. The three dimensional framework based on linkage of corner sharing polyhedron PO 4, GaO 4F and GaO 4F 2 delimit ten ring channels along b axis in which the triply protonated amines are located serving as charge compensating guests and supporters.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
The new mixed borates with formula(Rb 2 Ca [B 4 O 5 (OH) 4 ] 2 ·8H 2 O and Cs 2 Ca [B 4 O 5 (OH) 4 ] 2 ·8H 2 O)were prepared by reaction Rb (Cs )-borate aqueous solution with CaCl 2 .Two kinds of compounds w...The new mixed borates with formula(Rb 2 Ca [B 4 O 5 (OH) 4 ] 2 ·8H 2 O and Cs 2 Ca [B 4 O 5 (OH) 4 ] 2 ·8H 2 O)were prepared by reaction Rb (Cs )-borate aqueous solution with CaCl 2 .Two kinds of compounds were characterized by chemical analysis,X-ray powder dif fraction,FT-IR spectra and thermal analysis.展开更多
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.
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 new compound 2 6[Co(H 2O) 2(VO) 8(OH) 4(PO 4) 8] has been hydrothermally synthesized. Single crystal X-ray analysis indicates that this compound crystallizes in a monoclinic system, space group P2 1/n with a=1.438 5(3) nm, b=1.012 2(2) nm, c=1.832 5(4) nm, β=90.21°, V=2\^668 2(9) nm 3, Z=2, D c=2.112 g/cm 3, R=0.055, wR=0.149 7, S=1.037. The structure of 2 6[Co(H 2O) 2(VO) 8(OH) 4(PO 4) 8] is characterized by P-V-O layers constructed by [(VO) 4(OH) 2(PO 4) 4] 6- non-symmetric units. The P-V-O layers are pillared by [Co(H 2O) 2] 2+ group, resulting in the channels within which the protonated diaminoethane and H 3O + are located.
基金supported by the Fund for Young Scientists of Sichuan University, China (2011SCU11081)Research Fund for the Doctoral Program of Higher Education, Ministry of Education of China (20120181120103)~~
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A novel three dimensional fluorinated gallium phosphate has been hydrothermally synthesized by using diethylenetriamine as an organic structure directing agent. X ray single crystal structure analysis indicates this compound crystallizes in the orthorhombic space group Pbca, a =1.605 6(7) nm, b = 1 011 4 (4) nm, c =1.854 6(5) nm, V =3.011 6(19) nm 3, Z =4. The three dimensional framework based on linkage of corner sharing polyhedron PO 4, GaO 4F and GaO 4F 2 delimit ten ring channels along b axis in which the triply protonated amines are located serving as charge compensating guests and supporters.
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 new mixed borates with formula(Rb 2 Ca [B 4 O 5 (OH) 4 ] 2 ·8H 2 O and Cs 2 Ca [B 4 O 5 (OH) 4 ] 2 ·8H 2 O)were prepared by reaction Rb (Cs )-borate aqueous solution with CaCl 2 .Two kinds of compounds were characterized by chemical analysis,X-ray powder dif fraction,FT-IR spectra and thermal analysis.