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
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
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
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 compound, \[Ni(en)\-3\]\-2\[Ni(en)\-2(H\-2O)\-2\]\[As\-6V\-\{15\}O\-\{42\}\]·4H\-2O, was first prepared by hydrothermal synthesis and characterized by elemental analysis, IR, TGA\|DSC, ESR and single crysta...A new compound, \[Ni(en)\-3\]\-2\[Ni(en)\-2(H\-2O)\-2\]\[As\-6V\-\{15\}O\-\{42\}\]·4H\-2O, was first prepared by hydrothermal synthesis and characterized by elemental analysis, IR, TGA\|DSC, ESR and single crystal X\|ray diffraction. Crystal data: monoclinic, space group \%C\-c, a\%=1\^523 6(3) nm, \%b\%=2\^051 8(4) nm, \%c\%=2\^395 9(5) nm, \%β=97\^41(3)°, V\%=7\^427(3) nm\+3, \%Z=4, R=0\^057 0, wR\-2=0\^135 7\%. The polyanion consists of six AsO\-3 pyramids and fifteen VO\-5 pyramids. Counterions are complex ions with octahedral structure, which consist of NH\-2CH\-2CH\-2NH\-2 and Ni\+\{2+\}.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
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.
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 compound, \[Ni(en)\-3\]\-2\[Ni(en)\-2(H\-2O)\-2\]\[As\-6V\-\{15\}O\-\{42\}\]·4H\-2O, was first prepared by hydrothermal synthesis and characterized by elemental analysis, IR, TGA\|DSC, ESR and single crystal X\|ray diffraction. Crystal data: monoclinic, space group \%C\-c, a\%=1\^523 6(3) nm, \%b\%=2\^051 8(4) nm, \%c\%=2\^395 9(5) nm, \%β=97\^41(3)°, V\%=7\^427(3) nm\+3, \%Z=4, R=0\^057 0, wR\-2=0\^135 7\%. The polyanion consists of six AsO\-3 pyramids and fifteen VO\-5 pyramids. Counterions are complex ions with octahedral structure, which consist of NH\-2CH\-2CH\-2NH\-2 and Ni\+\{2+\}.
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.
