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
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 important synthetic precursor（Ⅲ）, 1-（prop-2-yn-1-yl）-7,8-dihydro-1Hbenzo[d][1,3]thiazine-2,5（4H,6H）-dione（C（11）H（11）NO2S）, was prepared through a three-component reaction, which was further transferre...The important synthetic precursor（Ⅲ）, 1-（prop-2-yn-1-yl）-7,8-dihydro-1Hbenzo[d][1,3]thiazine-2,5（4H,6H）-dione（C（11）H（11）NO2S）, was prepared through a three-component reaction, which was further transferred into cytotoxic triazoles by alkylation and ＂click＂ synthesis in satisfactory yields of 87%^95%. Their structures were characterized by IR, H-RESI-MS and NMR analysis. Meanwhile, the crystal of Ⅲ was obtained and determined by X-ray single-crystal diffraction. Crystal data： orthorhombic system, space group P212121, a = 5.189（4）, b = 8.661（6）, c = 23.498（17） A, V = 1056.2（13） A^3, Z = 4, F（000） = 464, Dc = 1.392 g/cm^3, μ =0.284 mm^-1, R = 0.0637 and wR = 0.1668 for 8182 independent reflections（R（int） = 0.1580） and 2166 observed ones（I 〉 2σ（I））.展开更多
A new zinc hydrogen phosphite C4H8N2H4·Zn（HPO3）2 was prepared by hydrothermal method in the presence of piperazine as a structure-directing agent and the crystal structure was determined by single-crystal X-ray...A new zinc hydrogen phosphite C4H8N2H4·Zn（HPO3）2 was prepared by hydrothermal method in the presence of piperazine as a structure-directing agent and the crystal structure was determined by single-crystal X-ray diffraction analysis and further characterized by X-ray powder diffraction, IR, ICP, elemental analysis and TG analysis. This compound has one-dimensional anionic chains containing four-membered rings built from corner-sharing linked alternating ZnO4 tetrahedra and HPO3 pseudo pyramids. The zinc hydrogen phosphite chains are interacted with the templates of diprotonated piperazine by N—H…O hydrogen bond. Crystal data for C4H8N2H4·Zn（HPO3）2∶monoclinic, space group C2/c. a=1.774 8（2） nm, b=0.724 28（9） nm, c=0.880 87（11） nm, β= 105.345（3）°, V=1.091 9（2） nm 3, Z=4, Dc=1^907 Mg/m 3, R1=0.022 9, wR2=0.058 8.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
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
The hetero-metal clusters [■5-C5H4C（O）CH2CH2C（O）OCH3]FeCoM（■3-S）（CO）8 （M = Mo 1, M = W 2） were prepared by thermal reactions of FeCo2（CO）9(（3-S） with metal exchange reagent [■5-C5H4C（O）CH2CH2C（O）O...The hetero-metal clusters [■5-C5H4C（O）CH2CH2C（O）OCH3]FeCoM（■3-S）（CO）8 （M = Mo 1, M = W 2） were prepared by thermal reactions of FeCo2（CO）9(（3-S） with metal exchange reagent [■5-C5H4C（O）CH2CH2C（O）OCH3]M（CO）3Na （M = Mo or W） in THF. Cluster 1 reacted with 2,4-dinitrophenylhydrazine at room temperature to yield the cluster hydrazone derivative (（3-S）CoFeMo（CO）8[(5-C5H4C（NR）Me] [R = NHC6H3-2,4-（NO2）2] 3. All the compounds were characterized by elemental analyses, IR and NMR spectra. Cluster 1 was determined by single crystal X-ray diffraction. Crystal data: C18H11O11SCoFeMo, Mr = 646.05, triclinic, space group P, a = 8.148（2）, b = 10.685（3）, c = 13.410（4） ?, ( = 100.077（5）, ( = 102.452（5）, ( = 91.108（6）(, V = 1120.4（5） ?3, Z = 2, Dc = 1.915 g/cm3, F（000） = 636, ( = 2.071 mm(1, the final R = 0.0378 and wR = 0.0968 for 5074 observations with (I > 2（（I））.展开更多
The two new compounds Cs5EuCl8· 14H2O(5∶ 1 type) and Cs2EuCl5· 4H2O(2∶ 1 type) were found and synthesized from CsCl EuCl3 11% HCl H2O quaternary systems by phase equilibrium method, and were characterized ...The two new compounds Cs5EuCl8· 14H2O(5∶ 1 type) and Cs2EuCl5· 4H2O(2∶ 1 type) were found and synthesized from CsCl EuCl3 11% HCl H2O quaternary systems by phase equilibrium method, and were characterized and measured by ultra violet absorption spectrometry and fluorescence spectrum. The results show that upconversion spectrum exhibit at 590nm and 610nm exited at 790nm, and the upconversion intensity increases with the EuCl3 ratio increasing in CsCl.展开更多
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.
基金Supported by the National Natural Science Foundation of China(No.21272136)Scientific Foundation from graduate school(2015CX131)Youth Talent Development Foundation of China Three Gorges University
文摘The important synthetic precursor（Ⅲ）, 1-（prop-2-yn-1-yl）-7,8-dihydro-1Hbenzo[d][1,3]thiazine-2,5（4H,6H）-dione（C（11）H（11）NO2S）, was prepared through a three-component reaction, which was further transferred into cytotoxic triazoles by alkylation and ＂click＂ synthesis in satisfactory yields of 87%^95%. Their structures were characterized by IR, H-RESI-MS and NMR analysis. Meanwhile, the crystal of Ⅲ was obtained and determined by X-ray single-crystal diffraction. Crystal data： orthorhombic system, space group P212121, a = 5.189（4）, b = 8.661（6）, c = 23.498（17） A, V = 1056.2（13） A^3, Z = 4, F（000） = 464, Dc = 1.392 g/cm^3, μ =0.284 mm^-1, R = 0.0637 and wR = 0.1668 for 8182 independent reflections（R（int） = 0.1580） and 2166 observed ones（I 〉 2σ（I））.
文摘A new zinc hydrogen phosphite C4H8N2H4·Zn（HPO3）2 was prepared by hydrothermal method in the presence of piperazine as a structure-directing agent and the crystal structure was determined by single-crystal X-ray diffraction analysis and further characterized by X-ray powder diffraction, IR, ICP, elemental analysis and TG analysis. This compound has one-dimensional anionic chains containing four-membered rings built from corner-sharing linked alternating ZnO4 tetrahedra and HPO3 pseudo pyramids. The zinc hydrogen phosphite chains are interacted with the templates of diprotonated piperazine by N—H…O hydrogen bond. Crystal data for C4H8N2H4·Zn（HPO3）2∶monoclinic, space group C2/c. a=1.774 8（2） nm, b=0.724 28（9） nm, c=0.880 87（11） nm, β= 105.345（3）°, V=1.091 9（2） nm 3, Z=4, Dc=1^907 Mg/m 3, R1=0.022 9, wR2=0.058 8.
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.
基金the National Natural Science Foundation of China.
文摘The hetero-metal clusters [■5-C5H4C（O）CH2CH2C（O）OCH3]FeCoM（■3-S）（CO）8 （M = Mo 1, M = W 2） were prepared by thermal reactions of FeCo2（CO）9(（3-S） with metal exchange reagent [■5-C5H4C（O）CH2CH2C（O）OCH3]M（CO）3Na （M = Mo or W） in THF. Cluster 1 reacted with 2,4-dinitrophenylhydrazine at room temperature to yield the cluster hydrazone derivative (（3-S）CoFeMo（CO）8[(5-C5H4C（NR）Me] [R = NHC6H3-2,4-（NO2）2] 3. All the compounds were characterized by elemental analyses, IR and NMR spectra. Cluster 1 was determined by single crystal X-ray diffraction. Crystal data: C18H11O11SCoFeMo, Mr = 646.05, triclinic, space group P, a = 8.148（2）, b = 10.685（3）, c = 13.410（4） ?, ( = 100.077（5）, ( = 102.452（5）, ( = 91.108（6）(, V = 1120.4（5） ?3, Z = 2, Dc = 1.915 g/cm3, F（000） = 636, ( = 2.071 mm(1, the final R = 0.0378 and wR = 0.0968 for 5074 observations with (I > 2（（I））.
文摘The two new compounds Cs5EuCl8· 14H2O(5∶ 1 type) and Cs2EuCl5· 4H2O(2∶ 1 type) were found and synthesized from CsCl EuCl3 11% HCl H2O quaternary systems by phase equilibrium method, and were characterized and measured by ultra violet absorption spectrometry and fluorescence spectrum. The results show that upconversion spectrum exhibit at 590nm and 610nm exited at 790nm, and the upconversion intensity increases with the EuCl3 ratio increasing in CsCl.
