The novel Schiff base(E)-8-chloro-NA-(4-(dimethylamino)benzylidene)-[1,2,4]triazolo[4,3-a]pyridine-3-carbohydrazide was synthesized and characterized by ^1H NMR,MS,elemental analysis and X-ray diffraction.The co...The novel Schiff base(E)-8-chloro-NA-(4-(dimethylamino)benzylidene)-[1,2,4]triazolo[4,3-a]pyridine-3-carbohydrazide was synthesized and characterized by ^1H NMR,MS,elemental analysis and X-ray diffraction.The compound crystallizes in the monoclinic space group P2_1/c with a = 7.091(2),b = 10.750(3),c = 21.380(6) A,β = 96.299(6)°,V = 1619.7(8) A^3,Z = 4 and R = 0.0351.Theoretical calculation of the title compound was carried out with the B3LYP/6-31 G basis set.The frontier orbital energy and atomic net charges were discussed.It is found that the experimental data show good agreement with the calculated values.And the compound exhibits good antifungal activity against Stemphylium lycopersici(Enjoji) Yamamoto.展开更多
A new Zn(Ⅱ) coordination polymer, [Zn(4-PP)(1,4-BDC)?(H_2O)]_n(1, 4-PP = 4-(1 H-pyrazol-3-yl)pyridine, 1,4-H_2BDC = 1,4-benzenedicarboxylic acid), has been synthesized and structurally characterized by single-crystal...A new Zn(Ⅱ) coordination polymer, [Zn(4-PP)(1,4-BDC)?(H_2O)]_n(1, 4-PP = 4-(1 H-pyrazol-3-yl)pyridine, 1,4-H_2BDC = 1,4-benzenedicarboxylic acid), has been synthesized and structurally characterized by single-crystal X-ray diffraction as well as elemental analysis, IR spectra, XRPD and TG. Structural analysis reveals that Zn(Ⅱ) ions are bridged by COO-from 1,4-BDC^(2-)to form a binuclear structure as the second building units(SBUs). Zn_2 clusters can be clarified as 4-connected nodes, so the framework of 1 can be considered as a 2 D(44?62)-sql sheet. Fluorescence measurements show that 1 has highly selective and sensitive detection of Fe^(3+) in water medium.展开更多
The title compound 8-chloro-3-((4-chlorobenzyl)thio)-[1,2,4]triazolo[4,3-a]pyridine was prepared from 1-chloro-4-(chloromethyl)benzene and 8-chloro-[1,2,4]triazolo[4,3-a]pyridine-3(2H)-thione in the presence o...The title compound 8-chloro-3-((4-chlorobenzyl)thio)-[1,2,4]triazolo[4,3-a]pyridine was prepared from 1-chloro-4-(chloromethyl)benzene and 8-chloro-[1,2,4]triazolo[4,3-a]pyridine-3(2H)-thione in the presence of Na OH, and its structure was determined by X-ray diffraction analysis. The crystal is of triclinic system, space group P1 with a = 6.8264(6), b = 7.5890(4), c = 13.0960(7) A, α = 93.447(4), β = 98.772(6), γ = 92.615(6)o, V = 668.26(8) A3, Z = 2, the final R = 0.035 and wR = 0.09 for 2259 observed reflections with I 〉 2σ(I). The preliminary biological test showed that the title compound has activities against Stemphylium lycopersici(Enjoji) Yamamoto, Fusarium oxysporum. sp. cucumebrium, and Botrytis cinerea with inhibitory to be 51.19%, 62.02% and 15.56%, respectively.展开更多
The reaction of CoCl2·6H2O with 2,6-bis(N,N'-bis(2,6-diisopropyl-4-(2,3-dimethy-oxyl-benzoylamide)phenylimino))pyridine(L) afforded the complex [CoCl2L],which was fully characterized by elemental analysi...The reaction of CoCl2·6H2O with 2,6-bis(N,N'-bis(2,6-diisopropyl-4-(2,3-dimethy-oxyl-benzoylamide)phenylimino))pyridine(L) afforded the complex [CoCl2L],which was fully characterized by elemental analysis,UV-vis,IR spectroscopy,fluorescence,and X-ray diffraction analysis.The compound is of triclinic system,space group P1 with a = 13.058(3),b = 13.798(3),c = 16.695(3) ,α = 98.191(3),β = 102.792(3),γ = 101.820(3)°,V = 2815.0(9) 3,Z = 2,F(000) = 1122,μ = 0.45 mm-1,R = 0.061 and wR = 0.1349 for 9842 observed reflections(Ⅰ 〉 2σ(Ⅰ)).The Co(Ⅱ) center adopts a distorted square-pyramidal coordination geometry.The extended structure shows a one-dimensional zigzag double chain linked by hydrogen bonds and π-π stacking interactions.展开更多
The crystal structure of [Ni(TAAB)(py)_2](BF_4)_2,where TAAB is the tetradentate macrocyclic ligand tetrabenzo[b,f,j,n] [1,5,9,13] tetraazacyclohexadecine,has been determined from X-ray diffraction analysis.The crys. ...The crystal structure of [Ni(TAAB)(py)_2](BF_4)_2,where TAAB is the tetradentate macrocyclic ligand tetrabenzo[b,f,j,n] [1,5,9,13] tetraazacyclohexadecine,has been determined from X-ray diffraction analysis.The crys. tai beiongs to monoclinic,space group P2_1/n with cell parameters a=16.465(6),b =12.486(5),e=20.219(1),β=113.79°, V=3803.9~3,Z=4,De=1.402 g/cm^3,F(000)=1640,The molecule has approximately S_4 symmetry.TAAB macrocyelic ligand presents a decidedly saddle-shaped appearance.Planes pyridine molecules are perpendicular to each other and the nickle(II)ion has coordination geometry.The final R and Rw are 0.068 and 0.070,respectively.展开更多
Unconsolidated sandstone reservoirs are most susceptible to sand production that leads to a dramatic oil production decline.In this study,the poly(4-vinyl pyridine)(P_(4)VP)incorporated with self-aggregating behavior ...Unconsolidated sandstone reservoirs are most susceptible to sand production that leads to a dramatic oil production decline.In this study,the poly(4-vinyl pyridine)(P_(4)VP)incorporated with self-aggregating behavior was proposed for sand migration control.The P_(4)VP could aggregate sand grains spontaneously throughπ-πstacking interactions to withstand the drag forces sufficiently.The influential factors on the self-aggregating behavior of the P_(4)VP were evaluated by adhesion force test.The adsorption as well as desorption behavior of P_(4)VP on sand grains was characterized by scanning electron microscopy and adhesion force test at different pH conditions.The result indicated that the pH altered the forms of surface silanol groups on sand grains,which in turn affected the adsorption process of P_(4)VP.The spontaneous dimerization of P_(4)VP molecules resulting from theπ-πstacking interaction was demonstrated by reduced density gradient analysis,which contributed to the self-aggregating behavior and the thermally reversible characteristic of the P_(4)VP.Dynamic sand stabilization test revealed that the P_(4)VP showed wide pH and temperature ranges of application.The production of sands can be mitigated effectively at 20-130℃ within the pH range of 4-8.展开更多
A new hydrogen bonded Cobalt(II) Schiff base complex,?N’-(pyridine-4-carboxaldehyde) isonicotinoylhydrazone Cobalt(II), has been synthesized from isoniazid and pyridine-4-carboxaldehyde and characterized by IR spectr...A new hydrogen bonded Cobalt(II) Schiff base complex,?N’-(pyridine-4-carboxaldehyde) isonicotinoylhydrazone Cobalt(II), has been synthesized from isoniazid and pyridine-4-carboxaldehyde and characterized by IR spectroscopy, 1H-NMR, elemental analysis, TGA and single crystal X-ray structure determination. X-ray crystal structure analysis shows an octahedral complex with a metal centre coordinated to two ligand molecules through the pyridine nitrogen atoms and four water molecules and containing two nitrate groups as counter ions. The complex crystallizes in the monoclinic crystal system and P2(1)/n space group. The unit cell dimensions are: a = 7.2108(4) Å, b = 16.6020(9) Å, c = 13.0389(6) Å,α = 90°, β = 103.972(4)°, γ = 90°. The molecule is symmetrical about the cobalt centre as observed from the 1H-NMR and 13C-NMR and confirmed by the single crystal X-ray structure of the complex. Thermogravimetric analysis shows two steps decomposition of the complex to leave a metal oxide residue. The title compound is expected to be biologically active as one of the precursors (isoniazid) is a therapeutic agent with well-established clinical applications.展开更多
Several new pyrazolo[4,3-b] pyridines 7a, b were prepared by reacting arylidenemalononitriles 1a, c or 1i, j with 4-nitrosoantipyrine 4. Reacting 1a, b, d with 4-azidomethylcarbonylantipyrine 8 give 2-aminopyrrole 14....Several new pyrazolo[4,3-b] pyridines 7a, b were prepared by reacting arylidenemalononitriles 1a, c or 1i, j with 4-nitrosoantipyrine 4. Reacting 1a, b, d with 4-azidomethylcarbonylantipyrine 8 give 2-aminopyrrole 14. Pyrano[3,2-c] quinolines 20a, b and 23 were obtained by reacting 4-hydroxyquinoline 15 with 1g, h, 2b respectively. Reaction of 1 with naphthalenediols 24, 27 and 29 yield naphthodipyrans 26a, b, 28a, b and 30a。展开更多
The Schiff base pyridine-2-carboxaldehyde-4-aminoantipyrine (CI7H16N4O 1) and its perchlorate (C17H17N4O·ClO4 2) have been prepared and characterized by elemental analysis, IR spectra and single-crystal X-ray...The Schiff base pyridine-2-carboxaldehyde-4-aminoantipyrine (CI7H16N4O 1) and its perchlorate (C17H17N4O·ClO4 2) have been prepared and characterized by elemental analysis, IR spectra and single-crystal X-ray crystallography analysis. Both 1 and 2 crystallize in the monoclinic system, space group P21/c. For 1, a = 8.6820(12), b = 24.934(3), c = 7.0064(10) A,, β= 97.942(3)°, V = 1502.2(4) A^3, Z = 4, Dc = 1.293 g/cm^3, F(000) = 616,μ = 0.084 mm^-1, the final R = 0.0592 and wR = 0.1244. For 2, a = 5.9302(2), b = 20.347(7), c = 14.663(6) A, β= 90.200(9)°, V= 1769.201) A^3, Z = 4, Dc = 1.475 g/cm^3, F(000) = 816, μ = 0.254 mm^-1, the final R = 0.0533 and wR = 0.0819. As expected, both molecular structures of 1 and 2 adopt a trans configuration about the central C=N double bond. 2 is an ionic compound with the protonation at N(1) of pyridine-2-carboxaldehyde-4- aminoantipyrine.展开更多
Reaction of FeCIz'6H20, pyridine-2,4,6-tricarboxylic acid(H3pyta) and NaOH in the hydrothermal system at 185 ℃ resulted in the formation of 1D coordination polymer[Fe(Hpyta)(H2O)2](1) based on Fe-Hpyta chain...Reaction of FeCIz'6H20, pyridine-2,4,6-tricarboxylic acid(H3pyta) and NaOH in the hydrothermal system at 185 ℃ resulted in the formation of 1D coordination polymer[Fe(Hpyta)(H2O)2](1) based on Fe-Hpyta chains. When the abpt[abpt=-4-amino-3,5-bis(4-pyridyl)-l,2,4-triazole] ligand was employed in the reaction system, a 3D supramolecular porous network (H2bpt)[Fe(pyta)(H2O)2]·4H2O(2) was obtained. The framework was constructed with negative (Fe-pyta) chains and the positive H3bpt^+ in situ, formed from the abpt reagent, to form 1D channels filled with guest water molecules via hydrogen-bonds. X-Ray diffraction crystal structure analysis shows that complex 1 crystallized in the monoclinic system, space group C2/c, a=1.1490(5) nm, b=0.9008(4) nm, c=1.0058(5) nm, B=107.254(9)°, V=0.9942(8) nm3, Z=4; and complex 2 crystallizes in the triclinic system, space group P1 with a=0.90392(11) nm, b=0.96027(11 ) nm, c=1.55540(18) nm, a=73.558(2)°,B= 86.126(2)°,r= 68.745(2)°, V=1.2059(2) nm^3 and Z=2.展开更多
A novel compound, {[Y(HPIDC)(OX)1/2(H2O)]·2H2O}n (1, H3PIDC = 2-(pyridin-4- yl)-1H-imidazole-4,5-dicarboxylic acid, H2OX = oxalic acid), has been synthesized under hydrothermal conditions and characteri...A novel compound, {[Y(HPIDC)(OX)1/2(H2O)]·2H2O}n (1, H3PIDC = 2-(pyridin-4- yl)-1H-imidazole-4,5-dicarboxylic acid, H2OX = oxalic acid), has been synthesized under hydrothermal conditions and characterized by thermal analysis (TGA), powder X-ray diffraction (PXRD), and single-crystal X-ray diffraction. Complex 1 crystallizes in monoclinic space group P21/c with a = 8.342(8), b = 14.61(1), c = 11.487(1), β = 90.78(9)°, V = 1400.4(2)3, Z = 4, C11H11N3O9Y, Mr = 418.14, Dc = 1.983 g/cm3, F(000) = 836, Rint = 0.0509, T = 293(2) K, μ = 4.240 mm-1, the final R = 0.0477 and wR = 0.1125 for 2770 observed reflections with I 2σ(I). Compound 1 exhibits a 3D framework and generates the 1D open channels filled with free water molecules. The structure of 1 can be rationalized as a diamondoid network when the atom yttrium is regarded as a 4-connected node linking four surrounding yttrium atoms. The luminescent property of compound 1 is also investigated.展开更多
[Objective]The paper was to synthesize a new structure of metal organic framework,and to provide new materials for plant pathogens testing.[Method]A mixture of 2,6-di(2’,4’-di-carboxylphenyl)pyridine,1,4-bis(1-imida...[Objective]The paper was to synthesize a new structure of metal organic framework,and to provide new materials for plant pathogens testing.[Method]A mixture of 2,6-di(2’,4’-di-carboxylphenyl)pyridine,1,4-bis(1-imidazolyl)benzene,Co(NO_(3))2·6H_(2)O were added to the solution of DMF:H2O=3:3 and heated at 433K for 4 d.[Result]Red crystals of the title compound were obtained(yield 76.3%,based on Co).[Conclusion]The crystal data were obtained as follows:C_(39)H_(24)Co_(2)N_(7)O_(8),monoclinic,P21/c,a=16.222(7)A,b=12.653(5)A,c=17.456(7)A,β=102.386(6)°,V=3500(2)A_(3),Z=4,Rgt(F)=0.0550,wRref(F2)=0.1509,T=293(2)K.展开更多
A 2D plane coordination compound [Ag_2(Dpya)_2.(NO_3)_2]n was synthesized and characterized by FT-IR,elemental analysis and TG analysis.The red crystal was obtained via solvent diffusion method at room temperature...A 2D plane coordination compound [Ag_2(Dpya)_2.(NO_3)_2]n was synthesized and characterized by FT-IR,elemental analysis and TG analysis.The red crystal was obtained via solvent diffusion method at room temperature and is slightly soluble in organic solvents.Its structure was determined by single-crystal X-ray diffraction analysis.It crystallizes in monoclinic,space group P1 with a = 10.7995(13),b = 7.4748(8),c = 18.364(2) A,β = 98.916(4)o,V = 1464.5(3) A^3,Z = 2,C_(26)H_(28)Ag_2N_(10)O_6,M_r = 792.32,Dc = 1.302 Mg/m^3,F(000) = 792,μ(Mo Ka) = 1.356 mm^-1,R = 0.0575 and w R = 0.0826.The compound [Ag_2(Dpya)_2.(NO_3)_2]_n is a two-dimensional structure and there are two kinds of coordination configurations about the Ag atoms in the compound.The Ag(1) center is tetrahedrally coordinated with two O atoms of NO_3^-and two N atoms from the ligand Dpya.Meanwhile,the Ag(2) is five-coordinated by five O atoms from three NO_3^-anions.The Ag centers(Ag(1) and Ag(2)) connect to themselves as well as with each other by the bridging NO_3^-anions.And the coordination compound shows photoluminescence with an emission peak at 530 nm(λex = 450 nm) as the ligand Dpya.展开更多
Reaction of 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-thioxo-1,2-dihydropyridine-3-carbonitrile) (1) with methyl iodide afforded the 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-(methylthio)nicotinonitrile) (2). Th...Reaction of 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-thioxo-1,2-dihydropyridine-3-carbonitrile) (1) with methyl iodide afforded the 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-(methylthio)nicotinonitrile) (2). The reaction of 2 with hydrazine hydrate followed by diazotization reaction af-forded the 1,1’-(1,4-phenylenebis(3-amino-6-methyl-1H-pyrazolo[3,4-b]pyridine-4,5-diyl))bis(e-than-1-one) (3) and 1,1’-(1,4-phenylenebis(3-(chlorodiazenyl)-6-methyl-1H-pyrazolo[3,4-b]-pyridine-4,5-diyl))bis(ethan-1-one) (4) respectively. On the other hand, reaction of 4 with malononitrile, 2-cyanoethanethioamide, ethyl acetoacetate, acetyl acetone, ethyl benzoylacetate, diethylmalonate, ethyl cyanoacetate and phenacylbromide aiming to build up pyrazolotriazine or pyrazole ring on the ring system of 4. Structures of all newly synthesized heterocyclic compounds in the present study were confirmed by considering the data of IR, 1H NMR, mass spectra as well as that of elemental analyses.展开更多
基金funded by National Natural Science Foundation of China(No.21002090)Zhejiang Provincial Natural Science Foundation of China(No.LY16C140007)the National Key Technologies R&D Program(2011BAE06B03-01)
文摘The novel Schiff base(E)-8-chloro-NA-(4-(dimethylamino)benzylidene)-[1,2,4]triazolo[4,3-a]pyridine-3-carbohydrazide was synthesized and characterized by ^1H NMR,MS,elemental analysis and X-ray diffraction.The compound crystallizes in the monoclinic space group P2_1/c with a = 7.091(2),b = 10.750(3),c = 21.380(6) A,β = 96.299(6)°,V = 1619.7(8) A^3,Z = 4 and R = 0.0351.Theoretical calculation of the title compound was carried out with the B3LYP/6-31 G basis set.The frontier orbital energy and atomic net charges were discussed.It is found that the experimental data show good agreement with the calculated values.And the compound exhibits good antifungal activity against Stemphylium lycopersici(Enjoji) Yamamoto.
基金supported by the Science and Technology Program of Hengshui City(No.2018011001Z)
文摘A new Zn(Ⅱ) coordination polymer, [Zn(4-PP)(1,4-BDC)?(H_2O)]_n(1, 4-PP = 4-(1 H-pyrazol-3-yl)pyridine, 1,4-H_2BDC = 1,4-benzenedicarboxylic acid), has been synthesized and structurally characterized by single-crystal X-ray diffraction as well as elemental analysis, IR spectra, XRPD and TG. Structural analysis reveals that Zn(Ⅱ) ions are bridged by COO-from 1,4-BDC^(2-)to form a binuclear structure as the second building units(SBUs). Zn_2 clusters can be clarified as 4-connected nodes, so the framework of 1 can be considered as a 2 D(44?62)-sql sheet. Fluorescence measurements show that 1 has highly selective and sensitive detection of Fe^(3+) in water medium.
基金funded by the National Natural Science Foundation of China(No.21002090)the Natural Science Foundation of Zhejiang Province(No.LY16C140007)the public program of Science and Technology of Zhejiang Province(2014C31127,2013C32SA700134)
文摘The title compound 8-chloro-3-((4-chlorobenzyl)thio)-[1,2,4]triazolo[4,3-a]pyridine was prepared from 1-chloro-4-(chloromethyl)benzene and 8-chloro-[1,2,4]triazolo[4,3-a]pyridine-3(2H)-thione in the presence of Na OH, and its structure was determined by X-ray diffraction analysis. The crystal is of triclinic system, space group P1 with a = 6.8264(6), b = 7.5890(4), c = 13.0960(7) A, α = 93.447(4), β = 98.772(6), γ = 92.615(6)o, V = 668.26(8) A3, Z = 2, the final R = 0.035 and wR = 0.09 for 2259 observed reflections with I 〉 2σ(I). The preliminary biological test showed that the title compound has activities against Stemphylium lycopersici(Enjoji) Yamamoto, Fusarium oxysporum. sp. cucumebrium, and Botrytis cinerea with inhibitory to be 51.19%, 62.02% and 15.56%, respectively.
文摘The crystal structure of [Ni(TAAB)(py)_2](BF_4)_2,where TAAB is the tetradentate macrocyclic ligand tetrabenzo[b,f,j,n] [1,5,9,13] tetraazacyclohexadecine,has been determined from X-ray diffraction analysis.The crys. tai beiongs to monoclinic,space group P2_1/n with cell parameters a=16.465(6),b =12.486(5),e=20.219(1),β=113.79°, V=3803.9~3,Z=4,De=1.402 g/cm^3,F(000)=1640,The molecule has approximately S_4 symmetry.TAAB macrocyelic ligand presents a decidedly saddle-shaped appearance.Planes pyridine molecules are perpendicular to each other and the nickle(II)ion has coordination geometry.The final R and Rw are 0.068 and 0.070,respectively.
基金support from the National Key R&D Program of China(grant number 2018YFA0702400)the Major Scientific and Technological Projects of CNPC(grant number ZD2019-183-007)the China Postdoctoral Science Foundation(grant number 2021M702041)。
文摘Unconsolidated sandstone reservoirs are most susceptible to sand production that leads to a dramatic oil production decline.In this study,the poly(4-vinyl pyridine)(P_(4)VP)incorporated with self-aggregating behavior was proposed for sand migration control.The P_(4)VP could aggregate sand grains spontaneously throughπ-πstacking interactions to withstand the drag forces sufficiently.The influential factors on the self-aggregating behavior of the P_(4)VP were evaluated by adhesion force test.The adsorption as well as desorption behavior of P_(4)VP on sand grains was characterized by scanning electron microscopy and adhesion force test at different pH conditions.The result indicated that the pH altered the forms of surface silanol groups on sand grains,which in turn affected the adsorption process of P_(4)VP.The spontaneous dimerization of P_(4)VP molecules resulting from theπ-πstacking interaction was demonstrated by reduced density gradient analysis,which contributed to the self-aggregating behavior and the thermally reversible characteristic of the P_(4)VP.Dynamic sand stabilization test revealed that the P_(4)VP showed wide pH and temperature ranges of application.The production of sands can be mitigated effectively at 20-130℃ within the pH range of 4-8.
文摘A new hydrogen bonded Cobalt(II) Schiff base complex,?N’-(pyridine-4-carboxaldehyde) isonicotinoylhydrazone Cobalt(II), has been synthesized from isoniazid and pyridine-4-carboxaldehyde and characterized by IR spectroscopy, 1H-NMR, elemental analysis, TGA and single crystal X-ray structure determination. X-ray crystal structure analysis shows an octahedral complex with a metal centre coordinated to two ligand molecules through the pyridine nitrogen atoms and four water molecules and containing two nitrate groups as counter ions. The complex crystallizes in the monoclinic crystal system and P2(1)/n space group. The unit cell dimensions are: a = 7.2108(4) Å, b = 16.6020(9) Å, c = 13.0389(6) Å,α = 90°, β = 103.972(4)°, γ = 90°. The molecule is symmetrical about the cobalt centre as observed from the 1H-NMR and 13C-NMR and confirmed by the single crystal X-ray structure of the complex. Thermogravimetric analysis shows two steps decomposition of the complex to leave a metal oxide residue. The title compound is expected to be biologically active as one of the precursors (isoniazid) is a therapeutic agent with well-established clinical applications.
文摘Several new pyrazolo[4,3-b] pyridines 7a, b were prepared by reacting arylidenemalononitriles 1a, c or 1i, j with 4-nitrosoantipyrine 4. Reacting 1a, b, d with 4-azidomethylcarbonylantipyrine 8 give 2-aminopyrrole 14. Pyrano[3,2-c] quinolines 20a, b and 23 were obtained by reacting 4-hydroxyquinoline 15 with 1g, h, 2b respectively. Reaction of 1 with naphthalenediols 24, 27 and 29 yield naphthodipyrans 26a, b, 28a, b and 30a。
基金supported by the NSF of Guangxi Province (No. 0575046, 0575049)the Program for New Century Ten-Hundred-Thousand Excellent Talents of Guangxi (No. 2003223)+1 种基金the National Natural Science Foundation of China (No. 20361002, 30460153) as well as TRAPOYTNCET-04-0836 of Chinese Ministry of Education
文摘The Schiff base pyridine-2-carboxaldehyde-4-aminoantipyrine (CI7H16N4O 1) and its perchlorate (C17H17N4O·ClO4 2) have been prepared and characterized by elemental analysis, IR spectra and single-crystal X-ray crystallography analysis. Both 1 and 2 crystallize in the monoclinic system, space group P21/c. For 1, a = 8.6820(12), b = 24.934(3), c = 7.0064(10) A,, β= 97.942(3)°, V = 1502.2(4) A^3, Z = 4, Dc = 1.293 g/cm^3, F(000) = 616,μ = 0.084 mm^-1, the final R = 0.0592 and wR = 0.1244. For 2, a = 5.9302(2), b = 20.347(7), c = 14.663(6) A, β= 90.200(9)°, V= 1769.201) A^3, Z = 4, Dc = 1.475 g/cm^3, F(000) = 816, μ = 0.254 mm^-1, the final R = 0.0533 and wR = 0.0819. As expected, both molecular structures of 1 and 2 adopt a trans configuration about the central C=N double bond. 2 is an ionic compound with the protonation at N(1) of pyridine-2-carboxaldehyde-4- aminoantipyrine.
基金the Scientific and Technological Project of Guangdong Province, China(No.2006B36703005)
文摘Reaction of FeCIz'6H20, pyridine-2,4,6-tricarboxylic acid(H3pyta) and NaOH in the hydrothermal system at 185 ℃ resulted in the formation of 1D coordination polymer[Fe(Hpyta)(H2O)2](1) based on Fe-Hpyta chains. When the abpt[abpt=-4-amino-3,5-bis(4-pyridyl)-l,2,4-triazole] ligand was employed in the reaction system, a 3D supramolecular porous network (H2bpt)[Fe(pyta)(H2O)2]·4H2O(2) was obtained. The framework was constructed with negative (Fe-pyta) chains and the positive H3bpt^+ in situ, formed from the abpt reagent, to form 1D channels filled with guest water molecules via hydrogen-bonds. X-Ray diffraction crystal structure analysis shows that complex 1 crystallized in the monoclinic system, space group C2/c, a=1.1490(5) nm, b=0.9008(4) nm, c=1.0058(5) nm, B=107.254(9)°, V=0.9942(8) nm3, Z=4; and complex 2 crystallizes in the triclinic system, space group P1 with a=0.90392(11) nm, b=0.96027(11 ) nm, c=1.55540(18) nm, a=73.558(2)°,B= 86.126(2)°,r= 68.745(2)°, V=1.2059(2) nm^3 and Z=2.
基金supported by the 973 key program of the MOST(2010CB933501,2012CB821705)the Chinese Academy of Sciences(KJCX2-YW-319,KJCX2-EW-H01)+1 种基金the National Natural Science Foundation of China(20873150,20821061,20973173,50772113 and 91022008)the Natural Science Foundation of Fujian Province(2007HZ0001-1,2009HZ0004-1,2009HZ0005-1,2009HZ0006-1,2006L2005)
文摘A novel compound, {[Y(HPIDC)(OX)1/2(H2O)]·2H2O}n (1, H3PIDC = 2-(pyridin-4- yl)-1H-imidazole-4,5-dicarboxylic acid, H2OX = oxalic acid), has been synthesized under hydrothermal conditions and characterized by thermal analysis (TGA), powder X-ray diffraction (PXRD), and single-crystal X-ray diffraction. Complex 1 crystallizes in monoclinic space group P21/c with a = 8.342(8), b = 14.61(1), c = 11.487(1), β = 90.78(9)°, V = 1400.4(2)3, Z = 4, C11H11N3O9Y, Mr = 418.14, Dc = 1.983 g/cm3, F(000) = 836, Rint = 0.0509, T = 293(2) K, μ = 4.240 mm-1, the final R = 0.0477 and wR = 0.1125 for 2770 observed reflections with I 2σ(I). Compound 1 exhibits a 3D framework and generates the 1D open channels filled with free water molecules. The structure of 1 can be rationalized as a diamondoid network when the atom yttrium is regarded as a 4-connected node linking four surrounding yttrium atoms. The luminescent property of compound 1 is also investigated.
基金Hainan Major Research Found of Science and Technology(ZDKJ201817).
文摘[Objective]The paper was to synthesize a new structure of metal organic framework,and to provide new materials for plant pathogens testing.[Method]A mixture of 2,6-di(2’,4’-di-carboxylphenyl)pyridine,1,4-bis(1-imidazolyl)benzene,Co(NO_(3))2·6H_(2)O were added to the solution of DMF:H2O=3:3 and heated at 433K for 4 d.[Result]Red crystals of the title compound were obtained(yield 76.3%,based on Co).[Conclusion]The crystal data were obtained as follows:C_(39)H_(24)Co_(2)N_(7)O_(8),monoclinic,P21/c,a=16.222(7)A,b=12.653(5)A,c=17.456(7)A,β=102.386(6)°,V=3500(2)A_(3),Z=4,Rgt(F)=0.0550,wRref(F2)=0.1509,T=293(2)K.
基金the sponsorship and financial support from the Key Laboratory of Organic Synthesis of Jiangsu Province
文摘A 2D plane coordination compound [Ag_2(Dpya)_2.(NO_3)_2]n was synthesized and characterized by FT-IR,elemental analysis and TG analysis.The red crystal was obtained via solvent diffusion method at room temperature and is slightly soluble in organic solvents.Its structure was determined by single-crystal X-ray diffraction analysis.It crystallizes in monoclinic,space group P1 with a = 10.7995(13),b = 7.4748(8),c = 18.364(2) A,β = 98.916(4)o,V = 1464.5(3) A^3,Z = 2,C_(26)H_(28)Ag_2N_(10)O_6,M_r = 792.32,Dc = 1.302 Mg/m^3,F(000) = 792,μ(Mo Ka) = 1.356 mm^-1,R = 0.0575 and w R = 0.0826.The compound [Ag_2(Dpya)_2.(NO_3)_2]_n is a two-dimensional structure and there are two kinds of coordination configurations about the Ag atoms in the compound.The Ag(1) center is tetrahedrally coordinated with two O atoms of NO_3^-and two N atoms from the ligand Dpya.Meanwhile,the Ag(2) is five-coordinated by five O atoms from three NO_3^-anions.The Ag centers(Ag(1) and Ag(2)) connect to themselves as well as with each other by the bridging NO_3^-anions.And the coordination compound shows photoluminescence with an emission peak at 530 nm(λex = 450 nm) as the ligand Dpya.
文摘Reaction of 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-thioxo-1,2-dihydropyridine-3-carbonitrile) (1) with methyl iodide afforded the 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-(methylthio)nicotinonitrile) (2). The reaction of 2 with hydrazine hydrate followed by diazotization reaction af-forded the 1,1’-(1,4-phenylenebis(3-amino-6-methyl-1H-pyrazolo[3,4-b]pyridine-4,5-diyl))bis(e-than-1-one) (3) and 1,1’-(1,4-phenylenebis(3-(chlorodiazenyl)-6-methyl-1H-pyrazolo[3,4-b]-pyridine-4,5-diyl))bis(ethan-1-one) (4) respectively. On the other hand, reaction of 4 with malononitrile, 2-cyanoethanethioamide, ethyl acetoacetate, acetyl acetone, ethyl benzoylacetate, diethylmalonate, ethyl cyanoacetate and phenacylbromide aiming to build up pyrazolotriazine or pyrazole ring on the ring system of 4. Structures of all newly synthesized heterocyclic compounds in the present study were confirmed by considering the data of IR, 1H NMR, mass spectra as well as that of elemental analyses.