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1.
A novel hybrid compound [Co(4,4'-bipy)2(H2O)4](4,4'- H2bipy)2[H2W12O40]·5.5H2Ohas been synthesized from an acidified aqueous solution and characterized by elemental and thermal analyses, IR and UV spectroscopy, and single-crystal X-ray structure determination. Structure analysis indicates that the title compound is of monoclinic, space group C2/c, with a = 21.315(9), b = 15.303 (7), c = 24.139(10) (A), β = 105.170(5)o, V = 7599(6) (A)3, Mr = 3706.99, Z = 4, F(000) = 6616, Dc = 3.231, μ = 18.395 mm-1, R = 0.0652 and wR = 0.1594. X-ray crystallographic study shows that the title compound consists of one [Co(4,4'-bipy)2(H2O)4]2 cation, two diprotonated 4,4'-bipyridine molecules, 5.5 water molecules of crystallization, and one metatungstate polyoxoanion [H2W12O40]6-, which approaches an effective Td point symmetry. TG-DTA analysis indicates that the framework of the metatungstate polyoxoanion is collapsed at 587.0 ℃.  相似文献   

2.
A novel hybrid compound [Co(4,4'-bipy)2(H2O)4](4,4'-H2bipy)2[H2W12O40]·5.5H2O has been synthesized from an acidified aqueous solution and characterized by elemental and thermal analyses,IR and UV spectroscopy,and single-crystal X-ray structure determination. Structure analysis indicates that the title compound is of monoclinic,space group C2/c,with a=21.315(9),b=15.303 (7),c=24.139(10),β=105.170(5)o,V=7599(6)3,Mr=3706.99,Z=4,F(000)=6616,Dc=3.231,μ=18.395 mm-1,R=0.0652 and wR=0.1594. X-ray crystallographic study shows that the title compound consists of one [Co(4,4'-bipy)2(H2O)4]2+ cation,two diprotonated 4,4'-bipyridine molecules,5.5 water molecules of crystallization,and one metatungstate polyoxoanion [H2W12O40]6-,which approaches an effective Td point symmetry. TG-DTA analysis indicates that the framework of the metatungstate polyoxoanion is collapsed at 587.0 ℃.  相似文献   

3.
以α-H5BW12O40·nH2O,Ce(NO3)3·6H2O和DMF为原料合成了组成为[Ce(DMF)4(H2O)][α-BW12O40]·H2O·(HDMA)2(HDMA:质子化的二甲胺;DMF:N,N-二甲基甲酰胺)的二维网状化合物,并对其进行了IR,UV光谱表征及TG-DTA研究.X射线单晶衍射结果表明,晶体属于单斜晶系,P21/n空间群,晶胞参数:a=1.1983(3),b=2.4216(5),c=1.9517(4)nm,β=92.91(3)°,Z=4,R1=0.07710,wR2=0.1416.结构测定结果表明,每一个[α-BW12O40]5?多阴离子通过端氧与三个[Ce(DMF)4(H2O)]3 单元相连;而每一个[Ce(DMF)4(H2O)]3 单元又通过Ce-Od-W桥与三个[α-BW12O40]5?多阴离子相连,以这种方式连接形成了二维网状结构.热分析结果表明,标题化合物失重分两步进行,阴离子骨架分解温度大约在560℃.电化学研究表明,pH=4~7时化合物存在三步氧化还原过程.  相似文献   

4.
The title compound, [Cu2(DMPz)2PMo12O40]·HDMPz (1, DMPz = 2,5-dimethyl pyrazine), has been synthesized and characterized by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1 with a = 11.075(2), b = 11.551(2), c = 11.886(2) A, α = 106.352(2), β = 109.862(3), γ = 109.504(1)°, V = 1206.8(3) A3, C18H26Cu2Mo12N6O40P, Mr = 2275.78, Z = 1, Dc = 3.131 g/cm3,μ = 4.011 mm-1, F(000) = 1073, S = 1.066, the final R = 0.0389 and wR = 0.1056 for 3739 observed reflections with I > 2σ(I). The structural analysis indicates that the title compound is composed of Keggin clusters [PMo12O40]3- connected by one-dimensional [Cu(DMPz)]2n2n+ chains to form a two-dimensional grid layer with holes occupied by mono-protonated DMPz molecules. In the solid of the title compound, the 2D grid layers are stacked together in an ABAB packing mode.  相似文献   

5.
A novel polyoxometalate-based organic-inorganic polymer [{Ca(DMF)5}2SiMo12O40]n has been synthesized and characterized by elemental analysis, IR, UV and X-ray single-crystal structural analysis. The title compound crystallizes in a monocline lattice, P21/n, with a =1.3379(3), b = 1.9796(4), c = 1.4574(3) nm, β = 92.24(3)°, V = 3.8568(13) nm3, Z = 2, R1 = 0.083 and Rw = 0.2065. The result of crystal structure analysis indicates that Ca2+ is surrounded by seven coordination oxygen atoms with pentagonal bipyramidal geometry and bridged with terminal oxygen atom of polyanion in the structure. The compound contains an unprecedented one-dimensional linear chain built by alternate polyanions and cationic units through Mo-Od-Ca-O-Ca links in crystal. The IR spectra and X-ray crystallography analysis exhibit that there is a strong interaction between the polyanion and organic group in solid state. The electronic spectra (λ = 200-500 nm) for the title compound dissolved in the mixed solvent of acetonitrile and  相似文献   

6.
A two-dimensional coordination polymer [Co(H_2tba)_2(DMF)_2]_n 1(H_2tba = 2-thiobarbituric acid anion, DMF = N,N-dimethylformamide) has been synthesized by Co Cl2·6H2O with the 2-thiobarbituric acid ligands under solvothermal conditions. Compound 1 was further characterized by FTIR, elemental analysis, TGA and powder XRD techniques. Single-crystal X-ray diffraction studies revealed that the title compound crystallizes in the monoclinic space group Pbca with a = 12.5948(12), b = 11.4269(11), c = 14.8939(15) ?, V = 2143.5(4) ?~3, Z = 4, Dc = 1.523 g·cm-3, F(000) = 1012, μ = 1.038 mm~(-1), R = 0.0358 and w R2 = 0.0888(I 2σ(I)). Single-crystal X-ray diffraction analysis reveals that 1 is the first two-dimensional noninterpenetrating(4, 4) net coordination polymer based on the 2-thiobarbituric acid. Coordination polymer 1 exhibits two luminescent emission spectra at 477 and 489 nm with the excitation peak at 273 nm.  相似文献   

7.
An organic-inorganic hybrid based on α-Keggin-typed [BW12O40]5- anionic cluster, [Co(BⅡM)3]2H[BW12O40]·7H2O(BⅡM = 2,2′-biimidazole), was hydrothermally synthesized and structurally characterized by thermogravimetric analysis, IR and UV spectra. The title compound crystallizes in monoclinic, space group P21/n with a = 12.3490(10), b = 33.270(3), c = 18.9660(16) β = 105.9950(10)°, V = 7490.5(11) 3, C36H50BCo2N24O47W12, Mr = 3905.80, Dc = 3.451g/cm3, μ(MoKα) = 18.886 mm-1, F(000) = 6972, Z = 4, S = 1.004, the final R = 0.0404 and wR = 0.0914 for 14683 observed reflections(I 2σ(I)). The compound consists of two isolated [Co(BⅡM)3]2+ cations and one [BW12O40]5- anion, in which each Co2+ ion is coordinated by six N atoms from three BⅡM ligands displaying a regular CoN6 octahedron. These components are finally linked together via N–H···O(polyoxometalate and water) hydrogen bonds into a two-dimensional framework. Full investigation of the intermolecular interactions by Hirshfeld surface and fingerprint plots clearly indicates that there are rare W–Oterminal···πimidazole ring interactions which cooperate with the classical N–H···O hydrogen bonds to stabilize the structural packing.  相似文献   

8.
The title compound N-tert-butyl-N-(4-methyl-1,2,3-thiadiazole)-5-yl-N'-(4-me-thyl-1,2,3-thiadiazole)-5-formyl-N'-3,5-dichloropyrid-2-yl-diacylhydrazines (C18H17Cl2N7O3S2, Mr = 514.41) has been synthesized by the reaction of N-tert-butyl-N'-3,6-dichloropyridine-2-formyl hydrazine with 4-methyl-1,2,3-thiadiazole-5-carbonyl chloride and triethylamine, and its structure was characterized by 1H NMR, HR MS, and single-crystal X-ray diffraction. The crystal of the title compound belongs to monoclinic, space group C2/c with a = 27.726(8), b = 11.045(3), c = 14.507(4), β = 96.758(4)°, Z = 8, V = 4412(2) 3, Dc = 1.549 g/cm3, μ = 0.521 mm-1, F(000) = 2112, R = 0.0405 and wR = 0.1153. X-ray analysis indicates that all rings are non-planar in this molecule. The bioassay results indicate that both the title compound and the positive control RH-5992 have weak fungicide activities, while the title compound has good insecticidal activity against Plutella xylostella L. and no insecticidal activity against Culex pipiens pallens.  相似文献   

9.
A new compound has been synthesized under hydrothermal conditions and characterized by IR, elemental analysis, XPS and single-crystal X-ray diffraction analysis. The title compound [Mn(en)3]2en0.5[HV16O38(Cl)]·4.5H2O crystallizes in monoclinic, space group C2/c, with a = 17.016(4), b = 18.858(4), c = 18.872(4) (A), β = 93.667(4)°, V = 6043(2) (A)3, Z = 4, Dc = 2.242 g/cm3, Mr = 2040.12, F(000) = 4020, μ = 2.895 mm-1, Rint = 0.0921, R = 0.0649 and wR = 0.1325. Single-crystal X-ray structure analysis indicates that the title compound consists of a polyanion [HV8VV8IVO38(Cl)]4( cage, two [Mn(en)3]22 cations, four and a half lattice waters and a half ethylenediamine. In addition, intermolecular O-H…N,O-H…O and C-H…O and C-H…O hydrogen bonds link the molecules together to form a three-dimensional structure.  相似文献   

10.
The novel title compound 4-chlorobenzaldehyde (2-trifluoromethyl-5,6,7,8- tetrahydrobenzo[4,5]thieno[2,3-d]pyrimidin-4-yl)hydrazone monohydrate (C18H14ClF3N4SH2O, Mr = 428.86) has been synthesized by a condensation reaction of 4-chlorobenzaldehyde with (2-trifluoromethyl-5,6,7,8-tetrahydrobenzo[4,5]thieno[2,3-d]pyrimidin-4-yl)hydrazine, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c with a = 7.4252(7), b = 26.344(2), c = 10.3095(9) , = 109.407(2)°, V = 1902.0(3) 3 , Z = 4, Dc = 1.498 g/cm3 , μ = 0.356 mm-1 , F(000) = 880, the final R = 0.0564 and wR = 0.1681 for 2343 observed reflections with I > 2 (I). X-ray diffraction analysis reveals that the title hydrazone molecule is nearly planar except for the cyclohexene and trifluoromethyl moieties. In the crystal packing, the molecules form stacks by a three-dimensional framework, which results from intermolecular N(3)-H(3)···O(1), O(1)-H(1B)···N(2), O(1)- H(1B)···N(4) and O(1)-H(1A)···F(1) hydrogen bonds via water molecules together with π-π stacking interactions. Molecular geometry of the title compound in the ground state optimized by B3LYP functional with 6-311G** basis sets indicates that the calculations are in agreement with the experimental data. The preliminary bioassay suggested that the title compound exhibits relatively good fungicidal activity against Fusarium oxysporium f.sp.vasinfectum and Dothiorella gregaria.  相似文献   

11.
One novel polyoxometalate compound connected via trivalent cerium cation as bridge H2{[K(H2O)2]2[Ce(H2O)5]2(H2Mo1.16W10.84O42)}·8H2O 1 was designed and synthesized in aqueous solution. X-ray diffraction analysis reveals that the structure of 1 is a three-dimensional framework assembled from the arrangement of H2Mo1.16W10.84O42 (named paradodecmetalate-B) and Ce(H2O)53 containing two planes, which are constructed through the unification of H2Mo1.16W10.84O4210- and Ce(H2O)53 along the [100] and [001] directions. Crystal data H96Ce4K4Mo2.32O128W21.68, Mr = 7074.89, monoclinic, P21/n, a = 12.5037(17), b = 17.002(2), c = 12.7473(17) (A), β = 105.966(2)°, V = 2605.4(6) (A)3, Z = 1, Dc = 4.509 g/cm3, F(000) = 3132, μ = 26.098 mm(1, R = 0.0377 and wR = 0.0789 (I > 2σ(I)).  相似文献   

12.
A novel supramolecular structural inorganic-organic hybrid [(4-bromoanilimiun)([18]crown-6)]_3[PMo_(12)O_40]·CH_3 CN has been synthesized through standard solvent evaporated method. The structure of the title compound was determined through single-crystal X-ray diffraction analysis. It crystallizes in monoclinic system with P21/n space group. The crystal data are a = 18.9529(4), b = 26.4444(5), c = 19.0985(4) ?, β = 90.132(6)o, V = 9572.1(3) ?~3, Z = 4, Dc= 2.203 g·cm~(–1), μ = 14.956 mm~(–1), F(000) = 6192, S = 1.098, the final R = 0.0859 and w R(I 2σ(I)) = 0.2100. Supramolecular cations are constructed through strong N–H…O hydrogen bonding interaction between the six oxygen atoms of [18]crown-6 molecule and nitrogen atom of(4-bromoanilimiun) cation. Three kinds of different arranged supramolecular cations exist in the title compound, which are filled into the large space formed by [PMo_(12)O_40] polyoxoanions. Thermogravimentic differential thermal analysis revealed that hydrogen bonding interaction and intermolecular interaction play an important role in maintaining the stability of the title compound.  相似文献   

13.
A novel compound (NH4)2Y(H2O)8[PMo10V2O40]·10H2O has been prepared in an aqueous solution and characterized by elemental analysis, IR, and TG-DTG analysis. X-ray diffraction analysis was carried out on (NH4)2Y(H2O)8 [PMo10V2O40]·10H2O single crystal, which crystallizes in the monoclinic system of a space group P21/C with a=0.9871(3) nm,b=1.5424(5) nm,c=2.7924(9) nm,β=94.183(5)°and Z=2. In the compound, a two-dimensional network is constructed by the PMo10V2O405- anion and the Y(H2O)83 cation building blocks via hydrogen bonding exhibiting the porous structure.  相似文献   

14.
The title compound, [Cu2(DMPz)2PMo12O40]·HDMPz (1, DMPz = 2,5-dimethyl pyrazine), has been synthesized and characterized by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1 with a = 11.075(2), b = 11.551(2), c = 11.886(2) A.α = 106.352(2), β = 109.862(3), γ = 109.504(1)°, V = 1206.8(3) A3, C18H26CU2Mo12N6O40P, Mr = 2275.78, Z = 1, Dc = 3.131 g/cm3, μ = 4.011 mm^-1, F(000) = 1073, S = 1.066, the final R = 0.0389 and wR = 0.1056 for 3739 observed reflections with I 〉 2σ(I). The structural analysis indicates that the title compound is composed of Keggin clusters [PMo12O40]3- connected by one-dimensional [CB(DMPz)]2n^2n+ chains to form a two-dimensional grid layer with holes occupied by monoprotonated DMPz molecules. In the solid of the title compound, the 2D grid layers are stacked together in an ABAB packing mode.  相似文献   

15.
The title compound α,α'-bis(3,5-bismethyl-pyrozole-N-yl)-carbene-acetyl-isopro-penyl hydrazine (C16H22N6O, Mr = 314.40) has been prepared. It was characterized by elemental analysis as well as IR, MS, 1H-NMR and 13C-NMR spectra. Its crystal structure was determined by single-crystal X-ray diffraction, getting the following data: triclinic, space group P1 with a = 6.9734(16), b = 10.773(3), c = 12.001(3) A, α = 75.311(4), β = 82.695(4), γ = 77.143(4)°, Z = 2, V = 847.9(3) A3, Dc : 1.231 g/cm3, F(000) = 336 and μ(MoKα) = 0.082 mm-1 (λ = 0.71073 A). The results of crystal structure determination show that there exist intermolecular and intramolecular hydrogen bonds, resulting in a two-dimensional supramolecular framework of the title compound. The binding of the title compound to DNA was investigated by absorption, emission, and viscosity measurements. The title compound shows absorption hyperchromicity accompanied by a blue shift at about 254 nm. The binding constant Kb for the title compound has been determined to be 1.89 × 104 M-1 from absorption measurements. The addition of the title compound to DNA pretreated with EB causes appreciable reduction in the emission intensity, indicating that the DNA-bound EB fluorophore is partially replaced by the title compound. The value of K is 3.093 × 104 M-1. The relative viscosity of DNA decreased with the addition of the title compound. Results suggest that the title compound binds to DNA with a non-classical intercalative or groove interaction mode. The observed efficient nuclease activity of the title compound is interesting and may have further influences on the chemistry of DNA minor groove binders.  相似文献   

16.
The title compound has been synthesized by the reaction of [RuCl2(PPh3)3] and closo-[B10H10]2- in (CH3)2CHOH solution. Crystals suitable for a single crystal X-ray diffraction analysis were obtained from n-pentane diffused to CH2Cl2 solution. The crystal {(PPh3)2ClRu(μ-Cl)Ru(PPh3)B10H7[OCH(CH3)2]3}·0.4(H2O) is monoclinic , space group P21/n , Mr=1359.47, with a=19.434(4), b =14.340(4), c=25.865(9)(A), β= 95.48(3)°, V=7175(4)(A)3, Dc=1.258 g/cm3, Z=4, λ(MoKα)=0.71073(A),μ=6.03 cm-1, F(000)=2784, R=0.0631, wR2= 0.1425, S=1.001. The title compound is a bimetallic species in which the second ruthenium center is bound to the cluster {(PPh3)RuB10H7[OCH(CH3)2]3} via an Ru-Cl-Ru and two Ru-H-B-Ru bridges. The third isoproxy group replaces a hydrogen atom on B(10) of the cage, which indicates the activity of the cage.  相似文献   

17.
One novel polyoxometalate compound connected via trivalent cerium cation as bridge H2{[K(H2O)2]2[Ce(H2O)5]2(H2Mo1.16W10.84O42)}·8H2O 1 was designed and synthesized in aqueous solution. X-ray diffraction analysis reveals that the structure of 1 is a three-dimensional framework assembled from the arrangement of H2Mo1.16W10.84O42 (named paradodecmetalate-B) and Ce(H2O)53+ containing two planes, which are constructed through the unification of H2Mo1.16W10.84O4210- and Ce(H2O)53+ along the [100] and [001] directions. Crystal data: H96Ce4K4Mo2.32O128W21.68, Mr = 7074.89, monoclinic, P21/n, a = 12.5037(17), b = 17.002(2), c = 12.7473(17) A, β = 105.966(2)°, V = 2605.4(6) 3, Z = 1, Dc = 4.509 g/cm3, F(000) = 3132, μ = 26.098 mm-1, R = 0.0377 and wR = 0.0789 (I > 2σ(I)).  相似文献   

18.
The first primary organicamine templated indium iodate with the formula (H2en)KIn(IO3)6·2(H2O) was hydrothermally synthesized via reaction at 100 °C for 7 d and characterized by single-crystal X-ray diffraction and thermal analysis. The compound crystallized in a triclinic system with space group P1, a=0.69803(14) nm, b=0.70863(14) nm, c=1.2091(2) nm, α=76.417(4)°, β=79.953(4)°, γ=72.206(3)°, V=0.55012(19) nm3. Structure determination indicates that it is made up of zero-dimensional units each of which consists of [In(IO3)6]3-anion, potassium, water and ethylenediamine cation. The most striking feature of the compound is that it possesses helical hydrogen bonds formed by organic amine template, water molecules and inorganic network.  相似文献   

19.
A new compound has been synthesized under hydrothermal conditions and characterized by IR,elemental analysis,XPS and single-crystal X-ray diffraction analysis. The title compound [Mn(en)3]2en0.5[HV16O38(Cl)]·4.5H2O crystallizes in monoclinic,space group C2/c,with a=17.016(4),b=18.858(4),c=18.872(4),β=93.667(4)o,V=6043(2)3,Z=4,Dc=2.242 g/cm3,Mr=2040.12,F(000)=4020,μ=2.895 mm-1,Rint=0.0921,R=0.0649 and wR=0.1325. Single-crystal X-ray structure analysis indicates that the title compound consists of a polyanion [HV8VV8IVO38(Cl)]4-cage,two [Mn(en)3]22+ cations,four and a half lattice waters and a half ethylenediamine. In addition,intermolecular O-H···N,O-H···O,N-H···O and C-H···O hydrogen bonds link the molecules together to form a three-dimensional structure.  相似文献   

20.
陈顺玉  杨娥  张健 《结构化学》2013,32(1):149-153
A new Zn(Ⅱ) coordination polymer [Zn3(btec)(OH)2(H2O)2]n (1, btec = 1,2,4,5- benzenetetracarboxylate) has been synthesized by hydrothermal reaction and its structure was determined by single-crystal X-ray diffraction analysis. The title compound crystallizes in mono- clinic, space group C2/c, with a = 19.580(3), b = 5.0137(8), c = 15.975(3), β = 121.629(2)°, V = 1335.3(4)3, C10H8O12Zn3, Mr = 516.27, Z = 4, Dc = 2.568g/cm3, μ = 5.419 mm-1, F(000) = 1016, R = 0.0590 and Rw = 0.1279 for 1110 observed reflections (I > 2σ(I)). X-ray analysis shows that the asymmetric unit of the title compound contains two crystallographically unique Zn(Ⅱ) atoms which are connected through the bridging carboxylate oxygen atoms of the btec ligands and μ2-bridging oxygen atoms of water molecules to generate an infinite one-dimensional chain. The adjacent chains are linked together through the benzene rings of the btec ligands to form a two-dimensional polymeric network. The adjacent two-dimensional layers are further connected together by the benzene rings of btec ligands to give the final three-dimensional structure. The benzene rings act as pillars between two layers.  相似文献   

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