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1.
A new lanthanum complex, (H3O)2[La(C7H3NO5)2(H2O)212.3(H2O) or (HaO)E[La(HChel)2(HEO)E]2.3(H2O) 1 (H3Chel = 4-hydroxypyridine-2,6-dicarboxylic(chelidamic) acid), has been prepared by the hydrothermal reaction, and its crystal structure was determined based on single-crystal diffraction data. Compound I crystallizes in triclinic, space group Pi with a = 9.6939(19), b = 10.176(2), c = 11.502(2)A, α = 111.52(3), β = 93.74(3), γ = 103.33(3)°, V = 1013.0(3)A3, Dc = 1.912 g/cm3, Z = 1, Mr = 1166.40, p = 2.188 mm-1, 2(MoKa) = 0.71073 A and F(000) = 574. The final R = 0.0342 and wR = 0.0737 for 4080 observed reflections with I 〉 2σ(I), and R = 0.0429 and wR = 0.0772 for all data. Compound 1 contains two lanthanum ions, four chelidamic acid ligands, four coordinated water molecules, two hydroniums, and three discrete water molecules. The LaⅢ atom is ten-coordinated by four oxygen and two nitrogen atoms from two tridentate chelating chelidamic acid ligands, two carboxylic oxygen atoms from an adjacent chelidamic acid ligand and two coordinated water molecules, leading to a distorted dodecahedral geometry. A three-dimensional network is formed by H-bonds.  相似文献   

2.
A new cerium complex,(C7H8)[Ce(C7H3NO5)2(H2O)3]·2H2O or (C7H8)[Ce(HChel)2-(H2O)3]·2H2O (1,H3Chel = 4-hydroxypyridine-2,6-dicarboxylic (chelidamic) acid),has been prepared by the hydrothermal reaction,and its crystal structure was determined based on single-crystal diffraction data. Compound 1 crystallizes in monoclinic,space group P21/c with a = 12.4267(9),b = 10.8195(7),c = 19.5650(13),β = 92.898(3)o,V = 2627.2(3) 3,Dc = 1.733 g/cm3,Z = 4,Mr = 685.55,μ = 1.809 mm-1,λ(MoKα) = 0.71073  and F(000) = 1372. The final R = 0.0455 and wR = 0.1984 for 5983 observed reflections with Ⅰ > 2σ(Ⅰ),and R = 0.0490 and wR = 0.2053 for all data. Complex 1 contains one cerium ion,two chelidamic acid ligands,three coordinated water molecules,one discrete toluene molecule,and two discrete water molecules. The Ce(IV) ion is nine-coordinate with the coordination polyhedron made up of four oxygen atoms and two nitrogen atoms from two tridentate chelating chelidamic acid ligands,and three coordinated water molecules. A three-dimensional network is formed by the H-bonds. Moreover,optical properties are investigated and the results show that this complex has sharp optical absorption at 221,396 and 571 nm but no marked fluorescent emission.  相似文献   

3.
A new lanthanum complex, (H3O)2[La(C7H3NO5)2(H2O)2]2·3(H2O) or (H3O)2[La(HChel)2(H2O)2]2·3(H2O) 1 (H3Chel = 4-hydroxypyridine-2,6-dicarboxylic(chelidamic) acid), has been prepared by the hydrothermal reaction, and its crystal structure was determined based on single-crystal diffraction data. Compound 1 crystallizes in triclinic, space group P with a = 9.6939(19), b = 10.176(2), c = 11.502(2) (A), α = 111.52(3), β = 93.74(3), γ = 103.33(3)°, V = 1013.0(3) (A)3, Dc = 1.912 g/cm3, Z = 1, Mr = 1166.40, μ = 2.188 mm-1, λ(MoKα) = 0.71073 (A) and F(000) = 574. The final R = 0.0342 and wR = 0.0737 for 4080 observed reflections with I > 2σ(I), and R = 0.0429 and wR = 0.0772 for all data. Compound 1 contains two lanthanum ions, four chelidamic acid ligands, four coordinated water molecules, two hydroniums, and three discrete water molecules. The LaIII atom is ten-coordinated by four oxygen and two nitrogen atoms from two tridentate chelating chelidamic acid ligands, two carboxylic oxygen atoms from an adjacent chelidamic acid ligand and two coordinated water molecules, leading to a distorted dodecahedral geometry. A three-dimensional network is formed by H-bonds.  相似文献   

4.
A new cobalt complex Co(C10H8N2)(H2O)3[C9H11O2(COO)] with methy-5-norbor- nene-2,3-dicarboxylic anhydride acid (MNA) and 2,2'-bipyridine as ligands has been synthesized in the mixed solvents of ethanol and water. It crystallizes in monoclinic, space group P21/c with α = 13.0430(13), b = 21.014(2), c = 7.5151(7) ?, β = 102.319(2)o, V = 2012.4(3) A3, Dc = 1.529 g/cm3, Z = 4, F(000) = 964, GOOF = 1.051, the final R= 0.0457 and wR= 0.0974. The crystal structure shows that the cobalt ion is coordinated with four oxygen atoms from one MNA molecule and three water molecules together with two nitrogen atoms from the 2,2'-bipyridine molecule, forming a distorted octahedral coordination geometry. The thermal stabilityand electrochemical properties have studied in this paper.  相似文献   

5.
A novel one-dimensional chain coordination polymer [Mn(NAAh(4,4′-bipy)(H2O)4], has been synthesized with a-naphthaleneacetic acid, 4,4′-bipy and manganese(Ⅱ) sulfate as raw materials. Crystal data for this complex: monoclinic, space group P21/c, a = 1.1421(2), b = 1.6337(3), c = 0.94177(19) nm, β = 112.15(3)°, V = 1.6275(6) nm^3, De = 1.407 g/cm^3, Z = 2, μ(MoKa) = 0.467 mm^-1, F(000) = 722, S = 1.007, R= 0.0412 and wR = 0.1022. The crystal structure shows that two neighboring manganese(Ⅱ) ions are linked together by one 4,4′-bipy molecule, and the whole complex molecule forms a one-dimensional chain structure. Each manganese(Ⅱ) ion is coordinated with two oxygen atoms of two a-naphthaleneacetic acid molecules, two nitrogen atoms of two 4,4′-bipy molecules and two oxygen atoms from two water molecules, giving a distorted octahedral coordination geometry. The electrochemical properties were also analyzed.  相似文献   

6.
A new 1D chain copper coordination polymer [CuE(H2L)2(C10HsN2)(HEO)2]n'3n(H20) with 2,3-pyridinedi carboxylic acid (H2L) and 2,2'-bipyridine (2,2'-bipy) as ligands has been synthesized in the mixed ethanol and water solvents. Crystal data for this complex are as follows: monoclinic, space group P2Jc, a = 7.7713(7), b = 27.478(3), c = 13.2621(13)/1,, fl = 100.6940(10), V= 2782.8(5) A3, Dc = 1.722 g/cm3, Z = 4, p = 1.61 mm-1, F(000) = 1472, the final R = 0.0363 and wR = 0.0933. In the crystal structure, the whole molecule consists of two cooper ions, two H2L, one 2,2"-bipy molecule and six water molecules. Each central copper ion is coordinated with three oxygen atoms from two H2L and one water molecule, two nitrogen atoms from one 2,2'-bipy molecule and two H2L, giving a distorted tetragonal pyramidal geometry. Thermal stability properties of the complex were investigated.  相似文献   

7.
A new complex, [Cd(Himc)2(H2O)2] 1, obtained from imidazole-4-carboxylatic acid (H2imc) and Cd(ClO4)2·6H2O, has been synthesized. The crystal structure was determined by X-ray diffraction. The title compound crystallizes in the orthorhombic system, space group Pccn, with a = 7.4886(11), b = 11.9667(18), c = 13.550(2) A, V= 1214.3(3) A3, Z = 4, Mr= 370.60, Dc = 2.027 mg/m3, F(000) = 728,μ (MoKa) = 1.829 mm^-1, the final R = 0.0243 and wR = 0.0591 for 1150 unique reflections with I 〉 2σ(I). The cadmium(II) center in the title complex is coordinated with two oxygen and two nitrogen atoms from two bidentate chelated imidazole-4-carboxlate ligands together with two water molecules, giving a distorted octahedral coordination geometry. A one-dimensional hydrogen bonding chain is formed via intermolecular O-H...O hydrogen bonds, and such adjacent chains are further stacked through intermolecular π-π and hydrogen bonding interactions to form a 3D supramolecular framework. Complex 1 exhibits a fluorescent emission band at 290 nm (λex = 236 nm) in the solid state.  相似文献   

8.
The title compound [Zn(btzb)2Cl2]·2H2O (1·2H2O, btzb = 1,2-bis(5-tetrazolyl)ben- zene) was synthesized in situ by the [2+3] cycloaddition reaction of phthalonitrile with NaN3 in water in the presence of ZnCl2 under refluxing conditions. 1·2H2O crystallizes in the monoclinic system, space group P2 1/c with a = 9.0119(18), b = 7.5566(15), c = 18.076(5)A, β= 114.67(2)°, V= 1118.6(4)A^3, Z = 2, Dc = 1.784 g/cm^3, T= 223(2) K, C16H16N16O2Cl2Zn, Mr = 600.74, F(000) = 608, μ(MoKα) = 1.393 mm^-1, S = 1.081, R = 0.0306 and wR = 0.0669 for 1896 observed reflections with I 〉 2σ(I). The Zn^2+ ion of 1 is coordinated by four N atoms from two btzb ligands and two Cl atoms, forming a distorted octahedral coordination geometry. A number of intermolecular hydrogen bon- ding interactions between molecules 1 and/or the solvated water molecules result in a 3D hydrogen-bonded structure. The luminescent property of 1·2H2O was also investigated.  相似文献   

9.
A new copper(Ⅱ) compound has been prepared and fully characterized by elemen-tal analysis,IR,TG and single-crystal X-ray diffraction.The compound [Cu(4-hba)2(inta)(H2O)]·H2O (4-hba=4-hydroxybenzoic acid,inta=isonicotinamide) 1 crystallizes in the monoclinic system,space group P21/c with a=7.590(5),b=11.027(5),c=23.761(5),β=102.5740(10)o,V=1974.1(16) 3,Mr=991.84,Z=2,Dc=1.669 g/cm3,F(000)=1020,μ=1.166 mm-1,R=0.0353 and wR=0.0604 for 3166 observed reflections (I 2σ(I)).In compound 1,the copper cation is penta-coordinated with two carboxylate oxygen atoms from two different 4-hba ligands,two oxygen atoms from two coordinated water molecules and one nitrogen atom from inta ligand,showing a slightly distorted square-pyramidal geometry.  相似文献   

10.
A three-dimensional coordination polymer {[Dy(H2btec)2/4(btec)3/6(H2O)]·2H2O} n has been synthesized through the reaction of DyCl3·6H2O and 1,2,4,5-benzenetetracarboxylic acid by solvothermal technique, and the crystal structure was determined by X-ray diffraction. The Dy(Ⅲ) coordination polymer crystallizes in monoclinic, space group P21/n with a=10.7063(1), b=7.1491(1), c=17.1197(3), α=90, β=97.10, γ=90°, V=1300.31(3)3 , C10H9DyO11 , Dc=2.389g/cm3 , Z=4, F(000)=892, the final R=0.0165 and wR=0.0448 for I > 2σ(I). The title coordination polymer possesses a three-dimensional framework consisting of nine-coordinate Dy(Ⅲ) centers and two kinds of coordination modes for the 1,2,4,5-benzenetetracarboxylic acid ligands. Every btec4- ligand (deprotonated four protons from 1,2,4,5-benzenetetracarboxylic acid) in the title coordination polymer can clamp three Dy atoms like forceps, which could make the Dy atoms closer in the area of metal-metal interaction. The 3-D framework of the coordination polymer has many channels occupied by the free guest water molecules, and the hydrogen bonds between the coordinated carboxylic groups and guest water molecules could stabilize the crystal structure of the title coordination polymer. In addition, the luminescence properties were also studied.  相似文献   

11.
杨燕  曾明华  张来军  梁宏 《结构化学》2009,28(7):785-788
A novel tetranuclear zinc(H) coordination polymer [Zn4(o-bda)a(p-pbim)4]n 1 (p-pbim = 4-pyridylbenzimidazole, o-bda2 = o-phenylenediacetic acid dianion) has been synthesized by a hydrothermal method and characterized by elemental analysis, IR and X-ray singlecrystal diffraction. The title complex crystallizes in monoclinic, space group of P21/n with α = 14.231(1), b = 16.257(1), c = 16.794(1) ]k, β = 100.26(1)°, V = 3823.1(2)A3, Z = 8, Dc = 1.573 g/cm^3,β = 1.321 mm^-1, F(000) = 1856, R = 0.0420 and wR = 0.111. The Zn(1) atom assumes a distorted trigonal bipyramidal geometry, involving three carboxyl O atoms from two different o-bda ligands and two N atoms from two p-pbim ligands. The Zn(2) atom is coordinated by two oxygens from two distinct bda2- anions and two nitrogen atoms from two p-pbim ligands to form a distorted tetrahedral geometry. The Zn(Ⅱ) atoms are alternately interlinked by o-bda ligands in bis-monodentate or chelating-bidentate and monodentate modes into one-dimensional undulate chains along axis c with the adjacent Zn…Zn distances of 8.32 and 8.47 A. Such neighboring chains are further extended into a 1D bi-chain structure with two different subrings A and B, which are 32- and 14-membered rings through interchain p-pbim ligands. There exists a 2D supramolecular network linked by intermolecular hydrogen-bonding interactions between the uncoordinated carboxylate 0(4) atom or coordinated carboxylate 0(7) atom and the uncoordinated imidazolyl N(2) and N(5) atoms with the O...N distances to be 2.695 and 2.807A.  相似文献   

12.
The title complex, [Ce(BA)3phen]2 (BA = benzoate, phen = 1,10-phenanthroline), was prepared by the reaction of Ce(NO3)3.6H2O, benzoic acid and 1,10-phenanthroline. The complex was characterized by single-crystal X-ray diffraction, elemental analysis, IR spectra and TG-DTG techniques. The results show that the crystal is of triclinic, space group P1 with a = 10.912(2), b = 11.962(3), c = 12.474(3) A, α = 104.889(3), β = 93.523(3), γ = 113.332(3)^o, C66H46Ce2N4O12, Mr = 1366.90, V= 1420.2(6) ,A^3, Z = 1, Dc = 1.598 g/cm^3, μ = 1.652 mm^-1, S = 1.024 and F(000) = 682. The final R = 0.0391 and wR = 0.0947 for 4878 observed reflections with I 〉 2σ(I). The structure of the title complex consists of two Ce(C6HsCOO)3(C12H8N2) units, forming a binuclear molecule. Each Ce(Ⅲ) is coordinated by two O atoms of one bidentate chelating carboxylate group, five O atoms of two bidentate bridging and two tridentate chelating-bridging carboxylate groups, and two N atoms of one 1,10-phenanthroline molecule to complete a distorted monocapped square antiprism geometry. Its thermogravimetric analysis was determined by TG-DTG techniques.  相似文献   

13.
A new two-dimensional Cd(Ⅱ) coordination polymer, [Cd(2,5-pdch)(H2O)]n·2n(ClO4)·nH2O (2,5-pdch = pyridine-2,5-dicarbohydrazide), was prepared and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction analysis. The crystal belongs to monoclinic, space group P21/c with a = 10.905(2), b = 11.602(1), c = 15.034(2) A, β = 117.794 (10°, V = 1682.8(4A3, Z = 4, C7H13CdCl2NsO12, Mr = 542.52, Dc = 2.141 g/cm^3,/μ = 1.691 mm^-1, F(000) = 1072, 2(MoKa) = 0.71073A, the final R = 0.0608 and wR = 0.1329 for 2972 observed reflections with I 〉 2σ(I). Single-crystal X-ray diffraction analysis reveals that the Cd(Ⅱ) atom displays a distorted pentagonal-bipyramidal geometry coordinated by three N atoms and three O atoms from three different 2,5-pdch ligands, and one water molecule. Interestingly, each two Cd(Ⅱ) atoms are bridged by two carbohydrazide groups of the 2,5-pdch ligands to form a dimeric unit, and such dimeric units are further connected by the 2,5-pdch ligand to generate a two-dimensional (4,4)-network.  相似文献   

14.
A new cobalt complex Co(C10H8N2)(H2O)3[C9H11O2(COO)] with methy-5-norbornene-2,3-dicarboxylic anhydride acid(MNA) and 2,2'-bipyridine as ligands has been synthesized in the mixed solvents of ethanol and water. It crystallizes in monoclinic, space group P21/c with a = 13.0430(13), b = 21.014(2), c = 7.5151(7) ?, β = 102.319(2)o, V = 2012.4(3) ?3, Dc = 1.529 g/cm3, Z = 4, F(000) = 964, GOOF = 1.051, the final R = 0.0457 and wR = 0.0974. The crystal structure shows that the cobalt ion is coordinated with four oxygen atoms from one MNA molecule and three water molecules together with two nitrogen atoms from the 2,2'-bipyridine molecule, forming a distorted octahedral coordination geometry. The thermal stability and electrochemical properties have studied in this paper.  相似文献   

15.
A new coordination compound [Ba(OBPT)2(H2O)2]·H2O was obtained at room temperature by the reaction of 4,6-bis(2-pyridyl)-1,3,5-triazin-2-ol(HOBPT) with BaCl2.It was characterized by elemental analysis,FTIR,TG analysis,powder X-ray diffraction analysis and single-crystal X-ray diffraction analysis.The complex crystallizes in the monoclinic P21/n space group,with a = 16.325(1),b = 6.7977(5),c = 24.164(2) ,β = 104.009(1),V = 2601.8(3) 3,Z =4,C26H22BaN10O5,Mr = 691.88,Dc = 1.766 g/cm3,F(000) = 1376 and μ(MoKα) = 1.587 mm-1.The final R = 0.0282 and wR = 0.0724 for 5095 observed reflections with I > 2σ(I) and R = 0.0312 and wR = 0.0744 for all data.In the complex,the barium ion is ten-coordinated with six nitrogen atoms from two ligands,two deprotonated hydroxyl oxygen atoms from another two ligands and two coordinated water molecules to form a double stranded chain.The extensive supramolecular interac-tions lead to the formation of an infinite 2D framework.  相似文献   

16.
徐涵  李一志 《结构化学》2010,(11):1606-1611
A novel NiII complex [{Ni(IBG)(4,4'-bipy)(H2O)2}·3H2O]n 1 (H2IBG = isophthaloylbisglycine and 4,4'-bipy = 4,4'-bipyridine) has been synthesized and characterized by singlecrystal X-ray diffraction, elemental analysis, IR spectra and thermogravimetric analysis. It crystallizes in monoclinic, space group P2/c with a = 15.5420(7), b = 22.4344(1), c = 8.3455(5), β = 101.538(3)o, V = 2670.1(7)3, Z = 4, C22H32N4NiO13, Mr = 619.23, Dc = 1.443 g/cm3, F(000) = 1296.0, μ(MoKα) = 0.750 mm-1, the final R = 0.0570 and wR = 0.1445 for 2296 observed reflections with I 2σ(I). In the structure, the NiII metal center is coordinated in an octahedral environment arranged by two water molecules, two carboxylate oxygen atoms and two nitrogen atoms from two 4,4'-bipy ligands. Thermal decomposition and powder X-ray diffraction results indicate that the transformation from the crystal form, [{Ni(IBG)(4,4'-bipy)(H2O)2}·3H2O]n, to the amorphous powder, Ni(IBG)(4,4'-bipy)(H2O)2, is reversible, so the latter form may be utilized as an absorbing agent for water and water vapor.  相似文献   

17.
The title compound Cd(Eim)3Cl2 (Eim = N-ethylimidazole) I has been synthesized and structurally characterized by single-crystal X-ray diffraction. The compound crystallizes in the monoclinic system, space group P2 1 with a = 8.0460(16), b = 29.186(6), c = 8.8960(18)A,β= 100.06(3)°, C15H24CdCl2N6, Mr = 471.71, V = 2056.9(7)A^3 Z = 4, Dc = 1.523 g/cm^3,/1 = 1.330 mm^-1, F(000) = 952, the final R = 0.0455 and wR = 0.0723. The title compound crystallizes with two molecules in the asymmetric unit. Each Cd^II ion is coordinated by three Eim ligands and two Cl anions in a trigonal bipyramidal geometry in two molecules. The weak intermolecular C-H……Cl hydrogen bonds link the molecules into two independent hydrogen-bonded chains running along the c axis. According to the cyclic voltammogram measurement in H2O, the electrode reaction should be a quasi-reversible process.  相似文献   

18.
李薇  李玉林  李昶红  谭雄文 《结构化学》2011,30(9):1279-1282
The nickel complex {Ni(2,2-bipy)(H2O)3[C8H11O2(COO)]}(H2O)3 with bicycle-[2.2.1]-2-hepten-5,6-dicarboxylic acid [C7H8(COOH)2] and 2,2'-bipyridine (bipy) as ligands has been synthesized and characterized. It crystallizes in monoclinic, space group P , with a = 0.74975(3), b = 1.20309(4), c = 1.30593(4) nm, α = 109.861(2), β = 98.519(2), γ = 90.575(2)o, V = 1.09337(7) nm3, Dc = 1.552 g/cm3, Z = 2, F(000) = 524, the final GOOF = 1.064, R = 0.0397 and wR = 0.1171. The crystal structure shows that the nickel ion is coordinated with four oxygen atoms from one bicycle[2.2.1]-2-hepten-5,6-dicarboxylic acid molecule and three water molecules and two nitrogen atoms from the 2,2′-bipyridine molecule, forming a distorted octahedral coordination geometry. The result of TG analysis shows that the title complex is stable under 200.0 ℃.  相似文献   

19.
A one-dimensional chain coordination polymer [Cu(phen)(2,4,6-TMBA)2(H2O)]n has been synthesized by reacting 2,4,6-trimethyl-benzoic acid, 1,10-phenanthroline and Cu(Ⅱ) perchlorate and its structure was characterized. Crystal data for this complex: tetragonal, space group I41, a = 2.0293(3), b = 2.0293(3), c = 1.3758(2) nm, α =β= γ = 90°, V= 5.6657(13) nm3, Dc= 1.379 g/cm3, Z = 8, μ(MoKa) = 0.815 mm-1, Mr = 588.14, F(000) = 2456, S = 1.047, R = 0.0459 and wR = 0.1053. The crystal structure shows that two neighboring Cu(Ⅱ) ions are linked together by one bridging-chelating 2,4,6-trimethyl-benzoic group, forming a one-dimensional chain structure. Each Cu(Ⅱ) ion is coordinated with two nitrogen atoms from one 1,10-phenanthroline molecule, three oxygen atoms from three 2,4,6-trimethyl-benzoic acid molecules and one oxygen atom from one water molecule, giving a six-coordinate distorted octahedral coordination geometry. The cyclic voltammetry behavior of the complex was also investigated.  相似文献   

20.
The mononuclear complex, Cu(H2SIP-O)(bpy)(H2O) (H4SIP-O = 4-hydroxyl- 5-sulfoisophthalic acid and bpy = 2,2'-dipyridyl), has been synthesized by the hydrothermal reaction of Cu(OH)2 with NaH2SIP and bpy at 160 ℃, and characterized by single-crystal X-ray diffraction, elemental analysis and IR spectrum. The new ligand 4-hydroxyl-5-sulfoisophthalic acid derived from 5-sulfoisophthalic acid ligand under an in situ hydrothermal condition. The crystal of the complex crystallizes in a triclinic system, space group P1, with a = 7.757(4), b = 10.663(6), c = 11.727(7)A, α = 94.272(4), β = 104.067(7), γ = 97.400(7)°, V= 927.4(9)A^3, Z = 2, C18H14N2O9SCu, Mr= 497.93, Dc= 1.783 g/cm^3,μ = 1.350 mm^-1, F(000) = 506, the final R = 0.0518 and wR = 0.1513 for 4180 observed reflections with I 〉 2σ(I). The central Cu(II) ion is five-coordinated by two oxygen atoms from the H2SIP-O^2- ligand and two nitrogen atoms of bpy ligand in a distorted square-planar geometry as well as a water oxygen atom in the apical position to complete a distorted square-pyramidal coordination geometry. The mononuclear copper molecules are linked by hydrogen bonds between coordinated water molecules and sulfonate groups to form a one-dimensional double-chain structure. The chains are further held together through extensive π-π stacking interactions between the aromatic rings to form a three- dimensional supramolecular structure.  相似文献   

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