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1.
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   

2.
A new cerium complex, (C7H8)[Ce(C7H3NO5)2(H2O)3]·2H2O or (C7Hs)[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 I crystallizes in monoclinic, space group P21/c with a = 12.4267(9), b = 10.8195(7), c = 19.5650(13)A, β = 92.898(3)°, V = 2627.2(3) A^3, Dc = 1.733 g/cm^3, Z = 4, Mr = 685.55, μ = 1.809 mm^-1, λ(MoKa) = 0.71073A 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 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   

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 lanthanum(III) complex, [LaL2(NO3)3].H2O (1) based on L (L = N-(na- phthalene-l-yl)-2-(quinolin-8-yloxy)acetamide), was synthesized and characterized by X-ray diffraction. The crystal of I belongs to the monoclinic system, space group C2c with Mr= 1017.69, a = 25.1438(17), b = 13.5950(9), c = 18.2349(12) A, β= 132.4980(10)° V= 4595.8(5) A3, Z= 4, Dc = 1.471 Mg/m3, F(000) = 2056,μ= 1.004 mm-1, R = 0,0588 and wR = 0.1402. The central La(lI1) ion is coordinated to four oxygen atoms, two nitrogen atoms from two independent acetarnide ligands and six oxygen atoms from three nitrate anions, possessing a distorted icosahedron coordination geometry. In the crystal of 1, intermolecular N-H……O hydrogen bonds linked the molecules into chains along the c axis. In solid state and CH3CN solution, complex 1 exhibits stronger fluorescent emission than the ligand L.  相似文献   

6.
A novel lanthanum(Ⅲ) complex, [LaL2(NO3)3]·H2O(1) based on L(L = N-(naphthalene-1-yl)-2-(quinolin-8-yloxy)acetamide), was synthesized and characterized by X-ray diffraction. The crystal of 1 belongs to the monoclinic system, space group C2 c with Mr = 1017.69, a = 25.1438(17), b = 13.5950(9), c = 18.2349(12) A, β = 132.4980(10)°, V = 4595.8(5) A3, Z = 4, Dc = 1.471 Mg/m3, F(000) = 2056, μ = 1.004 mm-1, R = 0.0588 and wR = 0.1402. The central La(Ⅲ) ion is coordinated to four oxygen atoms, two nitrogen atoms from two independent acetamide ligands and six oxygen atoms from three nitrate anions, possessing a distorted icosahedron coordination geometry. In the crystal of 1, intermolecular N–H···O hydrogen bonds linked the molecules into chains along the c axis. In solid state and CH3 CN solution, complex 1 exhibits stronger fluorescent emission than the ligand L.  相似文献   

7.
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   

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 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   

10.
A one-dimensional chain coordination polymer [Co(Ⅱ)(C6H5CH--CHCOOH)2(4,4'- bipy)(H20)5]n has been synthesized with cinnamylic acid, 4,4'-bipy and cobaltous chloride as raw materials. Crystal data for this complex: monoclinic, space group P21/c, a = 1.1481(3), b = 1.1230(2), c = 1.1759(3) nm, β = 97.054(4)^o, V= 1.5046(6) nm^3, Mr= 617.50, Dc = 1.363 g/cm^3, Z = 2, ,u(MoKa) = 0.627 mm^-1, F(000) = 646, S = 1.062, R 0.0443 and wR = 0.1178. The crystal structure shows that two neighboring cobalt(ID ions are linked together by one 4,4'-bipy, and the whole complex molecule adopts a one-dimensional chain structure. Each cobalt(H) ion is coordinated with two nitrogen atoms from two 4,4'-bipy molecules and four oxygen atoms from four water molecules, giving a distorted octahedral coordination geometry. The electrochemical properties were analyzed by combining with the crystal structure.  相似文献   

11.
One-dimensional chain copper(Ⅱ) coordination polymer has been synthesized and characterized in the solvent mixture of water and alcohol with o-acetamidobenzoic acid,4,4'-bipyridine and copper perchlorate.It is of tetragonal,space group P41212 with a=1.57756(10),b= 1.57756(10),c=2.1438(3)nm,V=5.3352(8) nm3,Dc=1.524 g/cm3,Z=4,F(000)=2536,R= 0.0479 and wR=0.0979.The crystal structure shows two coordination modes.The copper(1) is coordinated with two nitrogen atoms of one 4,4'-bipyridine molecule and two oxygen atoms from two o-acetamidobenzoic acid molecules,forming a distorted tetrahedral coordination geometry;the copper(2) is coordinated with two nitrogen atoms of one 4,4'-bipyridine molecule,four oxygen atoms from two o-acetamidobenzoic acid molecules and two water molecules,generating a distorted octahedral coordination geometry.The result of TG analysis shows that the title complex is stable below 180.0 ℃.  相似文献   

12.
A new Schiff base Dibenzoyl-bissemicarbazone C15H16N6O2(L) and its complex with neodymium(Ⅲ ) perchlorate [NdL2(H2O)2](ClO4)3 were synthesized. The crystal and molecular structure of the title complex were determined by single crystal X-ray diffraction. The crystal is monoclinic and conforms to space group P. with cell constants a=10. 893(2) A, b= 12. 118(3) A , c=22. 494(5) A , β=89. 86(3)% V = 2969.19A3. The final standard deviation R=0. 0919. In the complex Nd is coordinated by four nitrogen and six oxygen atoms, of which four nitrogen and four oxygen atoms are provided by two neutral ligands L, and the other two oxygen atoms are provided by two water molecules, forming a ten-coordinated complex cation, which the perchlorate groups exist in the outer sphere. The coordination polyhedron takes a bicapped anti-square prism arrangement. That the average bond length of Nd-N is 2. 735 A indicates that the coordination of N in groups to Nd( Ⅲ ) is very weak.  相似文献   

13.
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   

14.
The coordination polymer [Zn(HCOO)2(H2O)2]∞ has been synthesized using hydrothermal method and characterized by X-ray single crystal diffraction, elemental analysis, FTIR spectroscopy and TG-DTG analyses. The coordination polymer crystallizes in monoclinic, P21/c space group with crystal parameters of α=0.8688(1) nm, b= 0.7143(6) nm, c=0.9305(2) nm, β=97.61(5)°, V=0.5724(2) nm^3, Z=4, μ(Mo Kα)=42.50 cm^-1. The polymer features with two kinds of zinc centers: one is hexa-coordinated by four water ligands, two oxygen atoms of two formates and the other is coordinated by six oxygen atoms of six formates. By the formates as space linkers, three-dimensional frameworks were formed. Based on thermal analyses, thermal decomposition mechanisms were predicted that at the first step the polymer lost two coordination water molecules and at the second step lost two formates companied by the formation of some kinds of materials.  相似文献   

15.
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   

16.
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   

17.
<正> Crystal of the title complex K10H3[Dy(SiMo11O39)2]·29H2O(Mr= 4331.85) is monoclinic with space group P21/n,a= 17. 256(1) ,b = 26. 817(1) ,c = 21.797(1) A,β= 104. 39(1)°, V = 9770. 2 (A3), Z= 4, F (000) = 8140, and Dc= 2. 94g/cm3. The Dy3+ is coordinated by eight oxygen atoms from two tetradentate (SiMo11O39)8- ligands,forming a square antiprism. The cation K+ is coordinated by oxygen atoms from heteropoly ligands (SiMo11O39)8- and water molecules, the number of atoms that are coordinated to the potassium atoms can be divided into four groups:six,seven, eight and nine.  相似文献   

18.
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   

19.
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   

20.
A new metal-organic coordination polymer [Cd(5-hip)(phen)]n·nH2O 1 has been hydro- ermally synthesized and characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. The crystal of the complex crystallizes in monoclinic, space group P2/n with a = 8.8071(17), b =12.386(2), c = 16.981(3) A, β = 100.182(2)°, V = 1823.2(6) A^3, Mr=. 490.73, Dc =1.788 g/cm^3,μ(MoKa) = 1.240 mm^-1, F(000) = 976, Z= 4, the final R = 0.0458 and wR = 0.1373 for 2864 observed reflections (I 〉 2σ(I)). The Cd atoms are coordinated by two N atoms from the phen ligands and four O atoms from 5-hydroxyisophthalate ligands in a highly distorted octahedral geometry.  相似文献   

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