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1.
Complex VO(C10H9NO3)(C13H10NO2)(C10H9NO2-3=N-salicylidene-L-alaninate, C13H10NO-2=N-phenylbenzohydroxamate) was synthesized and characterized by means of elemental analysis, IR, UV, 1H NMR spectroscopies, cyclic voltammetry and single crystal X-ray diffraction. The complex crystallized in a monoclinic system with space group P21 and crystal cell parameters a=0.9720(1) nm, b=1.8274(2) nm, c=1.2542(1) nm, β=104.868(9)°, V=2.1532(4) nm3, Mr=470.34, Z=2. The two oxygen atoms and the one nitrogen atom of the tridentate Schiff base ligand and the one oxime oxygen atom of the hydroxamate ligand coordinate to the vanadium atom, forming an equatorial plane, the two axial positions are respectively occupied by the oxygen atom of the oxovanadium and the carbonyl oxygen atom of the hydroxamate and the vanadium atom exhibits a distorted octahedral VO(ONO)(OO) coordination sphere. The 1H NMR spectrum suggests that the two isomers, endo and exo in a molar ratio of 1/1.7, coexist in the solution of the title complex in CDCl3. There exists a quasi-reversible one-electron redox reaction corresponding to VⅤ/VⅥ couple in the three non-aqueous solvents, and the redox potential E1/2 of the title complex substantially shifts in the direction of the positive voltage increase in the order: CH2Cl2<CH3CN<DMF.  相似文献   

2.
杨明星  林深  余萍  陈丽娟  刘世雄 《中国化学》2005,23(10):1407-1411
The two trinuclear nickel(Ⅱ) complexes, Ni3(C13H15N2O3)2(C5H5N)4 (1) and Ni3(C13H15N2O3)2(C5H5N)2- (C3H7NO)2 (2), were prepared by the reaction of Ni(OAc)2·4H2O with N-hexanoylsalicylhydrazide. The crystal structures of complexes were determined by X-ray diffraction analysis. Complex 1 takes triclinic symmetry with space group P-1 and cell dimensions of a=0.92377(2) nm, b= 1.08786(6) nm, c= 1.29391(3) nm, α=76.395(4)°, β=78.418(3)°, γ=67.378(4)°, V= 1.15772(7) nm^3, Z= 1,μ= 12.63 cm^-1. Complex 2 belongs to triclinic system and P2(1) space group and the crystallographic data: a= 1.4889(2) nm, b= 1.0389(1) nm, c= 1.4994(2) nm, β= 96.174(4)°, V=2.3058(5) nm^3, Z=2,μ= 12.70 cm^-1. The structures of the two molecules are similar. The three nickel atoms in each molecule of the two title complexes arrange in a strictly linear structure. The central nickel atom of the molecule adopts octahedral configuration, while the two nickel atoms on the two sides adopt square-planar configuration in each molecule. But the central nickel atoms of the two complexes have different axial ligands, which cause a slight difference in the bond distances of the octahedron. The antibacterial activity of compound 1 against seven common bacteria was investigated.  相似文献   

3.
A mixed-ligand metal-organic complex [Cd(C7H3N3O2)(C12H8N2)]n was synthesized by cadmium(Ⅱ) nitrate, 1,10-phenanthroline(phen) and benzotriazole-5-carboxylate acid(H2btca). Single crystal X-ray analysis indicates that complex 1 has a two-dimensional layer structure and crystallizes in an orthorhombic space group(Pbca), with cell parameters, a=1.7422(6) nm, b=0.9264(3) nm, c=2.0729(7) nm, α=90°, β=90°,γ=90°, V=3.346(2) nm^3, Z=8. Each central Cd(Ⅱ) is six-coordinated by four N atoms, two of which are from 1,10-phenanthroline, and the other two from two different triazole nitrogen atoms and two O atoms from benzotriazole-5-carboxylate, forming a distorted octahedral geometry. Adjacent Cd(Ⅱ) centers are bridged by benzotriazole-5-carboxylate molecules to form a one-dimensional chain, which is further connected by the nitrogen atoms of btca^2- to form an extended two-dimensional wave-like layer, with OFF(offset face-to-face) stacking interactions between phen ligands in adjacent layers, which are helpful to forming the three-dimensional supramolecular structure.  相似文献   

4.
A palladium(Ⅱ) complex, [PdLCl]2· [PdCl4], [L=4-bromo-2,6-bis(N,N-diethylaminomethylene)pyridine], was synthesized and its crystal structure was determined by X-ray analysis. The complex crystallizes in monoclinic system with space group Cc, a=0.845 1(17) nm, b=1.836 5(4) nm, c=2.715 8(5) nm,β=93.99(3)°, V=4.204 8(15) nm^3, Z=4, R,=0.037 7 and wR2=0.076 9. The coordination geometry of the Pd atom in the cation is a slightly distorted square planar, with one pyridyl N and two N atoms of the diethylamine ligand, together with one Cl atom. The dihedral angle between the square planar (N3PdCl) and the pyridyl ring is 10.3(4)°. CCDC: 623421.  相似文献   

5.
张少华  杨颖群  李薇  李昶红  匡云飞 《结构化学》2011,30(10):1497-1500
One dinuclear manganese(II)complex [Mn2(C12H8N2)4(C8H5O4)2](C8H4O4)·H2O has been synthesized with o-phthalic acid and 1,10-phenanthroline.The crystal structure was determined by X-ray diffraction.The crystal belongs to the triclinic system,space group P1 with a = 1.17767(3),b = 1.22292(2),c = 1.35860(3)nm,α = 110.5300(10),β = 97.6140(10),γ = 93.7300(10)o,V = 1.80307(7)nm3,Dc = 1.404 g/cm3,Z = 2,F(000)= 784,the final GOOF = 1.047,R = 0.0398 and wR = 0.1038.The crystal structure of the title complex consists of one [Mn2(C12H8N2)4(C8H5O4)2]2+ cation,one uncoordinate o-phthalate anion(C8H4O4)2-and one uncoordinate water molecule.In [Mn2(C12H8N2)4(C8H5O4)2]2+,the central Mn(II)ion is coordinated by four nitrogen atoms and two oxygen atoms to give a distorted octahedral coordination geometry.The electrochemical property of the title complex was also studied.  相似文献   

6.
A new one-dimensional polymeric complex [Cd(SCN)2(H2O)]L (L = N,N′-bis(furan- 2-ylmethylene)hydrazine) has been synthesized and characterized by IR, UV spectra, TG-DTA technique and single-crystal X-ray diffraction analysis. It crystallizes in triclinic, pace group P1^- with a = 5.9268(8), b = 10.8678(15), c = 13.3671(19) A, α = 109.295(2), β = 95.092(2), γ = 97.8580(10)°, V = 796.70(19)A^3, Z = 2, C12H10CdN4O3S2, Mr = 434.76, μ = 1.648 mm^-1, Dc = 1.812 g/cm^3, F(000) = 428, R = 0.0308 and wR = 0.0769. The crystal structure reveals that the structure of [Cd(SCN)2(H2O)]n features di-μ-1,3-thiocyante bridges and 1D chains. The octahedrally coordinated Cd atom is surrounded by one oxygen atom from water molecule, three S atoms and two N atoms from five di-μ-1,3 thiocyanato bridges. The Cd atoms are connected by two di-μ-1,3 thiocyanato bridges with the Cd(1)…Cd(1A) separation of 4.239(1) A and Cd(1)...Cd(1B) of 5.852(1)/~. In addition, the one-dimensional straight chain structure is further connected by multiform intermolecular N-H…O hydrogen bonds and π-π interactions to form a three-dimensional supramolecular structure.  相似文献   

7.
A new La(Ⅲ) complex, {[La(L)(NO3)(H2O)3]·H2O}n (L = 1,10-phenanthroline- 2,9-dicarboxylate), has been synthesized and structurally determined by X-ray diffraction analysis. The complex crystallizes in the monoclinic system, space group P21/c with a = 7.7358(17), b = 8.1664(18), c = 28.271(6) A, β= 95.184(4)°, V= 1778.6(7) A3, Z = 4, C14H14LaN3O11, Mr = 539.19, Dc = 2.014 g/cm^3, μ= 2.471 mm^-1, F(000) = 1056, the final R = 0.0350 and wR = 0.0659. In this complex, each metal center adopts a ten-coordination geometry formed by two N atoms from a ligand L and eight O atoms from three H2O molecules, a nitrate ion and carboxylates of two ligands. Each ligand adopts a N2,O3-pentdentate coordination mode using two N and two O atoms chelating a La(Ⅲ), and using another O atom of carboxylate to bridge another La(Ⅲ) center resulting in a 1D helical chain molecule. Intermolecular strong O-H…O and weak C-H…O hydrogen bonds extend the 1D chain structure into a 3D supramolecular architecture.  相似文献   

8.
ZHAO Xiao-Fan 《结构化学》2008,27(7):853-857
A novel end-to-end azido-bridged polynuclear Schiff-base copper(II) complex, [Cu(C12H15Br2N2O)(N3)]n, was prepared and characterized by elemental analysis, IR spectra, and single-crystal X-ray diffraction. The crystal belongs to the orthorhombic system, space group Pbcn with a = 24.588(5), b = 10.377(2), c = 13.022(3) A, V= 3322.6(12) A^3, Z = 8, Dc = 1.874 g/cm^3, Mr = 468.65, λ(MoKa) = 0.71073 A,μ = 6.130 mm^-1, F(000) = 1832, R = 0.0637 and wR = 0.1176. The Cu atom in the complex is five-coordinated in a square pyramidal geometry by three donor atoms of the Schiff-base ligand, and two N atoms from two bridging azide ligands. The [2,4-dibromo-6-[(3-dimethylaminopropylimino)methyl]phenolato]copper(II) units are linked by the bridging azide ligands, giving zigzag polymeric chains with backbones of the [--Cu-N-N-N--Cu]n type running along the b axis.  相似文献   

9.
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   

10.
The title complex [CoL(H20)3]2·H2O (C26H46N4O21S4CO2), where L = taurine-5- methyl-2-hydroxyisophthalaldehydes, has been synthesized and characterized by IR and X-ray diffraction analysis. The crystal of the complex belongs to the triclinic system, space group P1, with a = 11.197(4), b = 13.309(5), c = 14.486(5) ]A, a = 78.827(13),β = 70.547(11), γ = 81.058(13)°, Mr = 996.77, S = 1.08, V= 1987.2(13) A3, Z = 2, Dc = 1.666 g/cm3, F(000) = 1032,μ = 1.131 mm^-1, R = 0.0633 and wR = 0.1293. According to the structural analysis, the Co( Ⅱ ) ion adopts a slightly distorted six-coordinated octahedral geometry. One N atom of the Schiff base of each molecule was hydrogenated to form hydrogen bond with O atom. Two coterminous molecules packed in one crystal water molecule are linked by intermolecular hydrogen bonds, thus generating an infinite chain constructed by hydrogen bonds.  相似文献   

11.
A new compound, semicarbazidium 3,5-dihydroxy-2,4,6-trinitrophenolate hemihydrate (SCDHTNP·0.5H2P), was synthesized by the reaction of the aqueous solutions of semicarbazide with trinitrophloroglucinol. Its structure was determined by single-crystal X-ray diffraction analysis and characterized by elemental analysis, FTIR, DSC and TG-DTG techniques. The crystal is monoclinic with space group P21/n and the empirical formula C7H9N6O10.50. The unit cell parameters are: a= 1.3791(3) nm, b=0.9256(2) nm, c=2.0468(4) nm,β= 106.93(3)°, V=2.4995(9)nm^3, Z=8, Dc= 1.835 g/cm^3, Mr=345.20, F(000)= 1416, s=0.945,μ(Mo Ka)=0.174 mm^-1. The final R and wR are 0.0401 and 0.0896. Its structure consists of two semicarbazidium cations, two 3,5-dihydroxy-2,4,6-trinitrophenolate anions and one crystal water molecule, which are interconnected by electrostatic forces and hydrogen bonds into layer structure, making the title compound very stable. Under a linear heating rate, the thermal decomposition processes of SCDHTNP·0.5H2O have one endothermal dehydration stage and two intensive exothermic decomposition stages at 178-241℃ to evolve abundant gas products.  相似文献   

12.
Two new mononuclear coordination compounds, bis{4‐[(hydroxyimino)methyl]pyridinium} diaquabis(pyridine‐2,5‐dicarboxylato‐κ2N,O2)zincate(II), (C6H7N2O)2[Zn(C7H3NO4)2(H2O)2], (1), and (pyridine‐2,6‐dicarboxylato‐κ3O2,N,O6)bis[N‐(pyridin‐4‐ylmethylidene‐κN)hydroxylamine]zinc(II), [Zn(C7H3NO4)(C6H6N2O)2], (2), have been synthesized and characterized by single‐crystal X‐ray diffractometry. The centrosymmetric ZnII cation in (1) is octahedrally coordinated by two chelating pyridine‐2,5‐dicarboxylate ligands and by two water molecules in a distorted octahedral geometry. In (2), the ZnII cation is coordinated by a tridentate pyridine‐2,6‐dicarboxylate dianion and by two N‐(pyridin‐4‐ylmethylidene)hydroxylamine molecules in a distorted C2‐symmetric trigonal bipyramidal coordination geometry.  相似文献   

13.
The title complexes [M(sac)2(mpy)2] [sac is saccharinate (C7H4NO3S) and mpy is 2‐pyridyl­methanol (C6H7NO)], with M = ZnII and CdII, are isostructural and consist of neutral mol­ecules. The ZnII or CdII cations are octahedrally coordinated by the two neutral mpy and two anionic sac ligands. The mpy ligand acts as a bidentate donor through the amine N and hydroxyl O atoms. The sac ligands exhibit an ambidentate coordination behaviour; one is N‐coordinated and the other is O‐coordinated within the same coordination octahedron. The crystal packing is determined by C—H?O‐type hydrogen bonding, as well as by weak py–py and sac–sac aromatic π–π‐stacking interactions.  相似文献   

14.
The two title mononuclear compounds are four‐coordinate bis[N‐(5‐oxo‐4,4‐diphenyl‐4,5‐dihydro‐1H‐imidazolidin‐2‐ylidene)glycinato]copper(II) dimethylformamide disolvate, [Cu(C17H14N3O3)2]·2C3H7NO, (I), and five‐coordinate aquabis[N‐(5‐oxo‐4,4‐diphenyl‐4,5‐dihydro‐1H‐imidazolidin‐2‐ylidene)glycinato]copper(II) dimethylformamide disolvate, [Cu(C17H14N3O3)2(H2O)]·2C3H7NO, (II). In (I), the CuII ion lies on an inversion centre with one‐half of the complex molecule in the asymmetric unit, while in (II) there are two independent ligand molecules in the asymmetric unit, with the CuII ion and coordinated water molecule located on a general position. In both crystal structures, the complex molecules assemble in ribbons via N—H...O hydrogen‐bond networks.  相似文献   

15.
The binuclear praseodymium(III) complex with N‐(1‐carboxyethylidene)‐salicylhydrazide (C10H10N2O4, H2L) was prepared in H2O‐C2H5OH mixed solution, and the crystal structure of [Pr2L2(HL)2(H2O)4]·3H2O·C6H6 was determined by X‐ray single crystal diffraction. The crystal complex crystallizes in the triclinic system with space group P‐1, and in the structure each Pr atom is 9‐coordinated by carboxyl O and acyl O and azomethine N atoms of two tridentate ligands to form two stable five‐membered rings sharing one side in keto‐mode and two water molecules. The coordination polyhedron around Pr3+ was described as a monocapped square antiprism geometry. In an individual molecule, four tridentate ligands were coordinated by two negative univalent (HL) and two bivalent forms (L) respectively. Two negative univalent ligands were coordinated via μ2‐bridging mode.  相似文献   

16.
The crystal structures of two complexes containing the peroxodisulfate anion are reported, namely μ‐peroxodisulf­ato‐1κO:2κO′‐bis­[(acetato‐κ2O,O′)aqua­(2,2′:6′,2′′‐terpyridine‐κ3N,N′,N′′)cadmium(II)] hepta­hydrate, [Cd2(C2H3O2)2(S2O8)(C15H11N2)2(H2O)2]·7H2O, (I), and catena‐poly[[[bis(2,2′‐bipy­ridine‐κ2N,N′)mercury(II)]‐μ‐peroxodisulfato‐κ2O:O′] 0.4‐hy­drate], {[Hg(C10H8N2)2(S2O8)]·0.4H2O}n, (II). In both structures, the anion behaves as a bridge, linking neighbouring coordination polyhedra in two different ways, either tightly bound to the hepta­coordinated Cd2+ cation forming neatly separated dimeric entities in (I) or across a shorter O—S—O path producing weakly connected chains by way of `semi­coordination' to the Hg2+ cations in (II).  相似文献   

17.
In coordination chemistry and crystal engineering, many factors influence the construction of coordination polymers and the final frameworks depend greatly on the organic ligands used. The diverse coordination modes of N‐donor ligands have been employed to assemble metal–organic frameworks. Carboxylic acid ligands can deprotonate completely or partially when bonding to metal ions and can also act as donors or acceptors of hydrogen bonds; they are thus good candidates for the construction of supramolecular architectures. We synthesized under reflux or hydrothermal conditions two new alkaline earth(II) complexes, namely poly[(1,10‐phenanthroline‐κ2N,N′)bis(μ‐3‐phenylprop‐2‐enoato‐κ3O,O′:O)calcium(II)], [Ca(C10H7O2)2(C10H8N2)]n, (1), and poly[(1,10‐phenanthroline‐κ2N,N′)(μ3‐3‐phenylprop‐2‐enoato‐κ4O:O,O′:O′)(μ‐3‐phenylprop‐2‐enoato‐κ3O,O′:O)barium(II)], [Ba(C10H7O2)2(C10H8N2)]n, (2), and characterized them by FT–IR and UV–Vis spectroscopies, thermogravimetric analysis (TGA) and single‐crystal X‐ray diffraction analysis, as well as by powder X‐ray diffraction (PXRD) analysis. Complex (1) features a chain topology of type 2,4 C4, where the Ca atoms are connected by O and N atoms, forming a distorted bicapped trigonal prismatic geometry. Complex (2) displays chains of topology type 2,3,5 C4, where the Ba atom is nine‐coordinated by seven O atoms of bridging/chelating carboxylate groups from two cinnamate ligands and by two N atoms from one phenanthroline ligand, forming a distorted tricapped prismatic arrangement. Weak C—H…O hydrogen bonds and π–π stacking interactions between phenanthroline ligands are responsible to the formation of a supramolecular three‐dimensional network. The thermal decompositions of (1) and (2) in the temperature range 297–1173 K revealed that they both decompose in three steps and transform to the corresponding metal oxide.  相似文献   

18.
Reaction of the flexible phenolic carboxylate ligand 2‐(3,5‐dicarboxylbenzyloxy)benzoic acid (H3L) with nickel salts in the presence of 1,2‐bis(pyridin‐4‐yl)ethylene (bpe) leads to the generation of a mixture of the two complexes under solvolthermal conditions, namely poly[[aqua[μ‐1,2‐bis(pyridin‐4‐yl)ethylene‐κ2N:N′]{μ‐5‐[(2‐carboxyphenoxy)methyl]benzene‐1,3‐dicarboxylato‐κ3O1,O1′:O3}nickel(II)] dimethylformamide hemisolvate monohydrate], {[Ni(C16H10O7)(C12H10N2)(H2O)]·0.5C3H7NO·H2O}n or {[Ni(HL)(bpe)(H2O)]·0.5DMF·H2O}n, 1 , and poly[[diaquatris[μ‐1,2‐bis(pyridin‐4‐yl)ethylene‐κ2N:N′]bis{μ‐5‐[(2‐carboxyphenoxy)methyl]benzene‐1,3‐dicarboxylato‐κ2O1:O5}nickel(II)] dimethylformamide disolvate hexahydrate], {[Ni2(C16H10O7)2(C12H10N2)3(H2O)2]·2C3H7NO·6H2O}n or {[Ni2(HL)2(bpe)3(H2O)2]·2DMF·6H2O}n, 2 . In complex 1 , the NiII centres are connected by the carboxylate and bpe ligands to form two‐dimensional (2D) 4‐connected (4,4) layers, which are extended into a 2D+2D→3D (3D is three‐dimensional) supramolecular framework. In complex 2 , bpe ligands connect to NiII centres to form 2D layers with Ni6(bpe)6 metallmacrocycles. Interestingly, 2D+2D→3D inclined polycatenation was observed between these layers. The final 5‐connected 3D self‐penetrating structure was generated through further connection of Ni–carboxylate chains with these inclined motifs. Both complexes were fully characterized by single‐crystal analysis, powder X‐ray diffraction analysis, FT–IR spectra, elemental analyses, thermal analysis and UV–Vis spectra. Notably, an interesting metal/ligand‐induced crystal‐to‐crystal transformation was observed between the two complexes.  相似文献   

19.
The CoII cation in poly[[aqua(μ‐benzene‐1,2‐dicarboxylato‐κ3O1,O2:O1)(μ‐4,4′‐bipyridine‐κ2N:N′)cobalt(II)] trihydrate], {[Co(C8H4O4)(C10H8N2)(H2O)]·3H2O}n, is octahedrally coordinated by two N atoms of two 4,4′‐bipyridine ligands, three O atoms from phthalate anions and a fourth O atom from a coordinated water molecule. The packing consists of planes of coordination polymers linked by hydrogen bonds mediated by three solvent water molecules; the linkage is achieved by the water molecules forming intricate oligomeric clusters which also involve the O atoms of the phthalate ligands.  相似文献   

20.
在水乙醇混合溶剂中,首次得到了2-羰基丙酸水杨酰腙、1,10-菲啰啉与硝酸钆形成的配合物[Gd(C10H9N2O4)(C10H8N2O4)(H2O)3]2·phen·4H2O,并测试了其单晶结构。该配合物属三斜晶系,空间群为P-1。每个配合物分子中有两个九配位的钆的结构单元,每个钆离子与两个三齿配体2-羰基丙酸水杨酰腙(分别以负一价和负二价形式)和三个水分子配位。每个钆单元在空间呈扭曲的单帽四方反棱柱。同时还有一个游离的1,10-菲啰啉存在于晶格中,通过氢键与配位水作用。生物活性试验表明该配合物对三种病原菌有一定的抑菌活性。  相似文献   

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