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1.
刘诚  刘起辉  葛树保  吴刚 《结构化学》2014,33(5):713-720
The self-assembly of 1,10-phenanthroline(phen) and 1,3-benzenedicarboxylic acid(H2bdc) with Pb(NO3)2 under solvothermal conditions in N,N-dimethylacetamide(DMA) gives rise to a one-dimensional chain coordination polymer, [Pb(phen)(bdc)](1), which was characterized by elemental analysis, FT-IR and single-crystal X-ray diffraction. This complex crystallizes in triclinic, space group P1 with a = 7.5595(6), b = 9.8199(8), c = 13.1663(11) , α = 69.7590(10), β = 80.6000(10), γ = 71.3180(10)o, Z = 2, C20H12N2O4Pb, Mr = 551.51, Dc = 2.112 g/cm3, F(000) = 520 and μ = 9.757 mm-1. The final R = 0.0304 and wR = 0.0763 for 3427 observed reflections with I 2σ(I) and R = 0.0365 and wR = 0.0894 for all data. The structure contains one crystallographic unique Pb(Ⅱ) atom, one phen molecule chelating with a Pb(Ⅱ) atom, and one bdc2- anion, acting as a bidentate bridging ligand linking the Pb(Ⅱ) atoms to form a one-dimensional structure. The two-dimensional layer and three-dimensional stacking structures are formed by C–H···O hydrogen bonding interactions. The thermal stable and fluorescent properties of 1 were investigated. PbO micro-crystal particles are produced by calcination of powder sample of complex 1. The obtained PbO is characterized and observed by XRD and SEM analyses.  相似文献   

2.
Two new zinc(Ⅱ) compounds with dibenzoylmethane and N-donor ancillary ligands,[Zn(μ-pyz)(dbm)_2]_n(1) and [Zn(dbm)_2(μ-bpe)Zn(dbm)_2](2)(Hdbm = dibenzoylmethane,pyz = pyrazine and bpe = 1,2-bis(4-pyridyl)ethane),have been prepared and characterized using elemental analysis,IR,~1H NMR and 13 C NMR spectroscopy,and studied by thermal gravimetric analysis as well as single-crystal X-ray diffraction. The crystal and molecular structures of 1 and 2 have been solved by X-ray diffraction and they turned out to be a one-dimensional coordination polymer with linear dispositions of metal atoms and binuclear compound,respectively. These one-dimensional polymers are further connected to form a 3D supramolecular network by C–H···O(only in 2) and π-π interactions.  相似文献   

3.
A novel mixed-ligand coordination polymer [Pb(phen)(NNDS)(H2O)]n·n H2O(1) was obtained from the reaction of 1,10-phenanthroine(phen), Pb(OAc)2 and sodium 1-nitroso-2-naphthol-3,6-disulfonate(Na2NNDS) in a mixed solvent. The complex was characterized by elemental analysis, IR and X-ray single-crystal diffraction. Crystal data for 1: monoclinic, space group P21/c, a = 11.5835(9), b = 14.6334(11), c = 13.9030(11) ?, β = 98.4180(10)o, V = 2331.3(3) ?3, Z = 4, Mr = 754.70, Dc = 2.150 mg/m3, μ = 7.483 mm-1, F(000) = 1456, the final R = 0.0430 and w R = 0.0841 for 4221 observed reflections with I 2σ(I). The Pb(II) center is coordinated by six O and two N atoms showing a distorted dodecahedron configuration. The multidentate ligand of NNDS dianion exhibits peculiar coordination mode, and the two O atoms of two sulfonate anions bridge two Pb(II) cations into a dimer, and the O atom of nitroso group links the other dimer into 2D sheets extending in the [011] plane. There exist significant π-π stacking interactions between adjacent phen and NNDS. The 3D network is formed by 2D sheets interlinked by hydrogen bonds and π-π stacking interactions. The thermostability of 1 was investigated by TG and DSC.  相似文献   

4.
赵华绒  王玲 《结构化学》2014,(2):284-288
The compound N-(phenethylcarbamothioyl)cyclopent-1-enecarboxamide was synthesized by the reaction of cyclopent-1-enecarbonyl isothiocyanate with phenethylamine in acetone, and its structure was characterized by IR, 1H NMR and X-ray crystal structure determination. The crystal of the title compound belongs to triclinic, space group P1 with a = 6.9500(7), b = 9.4618(9), c = 11.3256(11), α = 71.522(9), β = 81.830(8), γ = 89.237(8)o, Z = 2, V = 698.80(12)3, Dc = 1.304 g/cm3, μ = 0.225 mm-1, F(000) = 292, R = 0.0413 and wR = 0.1073 for 1996 observed reflections with I 2σ(I). Intramolecular N(2)–H(2)···O(1) interactions as well as intermolecular N(2)–H(2)···O(1), N(1)–H(1)···S(1) and C(12)–H(12)···S(1) hydrogen bonds help to stabilize the crystal structure. X-ray diffraction analysis reveals that the structure of the new compound exhibits a one-dimensional infinite chain-like structure. The cytotoxicity of the compound was investigated by MTT assay. The results show that the compound is toxic to A549 tumor cell.  相似文献   

5.
The title complex,(μ-pdt)Fe_2(CO)_5(Ph_2PCH_3)(pdt = SCH_2CH_2CH_2S),was obtained by the reaction of the parent complex(μ-pdt)Fe_2(CO)_6 with Ph_2PCH_3 and Me_3NO·2H_2O in good yield(90%). The title complex was characterized by IR,~1H NMR,~(31)P{~1H} NMR and ~(13)C{~1H} NMR spectroscopy as well as by single-crystal X-ray diffraction analysis. The molecular structure shows that the title complex contains a butterfly diiron propanedithiolate cluster with five terminal carbonyls and a monophosphine ligand Ph_2PCH_3. The crystal packing diagram reveals that intermolecular C H···O hydrogen bonds between CH_2 and carbonyls,π-π stacking interactions and van der Waals' interactions stabilize the solid state to form a three-dimensional network.  相似文献   

6.
苏清  赵天琦  张杰  李佩  赵晴  叶玲 《结构化学》2014,(2):237-243
6,8-Di-tert-butyl-3-(2,4-dimethyl-quinolin-7-yl)-3,4-dihydro-2H-benzo[e][1,3]oxa- zine(1) was obtained by one-pot reaction starting from 2,4-di-tert-butylphenol, 7-amino-2,4- dimethyl-quinoline and paraformaldehyde. The compound was structurally characterized by NMR, IR and single-crystal X-ray diffraction along with the elemental analysis. Compound 1 crystallizes as solvate with chloroform. The solvate 1·CHCl3(C28 H35 Cl3 N2 O, Mr = 521.93) belongs to the triclinic system, space group P1 with a = 10.852(2), b = 11.352(2), c = 13.050(3), α = 101.95(3), β = 92.94(3), γ = 114.64(3)o, V = 1412.4(5)3, Z = 2, Dc = 1.227 g/cm3, F(000) = 552, μ = 0.347 mm–1, R = 0.0959 and wR = 0.2725(I 2?(I)). The chloroform molecule displays a rotational disorder as one chloro atom can be located at two different positions. The packing of 1·CHCl3 was further stabilized by intramolecular C–H···O interactions, intermolecular C–H···N interactions, C–H···π interactions, and π···π interactions. The luminescent properties of compound 1 in both methylene chloride solution and the solid state were studied.  相似文献   

7.
A new Pb(Ⅱ) coordination polymer, [Pb(1,4-chdc)(L)]_n·nH_2O(1), was synthesized under hydrothermal condition(1,4-H2 chdc = 1,4-cyclohexanedicarboxylic acid and L = 2-(3-fluorophenyl)-1H-imidazo[4,5-f][1,10]phenanthroline). Its crystal structure was determined by singlecrystal X-ray diffraction. Compound 1 crystallizes in triclinic, space group P1 with a = 9.1182(8), b = 11.3249(10), c = 12.7326(12) ?, α = 77.897(2), β = 81.644(2), γ = 84.491(2)°, V = 1269.0(2) ?~3, Z = 2, C_(27)H_(24)FN_4O_5Pb, M_r = 710.69, D_c = 1.860 g/cm~3, F(000) = 690, μ(MoKa) = 6.701 mm~(-1), R = 0.0349 and wR = 0.0746. In 1, each 1,4-chdc anion bridges two neighboring Pb(Ⅱ) atoms in a bidentate chelating coordination mode to give a chain structure. The L ligands are attached on one side of the chain through chelating the Pb(Ⅱ) atoms, and are stacked with those of an adjacent chain through π-π interactions, yielding a layer structure. The O–H···O and N–H···O hydrogen bonding interactions further stabilize the supramolecular layer structure of 1. Moreover, solid state luminescent property of 1 was also studied.  相似文献   

8.
Two coordination polymers, namely [Pb(Hbtc)(phen)]n(1) and {[Cd3(btc)2(H2O)4]·2H2O}n(2, H3btc = biphenyl-2,5,3'-tricarboxylic acid, phen = 1,10-phenanthroline), were assembled. Single-crystal X-ray diffraction studies show that compound 1 possesses a zigzag chain 1D coordination network, which is further extended into a 3D supramolecular architecture via O–H···O hydrogen bonds and π-π packing interactions. Compound 2 features a 3D open framework based on a tricadmium(II) subunit, generating a trinodal 4,4,6-connected net with the 4,4,6T24 topology defined by the point symbol of(44·62)3(46·69)2. Thermal stability and luminescent properties of both compounds were studied and discussed.  相似文献   

9.
A homochiral complex, Zn3(Hsalen)2(Py)4(H2O)2 (salen = (1R,2R)-(-)-diamino-cyclohexane-N,N'-biscarboxyl-salicylidene) 1, has been synthesized by solvothermal procedure and characterized by IR, microanalysis, TGA, powder and single-crystal X-ray crystallography. It crystallizes in monoclinic space group P2 with a = 10.9439(7), b = 10.1722(6), c = 27.3450(17), β = 97.5060(10)o, V = 3018.1(3) 3, Z = 2, Zn3(Hsalen)2(Py)4(H2O)2, Mr = 1363.33, Dc = 1.500 g/cm3, F(000) = 1408, μ = 1.257 mm-1, GOOF = 1.042, the final R = 0.0601 and wR = 0.1464 for 10322 observed reflections with I 2σ(I). The coordination polymer 1 possesses a 1D infinite zigzag chain architecture constructed by strong hydrogen bonding interactions and the polymeric chains are further assembled into a 2D supramolecular network structure via C-H···π interactions between the cyclohexane and aromatic rings of the ligand of adjacent chains. Simultaneously, π···π stacking interactions play an important role in forming the 2D supramolecular framework.  相似文献   

10.
Two new complexes, [Cu(DMB)2(NAA)2](1) and [Co(DMB)2(NAA)2](2)(DMB = 5,6-dimethylbenzimidazole, HNNA = 1-naphthylacetic acid), were hydrothermally synthesized and characterized by elemental analysis, IR spectroscopy, TGA, PXRD and single-crystal X-ray diffraction analysis. The coordination geometry of the metal centers is a perfect square plane for 1 and a distorted tetrahedron for 2. In compound 1, the mononuclear units are linked by N–H···O hydrogen bonds to form a 1D chain structure, while mononuclear motifs of 2 are extended via N–H···O hydrogen bonding and π-π stacking interactions into a 2D supramolecular layer. The remarkable catalytic properties of the two complexes for the degradation of Congo red dye have been found.  相似文献   

11.
Studies on the synthesis and design of coordination polymers(CPs) with flexible ligands are of great interest owing to their dynamic structures and promising applications. The title coordination polymers, {[Cd·(HTTTA)·(phen)]·2H_2 O}n(1) and [Cd·(HTTTA)·(phen)]n(2)(H3 TTTA = 2,2',2'-[1,3,5-triazine-2,4,6-triyltris(thio)] tris-acetic acid, phen = 1,10-phenanthroline) have been synthesized and characterized by elemental analysis, IR, powder XRD and single-crystal X-ray diffraction. Complex 1 consists of one CdII ion, one HTTTA2-ligand and one phen co-ligand. The Cd(Ⅱ) metal clusters were bridged by the tridentate HTTTA2-ligands into infinite 1D chains, which are further connected into the 3D architecture by abundant hydrogen bonds. In 2, three carboxyl groups of HTTTA2-ligand show different coordination directions because of the C–S–C flexible bond angle, which leads to different 1D chains of 2. The strong π-π stacking interaction and four C–H···O hydrogen bonds connect the 1D chains into a 3D framework. The solid-state photoluminescence and catalytic properties were studied as well.  相似文献   

12.
The coordination polymer[Zn_(1.5)(2,2?,4??-tpt)(tpa)_2]_n(2,2?,4??-tpt=3,4-bis(2-pyridyl)-5-(4-pyridyl)-1,2,4-triazole,H_2tpa=terephthalic acid)has been obtained by solution evaporation method and characterized by elemental analysis,IR,TG and single-crystal X-ray diffraction.The title compound crystallizes in the triclinic system,space group P1,with a=10.331(3),b=10.596(1),c=14.966(3)?,β=99.029(0)o,V=1448.86(6)?~3,Z=2,D_c=1.668g/cm~3,μ=1.320 mm~(-1),F(000)=740,R=0.0359 and w R=0.0841 with I2σ(I)).In this polymer,the asymmetric unit contains two crystallographically independent Zn(II)ions in different coordination environments.Zn(1)ion is five-coordinated,forming a distorted tetragonal pyramidal geometry,while the Zn(2)ion is six-coordinated to get a distorted octahedral geometry.Each Zn(II)ion is linked by 2,2?,4??-tpt and H_2tpa ligands,forming an infinite 2D structure.The existence of O(8)–H(8)···O(2)hydrogen bonding interactions leads the 2D chains to generate a 3D structure.In addition,1 shows strong photoluminescent emissions in the solid state at room temperature,so it can be used as potential optical materials.  相似文献   

13.
An unsymmetrical macrocyclic dinuclear Zn(II) complex, [Zn2(H0.5L)(OAc)](ClO4)1.5(1, H2 L is the condensation product between 2, 6-diformyl-4-methylphenol and diethylenetriamine), was obtained and characterized by IR spectrum, elemental analysis and X-ray single-crystal diffraction. The complex crystallizes in monoclinic, space group P21/c with a = 16.784(2), b = 19.474(3), c = 10.3364(13), β = 92.923(2)°, V = 3374.1(7) 3, Z = 4, Dc = 1.672 g/cm3, F(000) = 1740, μ = 1.651 mm-1, the R = 0.0609 and wR = 0.1696 for 4745 observed reflections(I 2σ(I)). The interactions of the complex with DNA have been measured by electrochemical studies, UV spectroscopy and viscosity experiment. The interactions of the complex with calf thymus DNA were studied by UV-vis spectra and the binding constant is 1.58 × 104 mol·L-1. The phosphate hydrolysis catalyzed by the complex was investigated using 4-nitrophenyl phosphate(NPP) as the substrate; the observed first order rate constant value is 3.0 × 10–4 s-1.  相似文献   

14.
Two new coordination polymers {[Zn(Hbtc)(bpyb)]·H_2O}n(1) and {[Cd(Hbtc)-(bpyb)_(1.5)]·0.5 bpyb}_n(2)(H_3btc = 1,3,5-benzenetricarboxylic acid, bpyb = 1,4-bis(4-pyridyl)benzene) have been synthesized under hydrothermal conditions. The two compounds were characterized by elemental analysis, IR spectroscopy, and X-ray single-crystal diffraction. Compound 1 displays a 2-fold interpenetrating 3D supramolecular architecture through O–H···N/O hydrogen bonds and π-π stacking interactions. Compound 2 exhibits a 2D→3D polycatenated structure, which is further stabilized by O–H···N hydrogen bonds. The results indicate that the metal ion has significant effects on the formation and structure of the resulted coordination polymers. Furthermore, thermal stability and photoluminescent properties of 1 and 2 are also discussed in detail.  相似文献   

15.
李静  王玉红  宋瑞峰 《结构化学》2014,33(10):1488-1494
A novel two-dimensional lead(II) coordination polymer 1, [C11H7Cl2NO3Pb]n, has been prepared by solvothermal reaction of new bridging ligand(5-chloro-quinolin-8-yloxy)acetic acid(HL) with PbCl2, and its structure was characterized by IR, elemental analysis, TG-DTA and single-crystal X-ray diffraction analysis. The crystal is of monoclinic system, space group P21/c with a = 16.7603(7), b = 8.6907(4), c = 8.4745(3), β = 101.1110(11)°, C11H7Cl2NO3 Pb, Mr = 479.27, V = 1211.25(9)3, Z = 4, Dc = 2.628 g/cm3, F(000) = 880, μ = 14.367 mm-1, R = 0.0173 and wR = 0.0508. The asymmetric unit contains one lead(II) cation, one(5-chloro-quinolin-8-yloxy)acetate(L) ligand and a chloride ion. The PbII center is hepta-coordinated in a distorted pentagonal bipyramidal geometry. The coordination sphere of the Pb atom is completed by two oxygen atoms and one nitrogen atom of the same L ligand, two bridging chloride ions and two bridging oxygen atoms of two adjacent L ligands. Two PbII centers are linked by the two L ligands to form a C2-symmetric dimer unit with a planar [Pb2O2] ring. Each dimer unit acts as a secondary building unit(SBU) and links adjacent four dimer units by the chloride atoms and oxygen atoms of carboxylate groups of L, forming a two-dimensional array. Such two-dimensional layers are packed through intermolecular C–H···Cl hydrogen bonds into a three-dimensional supramolecular structure. When the dimer unit is viewed as a 4-connected node, 1 is simplified as a 4-nodal 2-D network with square lattices of the diagonal lengths to be 6.079(1). The fluorescence emission peak of complex 1 appears near 407 nm.  相似文献   

16.
Although the numbers of co-crystals,salts,polymorphs,hydrates,and solvates are growing steadily,trimers that contain both inorganic and organic acids are still very rare in the Cambridge Structural Database(CSD).When 3,5-dihydroxybenzoic acid was crystallized readily with 6-methyl-1,3,5-triazine-2,4-diamine in a 4:3 ratio of ethanol and water by adding a few drops of nitric acid upon slow evaporation in ambient conditions,6-methyl-1,3,5-triazine-2,4-diamine and 3,5-dihydroxybenzoic acid with the nitric acid form of 1:1:1 an inorganic-organic salt formulated as[(C4H8N5+)·(NO3-)·(C7H6O4)].The supramolecular architecture,which is quite elegant and simple,appeared as stacking of a 3D network in adduct.Proton transfer from the HNO3to 6-methyl-1,3,5-triazine-2,4-diamine N acceptor(triazine N)occurred in the organic salt and led to the ionic heterosynthon in the structure.Cooperation among the–COOH,–OH,NO3–,and–NH–functional groups for the observed hydrogen bond synthon was examined in the structure.In adduct,recognition among the constituents is established through N–H···O,O–H···N,and O–H···O hydrogen bonds.The agomelatine molecules are linked through the intermolecular hydrogen bonding interactions(O–H···O)to form a 1D chain.In addition,the nitric acid anions and base cations act as donors and acceptors of hydrogen bonds and interlink,almost to co-planarity,the hydrogen-bonded chains through interchain N–H···O,O–H···N,as well as O–H···O interactions into a 2D sheet structure.Persistent N–H···O interactions were found to play an important role in the formation of the final 3D array.The salt was characterized by elemental analysis,IR,thermogravimetric analysis,and singlecrystal X-ray diffraction,to better understand how intermolecular interactions influence its supramolecular assembly.  相似文献   

17.
Reaction of a tripodal ligand, N,N?,N??-tris(3-pyridinyl) phosphoric trimide(TPPA) and CuBr_2·2H_2O result in the assembly of a new polymeric copper coordination polymer, which was characterized by single-crystal diffraction, infrared spectroscopy and elemental analysis. The polymer crystallizes in the triclinic system, space group P1 with a = 9.0964(5), b = 10.2592, c = 10.5822(8) ?, V = 933.01(9) ?~3, Z = 2, C_(30)H_(24)Br_4Cu_3N_(12)O_2P_2, M_r = 985.02, D_c = 1.753 g/cm~3, F(000) = 4072 and μ(MoKα) = 0.746 mm~(-1). The final R and w R are 0.0588 and 0.1329 for 4260 observed reflections with I 2σ(I). Cu(Ⅰ) is tetrahedrally coordinated and Cu(Ⅱ) center adopts square planar coordination geometry. Because of the flexibility of the TPPA ligands, the pyridyl rings rotate though a certain angle and three pyridyl rings on the same TPPA rotate by about 45° with respect to the central P=O groups. TPPA ligand acts as a tridentate ligand and is coordinated with three metal centers with its pyridyl donors to form a 2D-sheet like structure, and it is further connected by N–H···O and N–H···Br, resulting in a 3D network packing. Oxidation states of the metal center have been determined by bond valence sum calculation.  相似文献   

18.
Reaction of 3,5-pyridine-dicarboxylic acid(3,5-PydcH2) with iron salt in hydrothermal condition results in the formation of a three-dimensional self-assembly network formulated as [C14H14Fe2N2O12]n,and it has been structurally characterized by elemental analysis,IR spectra and X-ray diffraction.It crystallizes in the monoclinic system,space group C2/c with a=9.9633(15),b=12.0942(18),c=7.4297(11) and β=105.822o.The units of Fe2(pydc)2·2H2O are linked into a one-dimensional structure via the chelate carboxylate groups from the 3,5-pyridine-dicarboxylate.The interlayer hydrogen bonding interactions result in a three-dimensional supramolecular architecture.In the complex,the Fe(Ⅲ) ion displays a slightly distorted pentagonal bipyramidal geometry with seven coordination numbers.Cyclic-voltammetry measurement reveals the oxidation and reduction processes for the complex are quasi-reversible in nature.  相似文献   

19.
Two novel clusters [Mn~Ⅲ_3(μ_3-O)(phendox)3]X·13H_2O(X = Cl(1), Br(2]) have been obtained from the solvothermal reactions of 1,10-phenanthroline-2,9-dicarbaldehyde dioxime(H_2phendox) with MnCl_2·4H_2O or anhydrous MnBr_2, and their structures were characterized by elemental analysis, FT-IR, XRD, TGA, MS and single-crystal X-ray diffraction. It crystallizes in trigonal, space group P3_1/c. X-ray analysis reveals that the neighbouring [Mn_3(μ_3-O)(phendox)_3]+ cores are linked by C–H···Cl hydrogen bonds and form an infinite supramolecular chain along the c-axis. Neighbouring chains are packed with each other by off-set p-p interactions of the aromatic rings on phenox2-. A 3D supramolecular architecture in a honeycomb topology is formed with 1D hexagonal channel in the dimensions of 13? × 13? along the c-axis. The gas adsorption studies show that compound 1·13H_2O is stable upon the removal of guest molecules and the desolvated compound absorbed considerable amount of CO_2.  相似文献   

20.
Three new Zn(Ⅱ)/Cd(Ⅱ) coordination polymers based on 2-mercaptonicotinic acid (H2mna) with 1,2-di(4-pyridyl)ethylene (dpe) introduced as a bridging ligand have been synthesized via hydrothermal method and structurally characterized by single-crystal X-ray diffraction as well as elemental analysis and IR. As reported in this paper, [Zn2(dpe)0.5(mna)2] (1) can be classified as a two-dimensional layer structure in which the 1D chain composed of Zn(Ⅱ) and mna ligands is bridged by dpe ligands, while the complex named [Zn4(dpe)4(mna)4] (2) is a tetra-nuclear cluster compound. These two compounds are further extended to three-dimensional structures by hydrogen bonds along with C-H…π and π…π interactions. Compound 3 with general formular [Cd2(dpe)0.5(mna)2]·H2O belongs to a three-dimensional porous structure in which the 2D metal layers formed by the coordination of Cd(Ⅱ) and mna ligands are connected with the bridging of dpe ligands.  相似文献   

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