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1.
Four new coordination complexes with azole heterocycle ligands bearing acetic acid groups, [Co(L1)2]n (1), [CuL1N3]n (2), [Cu(L2)2·0.5C2H5OH·H2O]n (3) and [Co(L2)2]n (4) (here, HL1=1H-imidazole-1-yl-acetic acid, HL2=1H-benzimidazole-1-yl-acetic acid) have been synthesized and structurally characterized. Single-crystal structure analysis shows that 3 and 4 are 2D complexes with 44-sql topologies, while another 2D complex 1 has a (43)2(46)-kgd topology. And 2 is a 3D complex composed dinuclear μ1,1-bridging azido CuII entities with distorted rutile topology. The magnetic properties of 1 and 2 have been studied.  相似文献   

2.
In this article, ten new coordination frameworks, namely, [Ni(H2O)6]·(L3) (1), [Zn(L3)(H2O)3] (2), [Cd(L3)(H2O)3]·5.25H2O (3), [Ag(L1)(H2O)]·0.5(L3) (4), [Ni(L3)(L1)] (5), [Zn(L3)(L1)0.5]·H2O (6), [Cd(L3)(L1)0.5(H2O)] (7), [CoCl(L3)0.5(L1)0.5] (8), [ZnCl(L3)0.5(L2)0.5] (9), and [CoCl(L3)0.5(L2)0.5] (10), where L1 = 1,1′-(1,4)-butanediyl)bis(imidazole), L2 = 1,1′-(1,4-butanediyl)bis(2-ethylbenzimidazole) and H2L3 = 3,3′-(p-xylylenediamino)bis(benzoic acid), have been synthesized by varying the metal centers and nitrogen-containing secondary ligands. These structures have been determined by single-crystal X-ray diffraction analyses, elemental analyses and IR spectra. In 1, the L3 anion is not coordinated to the Ni(II) center as a free ligand. The Ni(II) ion is coordinated by water molecules to form the cationic [Ni(H2O)6]2+ complex. The hydrogen bonds between L3 anions and [Ni(H2O)6]2+ cations result in a three-dimensional (3D) supramolecular structure of 1. In compounds 2 and 3, the metal centers are linked by the organic L3 anions to generate 1D infinite chain structures, respectively. The hydrogen bonds between carboxylate oxygen atoms and water molecules lead the structures of 2 and 3 to form 3D supramolecular structures. In 4, the L3 anion is not coordinated to the Ag(I) center, while the L1 ligands bridge adjacent Ag(I) centers to give 1D Ag-L1 chains. The hydrogen bonds among neighboring L3 anions form infinite 2D honeycomb-like layers, in the middle of which there exist large windows. Then, 1D Ag-L1 chains thread in the large windows of the 2D layer network, giving a 3D polythreaded structure. Considering the hydrogen bonds between the water molecules and L3 anions, the structure is further linked into a 3D supramolecular structure. Compounds 5 and 7 were synthesized through their parent compounds 1 and 3, respectively, while 6 and 9 were obtained by their parent compound 2. In 5, the L3 anions and L1 ligands connect the Ni(II) atoms to give a 3D 3-fold interpenetrating dimondoid topology. Compound 6 exhibits a 3D three-fold interpenetrating α-Po network structure formed by L1 ligands connecting Zn-L3 sheets, while compound 7 shows a 2D (4,4) network topology with the L1 ligands connecting the Cd-L3 double chains. In compound 8, the L1 ligands linked Co-L3 chains into a 2D layer structure. Two mutual 2D layers interpenetrated in an inclined mode to generate a unique 3D architecture of 8. Compounds 9 and 10 display the same 2D layer structures with (4,4) network topologies. The effects of the N-containing ligands and the metal ions on the structures of the complexes 1-10 were discussed. In addition, the luminescent properties of compounds 2-4, 6, 7 and 9 were also investigated.  相似文献   

3.
A series of new organotin (IV) complexes with 3-hydroxy-2-pyridinecarboxylic acid (3-OH-2-picH) of two types: R2SnCl(3-OH-2-pic) (I) (R = Me 1, n-Bu 2, Ph 3, PhCH24) and R2 Sn(3-OH-2-pic)2 (II) (R = Me 5, n-Bu 6, Ph 7, PhCH28)have been synthesized by reactions of diorganotin (IV) dichloride with 3-hydroxy-2-pyridinecarboxylic acid in the presence of sodium ethoxide. All complexes are characterized by elemental analyses, IR spectra and NMR spectra analyses. Among them, complexes 1, 5, 6 and 7 are also characterized by X-ray crystallography diffraction analyses. Complex 1 is a 1D polymeric chain with six-coordinate tin atoms and the packing of complex 1 is stabilized by the C-H?Cl intermolecular weak interactions, thus a 2D network of 1 is formed. Complex 5 is also a 1D polymeric chain with seven-coordinate tin atoms. Complex 6 is a zigzag polymeric chain linked by Sn?O intermolecular weak interactions. Complex 7 is a monomeric complex with distorted octahedral geometry.  相似文献   

4.
Reactions of different metal salts with 4-amino-3,5-bis(3-pyridyl)-1,2,4-triazole (3-abpt) gave rise to five new complexes, namely [Cu4(CN)4(3-abpt)2]n (1), [CuBr(3-abpt)]n (2), [CuI(3-abpt)]n (3), [Cu3I3(3-abpt)]n (4) and [Cu(3-abpt)(SO4)(H2O)]n (5). Compounds 1, 3, 4 and 5 are all 2D structures. Compound 1 is a double-layered polymer with an uncommon 3-nodal 3-connected (103)(102.4)4 network, 3 shows a 2D square layered structure, 4 is also a double-layered polymer with 2-nodal 4-connected (3.4.5.62.7)2(3.42.52.7) network and 5 is a 2D structure which is ultimately stacked with an ABAB repeat pattern. Compound 2 is a 1D coordination polymer which exhibits a ladder-like network. The photoluminescence of 1-2 has also been investigated. The long emission lifetimes of 1-2 could be assigned to metal-to-ligand charge transfer triple excited states [MLCT].  相似文献   

5.
A three-step synthesis of nineteen Z-shaped quadruple-bridged [6,6] and [6,4]orthocyclophanes comprising two quinoxaline-based sidewalls are described. The synthesis began from the bis-Diels−Alder adducts B1-B3 followed by ruthenium-promoted oxidation of dichloroetheno-bridges in the adducts to generate a bis-α-diketones, which were then condensed with various arene-1,2-diamines (9a-g) to construct sidewalls (phane parts) of Z-shaped quadruple-bridged orthocyclophanes D1-3, D2g, and D3g. Single-crystal structures of six orthocyclophanes (D1a, D2a, D2f, D3f, D2g-α, and D3g-α) were obtained and revealed that the CAr−H?π and π?π stacking interactions between N-containing arene rings are the major driving force for molecular assembly and crystal packing, in addition to the interactions involving the polar OCH3 groups and the solvate molecules.  相似文献   

6.
Five new 0D–2D Cd(II) complexes, [Cd2(Hbimt)2I4] (1), [Cd(bimt)(Hbimt)Br]n (2), [Cd(Hbimt)Cl2(H2O)]n (3), {[Cd(Hbimt)(SO4)(H2O)2]·1.5H2O}n (4) and [Cd(Hbimt)(SCN)2]n (5) (Hbimt = 2-((benzoimidazol-yl)methyl)-1H-tetrazole) have been synthesized by the reactions of Hbimt with suitable cadmium salts. Employment of different anions can influence the coordination modes of the Hbimt ligand, and accordingly result in different structures ranging from 0D to infinite 1D and 2D networks. Complex 1 displays a dimeric structure in which two Cd(II) ions are bridged through two iodine atoms. Complex 2 was caused by deprotonation of the Hbimt ligand, resulting in a 1D helical chain. While in complexes 3 and 4, Hbimt acts as a bidentate bridging ligand which joins two Cd(II) ions, leading to 1D stair-like chains. Complex 5 exhibits a 2D network structure with infinite 1D [Cd2(SCN)2]n chains. The distinct structures of 1, 2, 3, 4 and 5 reveal that the anions and the versatile coordination modes of the ligand play an important role in the structures of the complexes. In addition, the luminescent properties of complexes 15 have been investigated in the solid state at room temperature.  相似文献   

7.
A series of lanthanide(III) complexes with chelidamic acid ligand, [Ln(C7H2NO5)·3H2O]n·nH2O (Ln = La (1), Y (2), Sm (3), and Nd (4)), [Gd2(C7H2NO5)3·4H2O]n·2nH2O (5) and [Ce(C7H2NO5)·1.5H2O]n (6), have been synthesized by hydrothermal method and structurally characterized by single-crystal X-ray diffraction. Complexes 14 are isostructural and possess 2D framework. Complex 5 contains two different Gd(III) ions linked through carboxylate group to form a 2D framework. Complex 6 exhibits a (44) topology 2D network. The variable-temperature magnetic properties of 3 and 5 have been investigated. Furthermore, the photoluminescent properties of 1, 2, 3, and 5 at room temperature were also studied.  相似文献   

8.
Hydrothermal reactions of different lanthanide(III) salts with an amino-diphosphonate ligand (H4L=C6H5CH2N(CH2PO3H2)2) led to two series of lanthanide phosphonates, namely, Ln(H2L)(H3L) (Ln=La, 1; Pr, 2; Nd, 3; Sm, 4; Eu, 5; Gd, 6; Tb, 7). Compounds 1-5 feature a one-dimensional (1D) chain structure in which dimers of two edge-sharing LnO8 polyhedra are interconnected by bridging phosphonate groups, such 1D arrays are further interlinked via strong hydrogen bonds between non-coordinated phosphonate oxygen atoms into a two-dimensional (2D) layer with the phenyl groups of the ligands orientated toward the interlayer space. Compounds 6 and 7 also show a different 1D array in which the LnO6 octahedra are bridged by phosphonate groups via corner-sharing, such chains are also further interlinked by hydrogen bonds into a 2D supramolecular layer. Compounds 5 and 7 emit red and green light with a lifetime of 2.1 and 3.7 ms, respectively.  相似文献   

9.
Three novel polymers, {[Cd(m-bdc)(L)]·H2O}n (1), [Co(m-bdc)(L)0.5(H2O)]n (2) and [Zn5(L)2(p-bdc)5(H2O)]n (3) based on 1,1′-bis(pyridin-3-ylmethyl)-2,2′-biimidazole (L) ligand and benzenedicarboxylate isomers, have been prepared and structurally characterized. Compound 1 exhibits a 2D architecture with (42·6)(42·67·8) topology, which is synthesized by L and 1,3-benzenedicarboxylate (m-bdc) ligands. Compound 2 is constructed from 1D chains that are linked by L ligands extending a 2D (4,4) grid. Compound 3 is a 3D framework with (43)(46·618·84) topology, which is composed of trinuclear clusters and five-coordinated metal centers joined through 1,4-benzenedicarboxylate (p-bdc) and L ligands. Moreover, the fluorescent properties of L ligand, compounds 1 and 3 are also determined.  相似文献   

10.
Five new transition metal coordination polymers based on H2tzda and co-ligand bpe, {[M(tzda)(bpe)]·H2O}n [M=Zn(1), Cd(2), Mn(3), Co(4)] and [Ni2(tzda)2(bpe)2(H2O)]n (5) [H2tzda=(1,3,4-thiadiazole-2,5-diyldithio)diacetic acid, bpe=1,2-bis(4-pyridyl)ethane], have been hydrothermally synthesized and structurally characterized. Compounds 1-4 feature a 2D-layered architecture generated from [M(tzda)]n moiety with double-chain structure cross-linking bpe spacers. However, the conformations bpe adopts in 3 and 4 are different from those in 1 and 2 due to the rotation of C-C single bond in bpe. Polymer 5 exhibits an interesting 3D porous framework with 2-fold interpenetration, in which intriguing 1D double helix chains are observed. The photoluminescence properties of 1 and 2 in the solid-state at room temperature are investigated. In addition, variable-temperature magnetic data show weak antiferromagnetic behavior in 3-5.  相似文献   

11.
Four coordination polymers, [Zn(pda)(bpy)(H2O)]n·nH2O (1), [Cd(pda)(prz)(H2O)]n (2), [Co3(μ3-OH)2(pda)2(pyz)]n·2nH2O (3) and [Pr2(pda)3(H2O)2]n (4) (H2pda=1,3-phenylendiacetic acid, bpy=4,4′-bipyridine, prz=piperazine and pyz=pyrazine) have been hydrothermally synthesized and characterized. Complex 1 is a 1D wheel-like chain structure, which is further extended into a 3D metal-organic supramolecular framework by H-bonds and π-π stacking interactions. Complex 2 is a 1D ladder-like chain structure, which is also further extended into a 3D metal-organic supramolecular framework by H-bonds. Complex 3 possess a 2D sheet structure with infrequent two pairs of double-helix chains. Complex 4 features a 3D structure. Both 1 and 2 display strong blue fluorescent emission at room temperature. Magnetic susceptibility measurements of complexes 3 and 4 exhibit antiferromagnetic interactions between the nearest metal ions, with C=9.99 and 3.43 cm3 mol−1 K, and θ=−23.9 and −46.3 K, respectively.  相似文献   

12.
Twelve new organotin complexes with 4-sulfanylbenzoic acid of two types: RnSn[S(C6H4COOH)]4−n (I) (n = 3: R = Me 1, n-Bu 2, Ph 3; PhCH24; n = 2: R = Me 5; n-Bu 6, Ph 7, PhCH28) and R3Sn(SC6H4COO)SnR3 · mEtOH (II) (m = 0: R = Me 9, n-Bu 10, PhCH212; m = 2: R = Ph 11), along with the 4,4′-bipy adduct of 9, [Me3Sn(SC6H4COO)SnMe3]2(4,4-bipy) 13, have been synthesized. The coordination behavior of 4-sulfanylbenzoic acid is monodentate in 1-8 by thiol S atom but not carboxylic oxygen atom. While, in 9-13 it behaves as multidenate by both thiol S atom and carboxylic oxygen atoms. The supramolecular structures of 6, 11 and 13 have been found to consist of 1D molecular chains built up by intermolecular O-H?O, C-H?O or C-H?S hydrogen bonds. The supramolecular aggregation of 7 is 2D network determined by two C-H?O hydrogen bonds. Extended intermolecular C-H?O interactions in the crystal lattice of 9 link the molecules into a 2D network.  相似文献   

13.
Four new open-framework coordination polymers of lanthanide 2,5-pyridinedicarboxylates, with the formulas Pr2(pydc)3(H2O)2 (1), Ln(pydc)(Hpydc) (Ln=Tb (2), Er (3), Eu (5)), and Gd(pydc)(nic)(H2O) (4) (H2pydc=2,5-pyridinedicarboxylic acid, Hnic=nicotinic acid), have been hydrothermally synthesized and four of them (except Eu (5)) have been structurally characterized. Complex 1 consists of two types of ligand-binding modes contributing to link the PrO7N(H2O) polyhedral chains to three-dimensional (3D) open-framework architecture. Complexes 2 and 3 are isostructural and feature unique 3D cage-like supramolecular frameworks remarkably different from that of 1, owing to the different ligand-bridging pattern. Complex 4, however, has the distinct 3D open-framework architecture due to the presence of unexpected nicotinate ligands, which may be derived from pydc ligands via in-situ decarboxylation under the hydrothermal condition.  相似文献   

14.
A series of group 12 metal coordination polymers with 1,2-bis(diphenylphosphino)ethane dioxide (dppeO2), {[ZnCl2(μ-dppeO2)]·CH2Cl2}n (1·CH2Cl2), [ZnBr2(μ-dppeO2)]n (2), [CdI2(μ-dppeO2)]n (4), [(HgI2)2(μ-dppeO2)]n (5), [Zn(SCN)(μ-SCN)(μ-dppeO2)]n (6), and [Cd(NO3)(μ-SCN)(μ-dppeO2)]n (7), have been synthesized and structurally characterized. The structures of the compounds are all based on an infinite 1D chain constructed by four-coordinate metal ions and dppeO2 ligands adopting the trans bridging coordination fashion. In the coordination polymers 1, 2 and 4, the halide ions act as terminal ligands, leading to discrete 1D chains with alternative MX2 and dppeO2 repeating units. The mercury compound 5 features a unique square-wave-like inorganic chain –[Hg(1)–I–Hg(2)–I]–, and the 1D HgI2(μ-dppeO2) chains are further linked by HgI2 bridges to form a 3D network. In the thiocyanate-containing compounds 6 and 7, the 1D chains are linked by one (6) or two (7) bridging SCN ions to result in 2D layered structures. Solid-state emission spectra of the coordination polymers show different variations compared to the free dppeO2 ligand, such as enhancement (1, 2, 6 and 7), shift (3 and 4) and quenching (5) upon metal coordination.  相似文献   

15.
Five novel coordination polymers, [Co(bpb)2Cl2] (1), [Co(bpb)2(SCN)2] (2), [Cd(H4bpb)0.5(dmf)(NO3)2] (3), [Cd2(H4bpb)Br4] (4), and [Hg2(H4bpb)I4] (5) [bpb=N,N′-bis(3-pyridylmethyl)-1,4-benzenedimethyleneimine, H4bpb=N,N′-bis(3-pyridylmethyl)-1,4-benzenedimethylamine], were synthesized and their structures were determined by X-ray crystallography. In the solid state, complex 1 is a 1D hinged chain, while 2 has 2D network structure with the ligand bpb serving as a bridging ligand using its two pyridyl N atoms. The imine N atoms keep free of coordination and bpb acts as a bidentate ligand in both 1 and 2. Complexes 3, 4, and 5 with reduced bpb ligand, i.e. H4bpb, show similar 2D network structure, in which ligand H4bpb serves as a tetradentate ligand. Thermogravimetric analyses for complexes 1-5 were carried out and found that they have high thermal stability. The magnetic susceptibilities of compounds 1, 2 were measured over a temperature range of 75-300 K.  相似文献   

16.
A bioinorganic approach into the problem of the isomorphous substitution of calcium(II) by lanthanide(III) ions in biological systems is discussed. Reactions of malonamic acid (H2malm) with CaII and NdIII sources under similar conditions yielded the compounds [Ca(Hmalm)2]n (1), [Nd(Hmalm)2(H2O)2]n(NO3)n (2) and [Nd(Hmalm)2(H2O)2]nCln·2nH2O (3·2nH2O). Their X-ray crystal structure data show that the malonamate(-1) ligand presents two different ligation modes and coordinates through the two carboxylate and the amide-O atoms, thus bridging three CaII ions in 1 and two NdIII ions in 2 and 3·2nH2O. Complex 1 is a 3D coordination polymer based on neutral repeating units, whereas 2 and 3·2nH2O are 1D coordination polymers based on the same cationic repeating unit. Hydrogen bonding interactions further stabilize the 3D framework structure of 1 and assemble the 1D chains of 2 and 3·2nH2O into 3D networks. The three complexes were characterized spectroscopically (IR, far-IR, and Raman) and the thermal decomposition of 2 and 3·2nH2O was monitored by TG/DTA and TG/DTG measurements. Variable-temperature magnetic susceptibility data for 2 are also reported. The bioinorganic chemistry relevance of our results is discussed.  相似文献   

17.
Fanhong Wu  Fanhua Xiao  Yongjia Shen 《Tetrahedron》2006,62(43):10091-10099
Sodium dithionite initiated free-radical addition of polyfluoroalkyl iodides (2m-2s) with norbornene 1a and its derivatives, such as norbornene-2-carboxylates 1b and 1c, and norbornene-2-carboxylic acids 1d and 1e was investigated. In all the cases, the addition of RF group was stereoselectively delivered at exo-position and the predominant configuration of products was trans. Under the similar condition, norbornene-2-carboxylic ethyl ester 1b reacted with 2p to give 6-exo-RF-5-endo-iodo adduct 3bp and 5-exo-RF-6-endo-iodo adduct 5bp in the ratio of 4:1. While 1c, which has a heavy crowded group in the 2-endo-position, gave 6-exo-RF-5-endo-iodo adduct 3cp and polyfluoroalkylated product 4cp retaining the trans-configuration and the exo-orientation of RF group. The fluoroalkylation-lactonization reaction occurred in the reaction of norbornene-2-endo-carboxylic acids 1d and 1e with polyfluoroalkyl iodides to afford the corresponding fluoroalkylated γ-lactone products (7dp-7ds, and 7em-7er). The configuration of the products was further confirmed by 2D NMR and X-ray diffraction analyses for the first time.  相似文献   

18.
Five new lanthanide supramolecular complexes, namely, [Sm(oqa)2(H2O)4]2 (ClO4)2·(bpy)2 (1), [Ln(oqa)3]·2H2O [Ln=Sm(2), Gd(3)] and [Ln(oqa)2(NO3)(H2O)] [Ln=Pr(4), Eu(5)] (oqa=4-oxo-1(4H)-quinolineacetate, bpy=4,4′-bipyridine), have been synthesized under hydrothermal conditions. These complexes exhibit three typical structure features. Complex 1 possesses a dimeric structure, which is further connected together through hydrogen bonds and π-π attractions, forming a 3D supramolecular framework. Compounds 2-3 are isomorphous and contain 1D ring-like chains, which are further interconnected by the oqa ligands into 2D sheet-like structures. 4 and 5 exhibit eight-connected 3D network of 424·64-bcu topology. The various coordination modes of carboxylate ligands and the selection of the counterions have clearly affected the topological structures. Furthermore, the solid-state luminescent properties of complexes 1, 2 and 5 were investigated at room temperature and they show intense, characteristic emissions in the visible region.  相似文献   

19.
Oolongtheanin-3′-O-gallate (2b) was obtained by treatment of (−)-EGCg (1d) with CuCl2. This transformation was achieved over three steps, with the isolation of two intermediates; their chemical structures were determined through derivatization reactions, MS, and 1D/2D NMR techniques. One intermediate was identified as dehydrotheasinensin A (3); the other was identified as the novel dimer pro-oolongtheanin-3′-O-gallate (6). Compound 3 was converted to 6 by heating in aprotic solvent, and compound 6 was converted to 2b by addition of water.  相似文献   

20.
A new dimer of C16N2 type alkaloid, complanadine B (1), and two new C16N type alkaloids, obscurumines A (2) and B (3), have been isolated from the club moss Lycopodium complanatum and L. obscurum, respectively. The structures and stereochemistry of 1-3 were elucidated by combination of 2D NMR spectra and chemical transformation. Complanadine A (4) isolated together with 1 induced secretion of neurotrophic factors from human astrocytoma cells.  相似文献   

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