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1.
《Journal of Coordination Chemistry》2012,65(16-18):2732-2739
Abstract

Two C3-symmetric ligands, 4,4′,4″-[1,3,5-benzenetriyltris(carbonylimino)]trisbenzoic acid (H3BTA) and benzene-1,3,5-trisbenzoic acid (H3BTB), were used to coordinate Er(III) and In(III). Reactions of the two C3-symmetric ligands with Er(NO3)3·6H2O and In(NO3)2·3H2O under solvothermal conditions resulted in formation of two new three-dimensional porous coordination polymers, [Er(BTA)(DMF)](DMF)2(H2O) (1) and [In(H2O)(BTB)](DMF)2 (2). In addition, in vitro anticancer activities of 1 and 2 on three human glioma cells (SHG-44, SWO-38, and TJ905) were determined.  相似文献   

2.
A 3-D metal-organic framework [Cd3(L)2(DMF)2]?·?2H2O?·?2DMF (1) (H3L?=?2-(dimethylcarbamoyl)biphenyl-5,2′,5′-tricarboxylic acid, DMF?=?N,N-dimethylformamide) with trinuclear Cd(II) units has been prepared. Complex 1 is a (3,?6)-connected (42?·?6)2(44?·?62?·?88?·?10) coordination net, which results from the solvothermal in situ formation of a new asymmetric ligand, 2-(dimethylcarbamoyl)biphenyl-5,2′,5′-tricarboxylic acid (H3L), through amidation of biphenyl-2,5,2′,5′-tetracarboxylic acid (H4bptc). Additionally, the luminescence of 1 has been investigated.  相似文献   

3.
[Co2(TTBT)4(1,2-BDC)2] n ?·?4nH2O (1), [Pb2(TTBT)2(1,3-BDC)2] n ?·?nTTBT?·?2nH2O (2), [Fe(TTBT)(1,4-BDC)(H2O)] n (3), and [Zn(TTBT)(1,4-BDC)(H2O)] n (4) have been hydrothermally synthesized by self-assembly of TTBT (TTBT?=?10,11,12,13-tetrahydro-4,5,9,14-tetraaza-benzo[b]triphenylene), benzene-dicarboxylic acid ligands 1,2-H2BDC, 1,3-H2BDC or 1,4-H2BDC (1,2-H2BDC?=?1,2-benzenedicarboxylic acid, 1,3-H2BDC?=?1,3-benzenedicarboxylic acid, 1,4-H2BDC?=?1,4-benzenedicarboxylic acid), and various metal salts. Compound 1 has dinuclear cluster units, four dimeric Co2 units connected to form a 32-membered ring via weak offset π–π interactions, which are further stacked via strong π–π interactions to form a 3-D supramolecular framework. Complex 2 contains 2-D layers with rhombohedral grids, which are connected to a 3-D structure by π–π interactions. 3 and 4 feature 1-D infinite chains, which are further extended by strong π–π interactions and O–H···O hydrogen bonds resulting in 3-D supramolecular architectures. The photoluminescent properties of 2 and 4 have also been investigated.  相似文献   

4.
Twelve oxamide-bridged Ln(III)–Cu(II) heteropentanuclear complexes Ln[Cu(PMoxd)]4(ClO4)3 · 5H2O (Ln = La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Yb, and PMoxd = the N,N′-Bi(α-pyridylmethyl)-oxamide dianion) and 12 oxamide-bridged Ln(III)–Cu(II) heteropentanuclear complexes with the formula of Ln[Cu(PEoxd)]4(ClO4)3 · 5H2O (PEoxd = the N,N′-Bi(α-pyridylethyl)-oxamide dianion) were synthesized and characterized. The magnetic properties of Gd[Cu(PMoxd)]4(ClO4)3 · 5H2O (7) and Gd[Cu(PEoxd)]4(ClO4)3 · 2H2O (19) show that there are ferromagnetic interactions between Gd(III) and Cu(II) in the complexes with J Cu–Gd = 1.38 cm?1 and J Cu–Gd = 1.00 cm?1, respectively. Fluorescent quenching phenomena for Eu[Cu(PMoxd)]4(ClO4)3 · 5H2O (6) and Tb[Cu(PMoxd)]4(ClO4)3 · 5H2O (8) were also observed.  相似文献   

5.
Two coordination polymers, {[Zn(NiL)(DMA)(H2O)2] (DMA)(H2O)} n (1) (DMA?=?N,N-dimethylacetamide) and {[Zn2(NiL)2(DMF)(H2O)4]?·?3DMF} n (2) (DMF?=?N,N-dimethylformamide), have been prepared by reactions of Zn(NO3)2?·?6H2O and NiL in CH2Cl2-DMA–H2O and CH2Cl2-DMF–H2O, respectively. H2L denotes dimethyl 5,6,7,8,15,16-hexahydro-6,7-dioxodibenzo-9,10-benzo-[1,4,8,11]tetraazacyclotetradecine-13,18-dicarboxylate. Single-crystal X-ray diffraction analyses reveal that coordination geometries around Ni(II) are identical with slightly distorted square planar and all Ni–N bonds are very short. Complex 1 shows 1-D zigzag chain structure, while 2 has 1-D double-zigzag chains. The chains, which are packed parallel in 1 and 2, are interconnected by lattice solvent through O–H···O and C–H···O hydrogen bonds to form 3-D supramolecular networks. We discuss solvent effects on assembly of the two coordination polymers. The results reveal that coordinated solvent has influence on the assembly procedure.  相似文献   

6.
Three lanthanide coordination polymers, [Ln4(BDC)6(H2O)2] n (Ln = Er, 1; Ln = Tm, 2; BDC = 1,2-benzenedicarboxylate) and {[Nd2(BDC)(EDTA)(H2O)2] · 1.5H2O} n , 3, were prepared by hydrothermal synthesis and characterized by elemental analysis, IR spectra, as well as single-crystal X-ray diffraction. The isostructural coordination polymers 1 and 2 exhibit four different coordination modes, which are rarely found in one lanthanide complex. Complex 3 displays a 2-D wave-like network assembled by two polycarboxylate ligands.  相似文献   

7.
The reaction of α-[SiMo12O40]4? with trivalent cations Ln3+ and N-methyl-2-pyrrolidone leads to a series of complexes of formula [Ln(NMP)4(H2O) n ]H[SiMo12O40]?·?2NMP?·?mH2O [where Ln?=?La (1), Pr (2), Nd (3), Sm (4), Gd (5), n?=?4, Ln?=?Dy (6), Er (7), n?=?3. NMP?=?N-methyl-2-pyrrolidone]. The syntheses, X-ray crystal structures, IR, and ESR spectra and thermal properties of the complexes 1, 2, 4, 6, 7 have been reported previously. Here, we report X-ray crystal structures, IR, UV, ESR spectra and thermal properties of the complexes [Nd(NMP)4(H2O)4]H[SiMo12O40]?·?2NMP?·?1.5H2O (3), and [Gd(NMP)4(H2O)4]H[SiMo12O40]?·?2NMP?·?H2O (5). In addition, the electrochemical behaviour of this series of complexes in aqueous solution and aqueous-organic solution has been investigated and systematic comparisons have been made. All these complexes exhibit successive reduction process of the Mo atoms.  相似文献   

8.
The reactions of Ln(NO3)3?6H2O (Ln=Pr, Nd or Er) with the potentially tridentate O,N,O chelating ligand 2,6-pyridinedimethanol (H2pydm) in a 1:2 M ratio were investigated, and complexes with the formula [Ln(H2pydm)2(NO3)2](NO3) (Ln=Pr or Nd) (1 and 2) and [Er(H2pydm)3](NO3)3 (3) were isolated. The compounds contain 10-coordinate Pr(III) and Nd(III) ions that crystallize in the triclinic space group P-1 while the 9-coordinate Er(III) complex crystallizes in the monoclinic system (P21/n). A new lanthanide complex, [Pr(H2pydm)3](Cl)3?DMF (4), has been synthesized by reaction of PrCl3?6H2O and H2pydm. The nine-coordinate Pr(III) is bound to three H2pydm ligands. X-ray crystal structures of 1–4 reveal that the ligand coordinates tridentate via the pyridyl nitrogen and the two hydroxyl oxygens. The electronic absorption spectra of 1–4 show 4f–4f transitions.  相似文献   

9.
Two new hetero-tetranuclear complexes, [Sm2(o-phen)2(DMF)6(H2O)2(µ-CN)4Fe2(CN)8]·;5H2O·;CH3OH (1) and [Sm2(o-phen)2(DMF)6(H2O)2(µ-CN)4Co2(CN)8]·;5H2O (2), have been prepared from reaction of SmCl3·;6H2O, K3[Fe(CN)6]·;3H2O or K3[Co(CN)6], and o-phen in methanol/DMF, and characterized. The structure of 1 consists of a cyano-bridged discrete cyclic tetranuclear complex in which the Sm(III) and Fe(III) centers are linked by four CN groups. Mössbauer spectrum of 57Fe indicates that both Fe(III) atoms in 1 have the same low-spin (S?=?1/2) electronic ground state. From comparison of the magnetic data of 1 and 2, at low temperature for 1 indicates weak ferromagnetic coupling between Sm(III) and Fe(III).  相似文献   

10.
Hydrothermal reactions of Nd(ClO4)3·6H2O, Gd(ClO4)3·6H2O and Er2O3 with H3NTA (nitrilotriacetic acid) afford three new lanthanide coordination polymers, {[Nd(NTA)(H2O)]· 2H2O} n (1), {[Gd(NTA)(H2O)]·2H2O} n (2) and {[Er(NTA)(H2O)]·H2O} n (3), characterized by elemental analysis and IR spectroscopy. X-ray single crystal structural analyses showed that 1 and 2 are an isomorphous 2D-layered framework containing the nine-coordinated Nd(III) (or Gd(III)), and woven into a 3D suprastructure by interlayer hydrogen bonding while 3 is a 3D structure with eight-coordinate Er(III).  相似文献   

11.
The reactions of cobalt acetates with tetrachloroterephthalic acid (H2BDC‐Cl4) in different solvents gave two polymeric and one mononuclear CoII complexes. X‐ray single‐crystal structural determination revealed that the ligand BDC‐Cl4 displays a reliable bridging tecton to construct diverse supramolecular architectures through coordinative bonds or secondary hydrogen‐bonding interactions. The complexes [Co(BDC‐Cl4)(DMF)2(EtOH)2]n ( 1 ) and {[Co(BDC‐Cl4)(DMF)2(MeOH)2] · 2DMF}n ( 2 ) demonstrate a one‐dimensional (1D) coordination motif with infinite CoII‐tetrachloroterephthalate chains, which are tuned by different binding solvent systems of DMF/ethanol (EtOH) and DMF/methanol (MeOH). [Co(DMF)2(H2O)4] · (BDC‐Cl4) ( 3 ) represents a two‐dimensional (2D) metallosupramolecular network by hydrogen‐bonded bridging between the aqua ligand of the mononuclear complex with the uncoordinated BDC‐Cl4 solvates. The spectroscopic, thermal, and fluorescent properties of 1 – 3 were also investigated.  相似文献   

12.
The host and the apohost framework of [Zn2(1,4-bdc)2(dabco)]?·?4DMF?·?½H2O (1?·?4DMF?·?½H2O) (1,4-bdc?=?1,4-benzenedicarboxylate and dabco?=?1,4-diazabicyclo[2.2.2]octane) were used for the preparation of ZnO nanomaterials. With calcination of the host framework of 1?·?4DMF?·?½H2O, ZnO nanoparticles could be fabricated. By the same process on fully desolvated framework of 1, ZnO microrods composed of ZnO nanoparticles were formed. These results indicate with removal of the guest solvent from the pores of this metal-organic framework (MOF), nanoparticle agglomeration increases and the role of this MOF in preparation of ZnO nanoparticles was reduced.  相似文献   

13.
Sandwich coordination complexes, [LnIII(H3L)2]X3?solvents, of Tb(III), Eu(III), Dy(III), Ho(III) and Er(III) were prepared with two new zwitterionic ester-substituted tripodal amine ligands, tris((2-hydroxy-5-n-butyl benzoate)aminoethyl)-amine (H3L1) and tris((2-hydroxy-5-methyl benzoate)aminoethyl)-amine (H3L2). These ligands were synthesised by condensation of the appropriately substituted salicylaldehyde with tris(2-aminoethyl)amine (tren) followed by in situ reduction of the tris-imine to tris-amine. Subsequent 2:1 reaction with lanthanide(III) ions yields [LnIII(H3L)2]X3?solvents (L = L1, L2; X = Cl?, NO3?; solvents = MeOH or H2O). All complexes were characterised by microanalysis, infrared spectroscopy, high resolution mass spectrometry and solid-state photoluminescence measurements. The crystal structures of [TbIII(H3L1)2]Cl3·6MeOH, [Dy(H3L1)2]Cl3·6MeOH, [EuIII(H3L1)2]Cl3·6MeOH and [TbIII(H3L1)2](NO3)3 reveal high-crystallographic ?3 symmetry at the O6-coordinated octahedral lanthanide(III) ions and that the tripodal ligands are bound in zwitterionic form: the protons from the phenolic oxygens have migrated to the amino nitrogens. Photoluminescence measurements indicate various degrees of energy transfer of the ligand chromophore to the lanthanide ions, as both ligand and lanthanide emission features are observed. Despite the high-crystallographic symmetry and the likely small transverse magnetic anisotropy of the complexes, no evidence of slow relaxation of the magnetisation, characteristic of a single-molecule magnet, was observed for [TbIII(H3L1)2]Cl3·MeOH·3H2O, [DyIII(H3L1)2]Cl3·6H2O, [HoIII(H3L1)2](NO3)3·2H2O, [ErIII(H3L1)2]·H2O and [TbIII(H3L1)2](NO3)3 down to 2.0 K.  相似文献   

14.
Four lanthanide complexes with two tri-protonated hexacarboxylic acids [1,2,3,4,5,6-cyclohexane-hexacarboxylic acid (H6chhc) and mellitic acid (H6Mel)], [Pr(H3chhc)(DMF)3(H2O)]·H2O (1), Nd(H3chhc)(DMF)3 (2), [Er(H2O)8]·(H3Mel)·9(H2O) (3), and [Yb(H2O)8]·(H3Mel)·8.5(H2O) (4), have been synthesized in solution at room temperature and characterized by elemental analysis, IR spectrum, and single-crystal X-ray diffraction. The crystal structures of 1 and 2 are made up of a (44, 62) 2-D network extended infinitely parallel to the (1?0?0) plane. The H3chhc3? anions assume a cis-e,a,e,a,e,a-conformation with the central ring in chair-shaped configuration. In 3 and 4, the H3Mel3? as counter ions are interconnected by hydrogen bonds to form 2-D organic supramolecular layers. The coordination modes and abilities of H6chhc and mellitic acid are discussed and compared. The luminescences of 1–4 have been investigated.  相似文献   

15.
Two complexes, [Co(H2pimdc)2(H2O)2]?·?2DMF (1) and [Co(H2pimca)2(H2O)2]?·?4H2O (2), have been designed, synthesized, and characterized (X-ray single crystal analysis, thermal analysis, electrochemical analysis, and infrared spectrum) based on the imidazole ligand [H3pimdc?=?2-propyl-4,5-imidazoledicarboxylic acid]. Both compounds have 3-D hydrogen-bonding networks. Because of different coordination of water, 1 forms a layer-like geometry via hydrogen bonds, but 2 forms a fishingnet-like latticed geometry via hydrogen bonds.  相似文献   

16.
The reactions of m-H2BDC, NaOH with Cd(NO3)2?·?4H2O and Co(NO3)2?·?4H2O (m-BDC?=?1,3-benzene-dicarboxylate) in DMF gave two isostructural three-dimensional (3D) heterometallic coordination polymers: [CdNa(m-BDC)2]?·?[NH2(CH3)2] (1) and [CoNa(m-BDC)2]?·?[NH2(CH3)2] (2), respectively. The compounds were characterized by single-crystal X-ray diffraction, X-ray powder diffraction, ICP, TGA, IR, and photoluminescence spectroscopy. The crystal structures were determined by X-ray diffraction and refined by full-matrix least-squares methods to R?=?0.0221 and wR?=?0.0579 using 1925 reflections with I?>?2σ(I) for 1; and R?=?0.0654 and wR?=?0.1591 using 1881 reflections with I?>?2σ(I) for 2. Their frameworks are constructed from M–O–C (M?=?Na, Cd and Co) chains composed of alternating six-coordinate Na(I) centers and four-coordinate Cd(II) or Co(II) centers. These chains are further linked by m-BDC to form unusual 3D open-framework structures.  相似文献   

17.
This article describes supramolecular interactions induced in a high molecular weight dithiocarbamate, padtc, by its design. Synthesis, spectral studies involving zinc, cadmium and mercury, padtc, and adducts with tmed, such as [Zn(padtc)2] (1), [Zn(padtc)2(tmed)]?·?C6H5CH3?·?0.5(H2O) (2), [Cd(padtc)2] (3), [Cd(padtc)2(tmed)]?·?C6H5CH3?·?0.36(H2O) (4), [Hg(padtc)2]?·?H2O (5), [Hg(padtc)2(2,2′-bipy)]?·?H2O (6), [Hg(padtc)2(1,10-phen)]?·?H2O (7), and [Hg(padtc)2(oxine)]?·?H2O (8) (where padtc??=?N,N′-(iminodiethylene)bisphthalimidedithiocarbamate, 1,10-phen?=?1,10-phenanthroline, tmed?=?tetramethylethylenediamine, 2,2′-bipy?=?2,2′-bipyridine, oxine?=?8-hydroxyquinoline) along with the single crystal X-ray structural analysis of [Zn(padtc)2(tmed)]?·?C6H5CH3?·?0.5(H2O) (2) and [Cd(padtc)2(tmed)]?·?C6H5CH3?·?0.36(H2O) (4) are reported. All the complexes were characterized by IR, NMR (1H and 13C), and thermogravimetric study. The IR spectra of the complexes show the contribution of the thioureide form to the structures. In 13C NMR spectra, the most important thioureide (N13CS2) carbon signals are observed at 210–212?ppm. Single crystal X-ray structural analyses of 2 and 4 show the presence of extensive supramolecular interactions stabilizing the solid-state structure. Both zinc and cadmium are in a distorted octahedral environment with MS4N2 chromophores. VBS of Zn and Cd are 1.76 and 1.98, respectively, supporting the correctness of the determined structure and the valence of the central metal ions.  相似文献   

18.
Three 1-D reduced molybdenum(V) phosphates, [Ni(OH)2][Na2(H2O)3]2{Ni[(MoO2)6(OH)3(HPO4)3(PO4)]2}?·?2C6H14N2?·?2H3O?·?5H2O (1), [Ni(H2O)2][K(H2O)5]2{Ni[(MoO2)6(OH)3(HPO4)3(PO4)]2}?·?2C6H14N2?·?2H3O?·?4H2O (2), and [Cu(H2O)2][Na(H2O)5]2{Cu[(MoO2)6(OH)3(HPO4)3(PO4)]2}?·?2C6H14N2?·?2H3O?·?4H2O (3), have been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. The crystallographic analysis reveals that 1 is based on {Ni[Mo6O12(OH)3(HPO4)3(PO4)]2} clusters connected through {[Ni(OH)2][Na2(H2O)3]2} pentanuclear mixed-metal cluster units to yield unusual 1-D chains along the c-axis, which further form 3-D supramolecular networks via hydrogen-bonding. Compounds 2 and 3 are heterogeneous isostructural compounds. Both are built from M[Mo6P4]2 (M?=?Ni or Cu) blocks as the structural motif combined with [MO4(H2O)2] (M?=?Ni or Cu) octahedra to form 1-D chains, where M[Mo6P4]2 (M?=?Ni or Cu) is bonded by [M′(H2O)5] (M′?=?K or Na). Furthermore, bulk carbon paste electrode modified with 1 (1-CPE) displays good electrocatalytic activity toward reduction of nitrite or bromate.  相似文献   

19.
A new oxamido-bridged dinuclear compound [Cu2(µ-pmox)(DMF)4]?·?2ClO4 (1) (H2pmox?=?N,N′-bis-(2-methylpyridyl)oxalamide, DMF?=?dimethylformamide) was synthesized and structurally characterized. The five-coordinate Cu(II) is bridged by oxamido groups and further cross-linked by C–H···O hydrogen bonds between the uncoordinated oxygen of perchlorate and methyl of DMF. The complex was also characterized by infrared spectroscopy and magnetic measurement. The copper complex exhibits strong antiferromagnetic interactions via the trans oxamido bridge with J of ?414?cm?1, where J is the exchange parameter in the isotropic Hamiltonian H?=??JS1S2.  相似文献   

20.
Five lanthanide(III) coordination polymers with 2-methyl-1H-imidazole-4,5-dicarboxylic acid (H3MIDC) and ammonium oxalate, {[(Ln1)2(HMIDC)2(C2O4)(H2O)3]?·?3H2O} n (Ln1?=?Nd (1), Sm (2)), {[Eu2(HMIDC)2(C2O4)(H2O)3]?·?0.5EtOH?·?3H2O} n (3), {[Ce2(HMIDC)2(C2O4)(H2O)3]?·?EtOH?·?3H2O} n (4), and {[Gd2(HMIDC)2(C2O4)(H2O)3]?·?MeOH?·?3H2O} n (5), have been prepared and structurally characterized. Single-crystal X-ray diffraction analyses reveal that 1 and 2 are isostructural, as are 3, 4, and 5. Each exhibits a 3-D open framework, which is built by a regular 2-D grid connected by HMIDC2? and Ln(III). The luminescence and thermal properties of these complexes have been investigated as well.  相似文献   

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