首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到20条相似文献,搜索用时 31 毫秒
1.
A new structural supramolecular zinc(II) complex (1), [Zn(H2O)6]2+[Zn(4,4′-bipy)(SO4)2(H2O)2]2?[Zn(4,4′-bipy)(SO4)(H2O)3] is synthesized in mixed solvent system at room temperature. The complex was characterized by elemental analysis, IR spectroscopy and single crystal X-ray diffraction. Structural analyses reveal that the complex is crystallized in the triclinic system with P1 space group. Cell parameters: a = 7.3145 (15) Å, b = 11.194 (2) Å, c = 11.442 (2) Å, α = 72.48 (3)°, β = 73.78 (3)°, γ = 83.39 (3)°, V = 857.3 (3) Å3. Zn atoms (Zn1, Zn2 and Zn3) are all six-coordinated, however, the coordination environments of them are different. Owning to the abundant intro- and inter- hydrogen bonding interactions, the adjacent molecular units were connected to form a 2D supramolecular chain, and the two adjacent chains were furthermore linked to form a 3D supermolecular network structure via the hydrogen bonds. In addition, it is found that the complex has potential applications as fluorescent-emitting materials due to the strong fluorescence.  相似文献   

2.
The series of isostructural lanthanide coordination polymers with the empirical formula [Ln2(PDA)3(H2O)]·2H2O, where PDA = 1,4-phenylenediacetate anion = [C8H8(COO)2]2?; Ln = La-Lu(III), and Y(III) were produced in the reaction of LnCl3·nH2O with ammonium salt of 1,4-phenylenediacetic acid in water solution. The compounds were characterised structurally using powder X-ray diffraction, elemental and thermogravimetric analyses as well as FT-IR spectroscopy. Thermogravimetric analyses show that in the range 60–170 °C the dehydration process occurs. The thermal stability of dehydrated compounds, Ln2(PDA)3 increased from about 200–350 °C in the whole series of complexes. Single-crystal X-ray diffraction analysis for the Gd(III) complex revealed that the compound crystallizes in the monoclinic P21/c space group with a = 21.863(2) Å, b = 10.035(1) Å, c = 13.854(1) Å, β = 91.53(1)° and V = 3,038.5(4) Å3. The complex contains one-dimensional gadolinium-carboxylato chains, which are connected with the –CH2–C6H4–CH2– spacers of PDA ligand to the three-dimensional metal–organic framework.  相似文献   

3.
The single-crystal structure of |Zn35.5|[Si121Al71O384]-FAU per unit cell, a = 24.794(1), dehydrated at 673 K and 1 × 10?6 Torr, has been determined by single-crystal X-ray diffraction techniques in the space group \( Fd\bar{3}m \) at 294(1) K. The structure was refined using all intensities to the final error indices (using the 930 reflections for which F o > 4σ(F o)) R 1 = 0.0448 (based on F) and wR 2 = 0.1545 (based on F 2). About 35.5 Zn2+ ions per unit cell are found at an unusually large number of crystallographic distinct positions, six. The 0.5 Zn2+ ion per unit cell is located at the center of double 6-ring (D6R, site I; Zn(I)-O(3) = 2.642(3) Å and O(3)-Zn(I)-O(3) = 81.23(12) and 98.77(12)°). Two different site-I′ positions (in the sodalite cavities opposite D6Rs) are occupied by 14 and 3 Zn2+ ions per unit cell, respectively; these Zn2+ ions are recessed 0.67 Å and 1.02 Å, respectively, into the sodalite cavities from their 3-oxygens plane (Zn(I′a)-O(3) = 2.094(3) Å, Zn(I′b)-O(3) = 2.23(5) Å, O(3)-Zn(I′a)-O(3) = 110.32(12)°, and O(3)-Zn(I′b)-O(3) = 100.9(30)°). Site-II′ positions (in the sodalite cavities opposite S6Rs) are occupied by 6 Zn2+ ions, each of which extends 0.63 Å into the sodalite cavities from their 3-oxygens plane (Zn(II′)-O(2) = 2.164(3) Å and O(2)-Zn(II′)-O(2) = 112.00(12)°). Twelve Zn2+ ions are found at two nonequivalent sites II (in the supercage) with occupancies of 7 and 5 ions, respectively; these Zn2+ ions are recessed 0.52 Å and 0.96 Å, respectively, into the supercage from their 3-oxygens plane (Zn(IIa)-O(2) = 2.138(12) Å, Zn(IIb)-O(2) = 2.28(4) Å, O(2)-Zn(IIa)-O(2) = 114.2(10)°, and O(2)-Zn(IIb)-O(2) = 103.7(25)°).  相似文献   

4.
A novel tetra-nuclear macrocyclic Cu(II) complex has been synthesized by the reaction of cupric acetate monohydrate with N-acetyl-l-phenylalanine and 4,4-bipyridine in water/ethanol (v:v = 1:1) solution, and characterized by elemental analysis, IR and X-ray single crystal diffraction analysis. The results show that the Cu(II) complex belongs to monoclinic, space group P 21 with a = 14.993(3) Å, b = 14.831(3) Å, c = 22.262(4) Å, β = 99.37(3)°, V = 4884.2(16) Å3, Z = 2, D c  = 1.420 μg m?3, μ = 0.942 mm?1, F(000) = 2,160, and final R 1 = 0.0701, ωR 2 = 0.1905. The molecules form three dimensional tubular structures by the interaction of hydrogen bonds and π–π interaction. The A3 coupling reaction of phenylacetylene, aldehyde and amine (piperidine) in the presence of Cu(II) complex as an efficient heterogeneous catalyst has been studied. The catalyst displayed high activity and afforded the corresponding propargylamines with excellent yields. The Cu(II) complex catalyst was reused three times without significant loss of its catalytic activity.  相似文献   

5.
The self assembly of [Ni(L)]Cl2·2H2O (L = 3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,01.18,07.12]docosane) and 1,2,3,4-cyclobutanetetracarboxylic acid (H4cbtc) acid generates a 1D coordination and 2D hydrogen-bonded polymer [Ni(L)(H2cbtc)2·3H2O] n (1). Complex 1 is characterized by X-ray crystallography, spectroscopy and magnetic susceptibility. Each nickel(II) ion has a distorted octahedral coordination environment with the four secondary amines of the macrocycle in which two carboxylate anions of the H2cbtc2? ligand have assembled around each nickel center. The compound crystallizes in the triclinic system P-1 with a = 9.715(3) Å, b = 12.891(5) Å, c = 13.903(6) Å, α = 72.64(2)°, β = 75.70(3)°, γ = 73.27(3)°, V = 1566.6(10) Å3, Z = 2. The electronic spectrum of 1 indicates a high-spin octahedral environment. The magnetic behavior of 1 reveals a weak intramolecular antiferromagnetic interaction with J = ?1.23(1) cm?1.  相似文献   

6.
A novel metal–organic framework {[Zn(2,3-pydc)(bbi)]·0.5CH3CN·2H2O} n (2,3-pydc = pyridine-2,3-dicarboxylate, bbi = 1,1′-(1,4-butanediyl)bis(imidazole)) (1), was prepared under hydrothermal conditions and characterized by elemental analyses, IR and X-ray diffraction. Crystal data for 1 are monoclinic, space group C2/c, a = 19.685(2) Å, b = 14.332(1) Å, c = 16.930(2) Å, β = 121.205(2)°, U = 4085.3(6) Å3, Z = 4. The results reveal that the Zn(II)-atom is five-coordinated with two O-atoms and three N-atoms forming a distorted trigonal bipyramidal geometry. The Zn(II) atoms are bridged by 2,3-pydc and bbi ligands, leading to a three-dimensional network. The Zn···Zn separations are 8.277 Å [through the 2,3-pydc bridge] and 12.638 Å [through the bbi bridge]. Additionally, 1 shows strong fluorescence in the solid state at room temperature.  相似文献   

7.
A new flexible triazine-based polycarboxylate metal–organic framework, [Sm2(TTHA)(H2O)4]·9H2O (I) (TTHA = 1,3,5-triazine-2,4,6-triamine hexaacetate), has been synthesized under hydrothermal conditions and characterized by single crystal X-ray diffraction, elemental analysis and FT-IR spectroscopy. Crystal data for I are monoclinic C2/c, a = 12.6974(13) Å, b = 16.7309(12) Å, c = 14.8076(15) Å, β = 91.452(8)°, V = 3,144.7(5) Å3. Each SmIII ion is 9-coordinate in a distorted tri-capped trigonal prismatic geometry; but, the principal inorganic building block is {Sm2O16}, which comprises two of these polyhedra that share an edge. The complex exhibits a three-dimensional open-framework structure of approximately 31 % void volume, which comprises two types of channels oriented in three directions; [0 0 1], [1 1 0] and [?1 1 0]. The network can be simplified into either the cooperite (pts) or anatase (ant) topologies depending on the choice of nodes. The UV–Vis spectra of the compound are dominated by the absorption of the TTHA ligand. Thermogravimetric analysis shows that the loss of channel and coordinated water upon heating occurs in two distinct steps.  相似文献   

8.
The ionic salt [2(C5H6N2Cl)+], [CuCl4]2? complex of copper(II) has been synthesized and characterized. The X-ray diffraction analysis with a single crystal of this compound showed that the title compound (4-amino-2-chloropyridinium)2CuCl4 [(CAP)2CuCl4], crystallized at room temperature in the monoclinic system, space group C2/c (N°.15) and the following : a = 16.0064 (2) Å; b = 7.7964 (10) Å; c = 14.7240 (2) Å; β = 102.497 (10)°; V = 1793.91 (4) Å3 and Z = 4. The structure was solved by using 1,589 independent reflections down to R value of 0.021. The unit cell is made up of tetrachlorocuprate(II) anions and 4-amino-2-chloropyridinium cations linked together by an extensive hydrogen bond network of types N–H···Cl (N: pyridinium) and N–H···Cl (N: amine), and cation-lone pair of nitrogen element interactions. Solid state NMR spectra showed one and five isotropic resonances, 63Cu and 13C, respectively, confirming the solid state structure determined by X-ray diffraction. Impedance spectroscopy study, reported for single crystal, revealed that the conduction in the material was due to a hopping process. This work aims to reveal the thermal properties of a new copper(II) based organic–inorganic hybrid and the conductivity properties that these compounds exhibit.  相似文献   

9.
A novel –M–X–M–X– type infinite chain 1D copper(II) complex of Eflornithine, Dichloro-[2-amino-5-ammonio-2-(difluoromethyl)pentanoate]copper(II) hydrate, [Cu(C6H12F2N2O2)Cl2]·H2O 1 has been synthesized and characterized by elemental analysis, spectroscopic techniques (UV/Vis and FT-IR), TGA and X-ray diffraction. Single-crystal X-ray diffraction analysis of the complex 1 showed the structure to be monoclinic with space group Cc, a = 13.1295(15) Å, b = 12.1859(14) Å, c = 8.1927(9) Å, β = 118.359(3) Å, V = 1153.5(2) Å3, Z = 4. The complex exhibits a quadratic planar coordination of the Cu-atom. The Cu(II) centre is coordinated by two chloride atoms, an oxygen atom of the carboxyl- and a nitrogen atom of the amino-group, respectively, forming a quadratic planar geometry. The terminal amino group of the ligand is protonated to form NH3 + while the carboxylic moiety is deprotonated to form Zwitterionic eflornithine ligand, with the coordination of the metal at the nitrogen atom of the second amino group. The compound has –M–X–M–X– infinite 1D chain polymeric structure. Two neigbouring Cu(EFL)Cl chain units are bridged by an Cl? ion, forming a –Cu–Cl–Cu–Cl– linear chain structure along C-axis. The antibacterial activities of the complex on Escherichia coli (E. coli), Staphylococcus aureus (S. aureus) and Pseudomonas aeruginosa (P. aeruginosa) were investigated and found to be active at higher concentration than the parent ligand.  相似文献   

10.
This paper presents the synthesis, crystal structure and spectroscopic properties of a novel half-sandwich mononuclear cobalt(III) complex with hydrotris(3,5-dimethylpyrazolyl)borate ligand and thiocyanate [Tp*Co(Hpz*)(NCS)2]·H2O·CH3OH (Tp*: hydrotris(3,5-dimethyl- pyrazolyl)borate, Hpz*: 3,5-dimethylpyrazole). The structure was determined by X-ray diffraction. The complex crystallizes in the monoclinic system, space group Cc, a=18.591(6) Å, b=10.536(3) Å, c=17.568(5) Å, β=11.284(5)°, Z=4, R1=0.0501, wR2=0.1179. The cobalt(III) ion in the complex is six-coordinated with nitrogen atoms, three from Tp*, two from pyrazole and two from two thiocyanates, to form octahedral environment. The hydrogen atoms of O(2) of water molecule are connected by hydrogen bonds with S atoms of two adjacent complex molecules to form 1-D chains. The hydrogen atom of N(8) of complex molecule is connected by hydrogen bond with methanol. The spectroscopic results are consistent with the crystallographic study.  相似文献   

11.
Anhydrous ammonium pentaborate NH4B5O8 has been synthesized by thermal dehydration of larderellite NH4[B5O7(OH)2] · H2O at a temperature of 290°C for 7 h. The crystal structure has been determined from the X-ray powder diffraction data: a = 7.58667(5) Å, b = 12.00354(8) Å, c = 14.71199(8) Å, R p = 6.23, R wp = 7.98, R B = 12.7, R F = 8.95, and β-KB5O8 structure type. The double interpenetrating framework is formed by pentaborate groups, each consisting of a boron-oxygen tetrahedron and four triangles, in which all oxygen atoms are bridging. The thermal behavior of the NH4B5O8 compound has been investigated using thermal X-ray diffraction. As for other pentaborates of this type, the thermal expansion of the NH4B5O8 compound is anisotropic and reaches a maximum along the a axis. The thermal expansion coefficients are as follows: α a = 39 × 10?6, α b = 6 × 10?6, α c = 20 × 10?6, and α V = 65 × 10?6 °C?1.  相似文献   

12.
A new copper(II) molybdenum(VI) arsenate(III), (C5H5NH)2(H3O)2[(CuO6)Mo6O18(As3O3)2], has been hydrothermally synthesized and characterized by single crystal X-ray diffraction and TG analysis. The compound crystallizes in the monoclinic space group P21/n with a=9.303(2), b=20.731(4), c=12.617(3) Å, β=104.17(3)°, V=2359.3(8) Å3, Z=2 and R1(wR2)=0.0296(0.0683). The structure is composed of pyridinium cations, proton hydrates and [(CuO6)Mo6O18(As3O3)2]4− polyanions. The polyanion framework derives from the Anderson type; the central octahedron is filled up by copper(II) and is capped on both sides by a cyclic As3O6 group.  相似文献   

13.
The reaction of EuOCl (EuCl3) with dibenzoylmethane (HDBM) in the presence of N-methylmorpholine yields a novel Eu5 square-pyramid polynuclear complex with a rare μ4-OH bridging mode, Eu54-OH)(μ3-OH)4(μ-DBM)4(DBM)6 (1). The compound was characterized by elemental analysis, IR, fluorescence and Mössbauer spectra as well as by an X-ray single crystal structure determination. Crystallographic data for 1, C150H115Eu5O25, monoclinic, P21/c, a=22.223(5), b=17.427(1), c=35.708(5) Å, β=100.11(2)°, V=13614(4) Å3, Z=4, R1=0.0979, wR2=0.1695.  相似文献   

14.
New ligand [KH2B(tz*)2] (tz*=3,5-dimethyl-1,2,4-triazolyl) has been synthesized and the reactions of two different metal salts (copper and zinc) with the new ligand in agar gave two similar crystalline polymorphic forms: [Cu{H2B(tz*)2}2(H2O)] (1) and [Zn{H2B(tz*)2}2(H2O)] (2). A single crystal X-ray study revealed that the compound 1 was the monoclinic system with space group C2/c and a=8.462(3) Å, b=14.039(6) Å, c=19.991(8) Å, β=94.622(7)°, Z=4, R1=0.0451, wR2=0.1110. And the compound 2 was the monoclinic system with space group C2/c and a=8.4214(4) Å, b=13.8765(7) Å, c=20.2969(6) Å, β=95.615(2)°, Z=4, R1=0.0667, wR2=0.1375. The metal(II) ion in the complex is five-coordinated with four nitrogen atoms which come from triazolyl and one oxygen atom which come from water molecular. In both compounds, the hydrogen atoms of water molecule are connected by hydrogen bonding with N atoms of two adjacent complex molecules to form 2-D planes. The spectroscopic results are consistent with the crystallographic study.  相似文献   

15.
The crystal structure and molecular conformation of 2,4,6-tricyano-4'-N,N-diethylaminoazobenzene (C19H16N6, mol. wt. 328.4a.m.u.) has been determined from X-ray diffraction data: monoclinic P21/c, a = 9.302(7)Å, b = 8.733(5)Å, c = 20.98(1) Å, β = 94.93(6)°, V = 1699(2)Å3, Z = 4, Dc = 1.284gem?3, F(000) = 688, λ(MoKα) = 0-71069Å, μ(MoKα) = 0.76cm?1. The structure was solved by MULTAN andrefined by full-matrix least-squares toR = 0.050 for 1358 independent observed reflections. The azobenzene skeleton is planar to within 0.12Å. Most significant bonding data are: NN, 1.286(4) Å; mean C-N (azo) 1.383(4) Å; mean C-C (cyano) 1.439(5) Å; mean CN 1.146(5)Å; NN-C, 112.8(2)° and 115.9(2)°; N-C-C (cis relative to NN) 127.6(2)° and 124.3(2)° ; N- C- C(trans) 115.2(2)° and 117.7(2)°.  相似文献   

16.
A new 14-membered hexazamacrocyclic copper(II) complex [Cu(H2L1)](ClO4)4(L1=1,8-bis(2-aminoethyl)-1,3,6,8,10,13-hexaazacyclotetradecane) has been prepared by the one-pot reaction of ethylenediamine and formaldehyde in the presence of the Cu(II) ion. The crystal structure of [Cu(H2L1)](ClO4)4 was determined by X-ray diffraction. It crystallizes in the triclinic space group P−1 with a=12.118(2) Å, b=12.438(2) Å, c=12.466(2) Å, α=102.26(1)°, β=112.82(1)°, γ=111.51(1)°, and Z=2. The coordination geometry around the copper(II) ions is axially elongated octahedral with four nitrogen atoms of the macrocycle [Cu–N 2.012(7) Å for Cu(1) and 2.013(6) Å for Cu(2), average value] and two oxygen atoms of two ClO4 anions [Cu–O=2.550 Å for Cu(1) and 2.601(6) Å for Cu(2)]. [CuL2](ClO4)2(L2=3,7-bis(2-aminoethyl)-1,3,5,7-tetraazabicyclo[3,3,2]decane) with a novel tetraazabicyclic ligand was obtained from the same reaction system as an additional product. Crystal structure of [CuL2](ClO4)2: monoclinic space group Cc, a=16.393(3) Å, b=8.8640(18) Å, c= 13.085(3) Å, β=105.01(3)°, and Z=4.  相似文献   

17.
The structure of 2,6-dichloro-4′-N,N-diethylaminoazobenzene has been determined from X-ray diffractometer data: C16H17Cl2N3, MW = 322·2, monoclinic, P21/n, a = 11·160 (2), b = 12·066 (2), c = 13·633 (3) Å, β = 116·46 (2)°, V = 1643·5 Å3, Z = 4, Dc = 1·30 g cm?3, F(000) = 672, λ(MoKα) = 0·71069 Å, μ(MoKα) = 3·94 cm?1. The structure was solved by direct methods and refined to R = 0·073 for 1495 independent reflexions. The molecule is non-planar with a dihedral angle of 87·8° between the phenyl rings. The effects of substituents on the aromatic ring geometry are discussed. Significant molecular parameters are: NN, 1·164 (9) Å; mean ClC, 1·741 (6) Å; mean CN(azo), 1·487 (9) Å; NNC, 112·4 (2)° and 109·1 (2)°; NCC (cis relative to NN), 125·5 (3)° and 122·4 (2)°; NCC (trans relative to NN) 114·0 (3)° and 119·5 (3)°; mean CC(Cl)C, 122·3 (3)°.  相似文献   

18.
A novel coordination polymer [Cd(l-trp) (d-trp)] n (where l-trp and d-trp are l-tryptophan and d-tryptophan or (S)-2-amino-3-(3-indolyl)propionic acid and (R)-2-amino-3-(3-indolyl)propionic acid) was prepared by a solvent-thermal method and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The compound(monoclinic space group P2(1)/c with a = 19.759(2) Å, b = 5.2496(10) Å, c = 9.7594(16) Å, β = 97.2760(10)°, Z = 2) shows a two-dimensional plane structure. The crystallized coordination polymer has a centrosymmetric space group. Each Cd2+ ion coordinates with a pair of racemes, and the complex is a mesomer. Although l-trp was used, both l-trp and d-trp appear in the complex.  相似文献   

19.
The structural and electrochemical properties of the double perovskite-type oxide, PrBaMnMoO6-δ, was investigated using neutron diffraction with in-situ conductivity measurement under a dry Argon atmosphere from 25 °C to 700 °C. A Rietveld refinement of the neutron diffraction data confirmed monoclinic symmetry in the P21/n space group. Rietveld refinement also confirms the unit cell parameters of a = 5.6567 (1) Å, b = 5.6065 (2) Å, c = 7.9344 (1) Å and β = 84.43° with reliable atomic positions and refinement factors (R-factors). Neutron diffraction data refinement shows two minor phases (<5%), an orthorhombic AB2O5 type phase of PrMn2O5 in the Pbam (No. 32) space group with unit cell parameters, a = 7.9672 (1) Å, b = 8.9043 (2) Å and c = 5.8540 (1) Å and a scheelite phase of BaMoO4 in the tetragonal I41/a (88) space group with the unit cell parameters, a = b = 5.9522 (1) Å, and c = 12.3211 (2) Å. Morphological images revealed a porous and intertwined microstructure. In-situ conductivity measurement shows that the total conductivity of this material was 130.84 Scm?1 at 700 °C.  相似文献   

20.
设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号