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1.
《结构化学》2020,39(8):1475-1482
A new Cu(Ⅱ) coordination polymer,{[Cu_3(oba)_2(μ~3-OH)_2(H_2O)_2].6H_2O}_n(H_2 oba=4,4'-oxydibenzoic acid),was synthesized by the solvothermal route and characterized by IR,TGA and XRD.The complex crystallizes in the monoclinic system,space group P2_1/c with a=5.957(6),b=29.746(3),c=9.351(7) A,β=125.709(4)°,V=1345.4(2) A~3,Z=2,C_(28)H_(36)Cu_3O_(20),M_r=883.09,D_c=1.913 g/cm~3,F(000)=782,μ=2.427 mm~(-1),R=0.0780 and wR=0.1688 for 3120 observed reflections with I 2σ(I).The complex forms a 3D framework based on rare infinite rod-shaped secondary building units(SBUs),and C-H…π interactions play an important role in stabilizing the 3D supramolecular architecture.It shows excellent catalytic activities for the degradation of safranin O(SO) and methylene blue(MB) dyes in aqueous solution under UV light irradiation.Furthermore,the apparent rate constants have also been investigated.  相似文献   

2.
A new cobalt complex with flavonoid carboxylate ligand was synthesized and characterized. X-ray diffraction data revealed that the compound crystallizes in the monoclinic crystal system, space group P2_1/c with a = 7.936(3), b = 21.475(7), c = 20.010(7) ?, β = 102.856(14)o, V = 3325(2) ?~3, Z = 4, C_(34)H_(32)CoO_(15), M_r = 739.53, D_c = 1.477 g/cm~3, F(000) = 1532, μ = 0.591 mm~(-1), R = 0.1123 and w R = 0.1419. In the crystal structure, the Co(Ⅱ) shows 6 coordination geometry, and the flavonoid ligand coordinated with the Co(Ⅱ) ion in a monodentate mode. Hydrogen bonding interactions and π-π stacking interactions lead to the three-dimensional stacking of crystal and increase its stability. Moreover, the thermal stability and luminescent properties of the complex are also investigated. The fluorescence of the complex shows a great reduction of the intensity than that of the ligand.  相似文献   

3.
《结构化学》2020,39(5):918-926
A new dinuclear copper(Ⅱ) compound [Cu_2(CH_3COO)_2(L)_2(H_2O)_2]·4H_2O(1, HL = 4-pyridyl-NH-1,2,3-triazole) has been synthesized and characterized. Single-crystal X-ray diffraction showed that complex 1 crystallizes in monoclinic space group P2_1/c with a = 0.8427(1), b = 1.0981(1), c = 1.3610(1) nm, β = 93.364(4)°, V = 1.2573(1) nm~3, M_r = 643.56, Z = 2, D_c = 1.700 g/cm~3, μ = 1.760 mm~(-1), R = 0.0376, wR = 0.0981, and possesses a planar Cu_2N_4 six-membered ring, in which both Cu(Ⅱ) ions are bridged by two 1,2,3-triazole ligands. The neighboring dinuclear molecules are bound by strong intermolecular hydrogen bonds to create 1-D chains expanding along the b axis, which further form a 3-D supramolecular framework. Magnetic susceptibility measurement indicated the presence of weak antiferromagnetic interactions within the complex. The best fit using spin Hamiltonian yields the magnetic coupling constant J = –14.82 cm~(-1) above 30 K. The magnetic data are compared to those obtained for related double diazine bridged dinuclear copper(Ⅱ) complexes and magnetostructural correlations are discussed.  相似文献   

4.
Two new copper complexes based on pyrazole-3-carboxylic acid(H_2pca)ligand,Cu(Hpca)_2(H_2O)_2·2H_2O(1)and Cu_2(pca)_2(H_2O)_4(2)have been synthesized and fully characterized by single-crystal X-ray diffraction(SXRD),infrared spectroscopy(IR),thermal gravity analysis(TGA),powder X-ray diffraction(PXRD)and elemental analyses.Complex 1 is mononuclear while complex 2 shows a dinuclear structure.Complex 1 crystallizes in the monoclinic system,space group P2_1/c with Z=2,a=6.5591(5),b=21.696(2),c=4.9486(2)?,V=680.94(9)?~3,F(000)=366,D_c=1.745 g/cm~3,μ=1.650 mm~(-1),the final R=0.0340 and w R=0.0792.Complex 2crystallizes in the monoclinic system,space group P2_1/n with Z=2,a=5.1935(4),b=9.6052(7),c=12.7347(9)?,V=634.44(8)?~3,F(000)=420,D_c=2.195 g/cm~3,μ=3.404 mm~(-1),the final R=0.0305 and w R=0.0653.The three-dimensional frameworks of two complexes are formed by the O-H···O and N-H···O hydrogen bonding interactions.Notably,two copper complexes are further used as catalysts in the oxidation of alkylbenzenes using t-butylhydroperoxide(TBHP)as the oxidant and they exhibit excellent catalytic performance(Conv.up to 98.9%,Sele.up to 98.7%).  相似文献   

5.
Treatment of bis(2-dimethylaminoethyl) ether(BDMAE) with nickel acetate afforded a novel 3D nickel(Ⅱ) complex [Ni(BDMAE)(H_2O)_3·(CH_3COO)_2·(H_2O)_2] under solvothermal conditions. Its crystal structure was characterized by elemental analysis, IR spectrum, PXRD and single-crystal X-ray diffraction analysis. The complex belongs to the orthorhombic system, space group C2221 with a=8.823(2), b=13.932(3), c=17.563(4) ?, V=2158.9(8) ?~3, Z=4, C_(12)H_(36)N_2NiO_(10), Mr=427.14, Dc=1.314 g/cm~3, F(000)=920 and μ=0.944 mm~(-1). Single-crystal X-ray diffraction reveals that the mononuclear nickel(Ⅱ) ion is six-coordinated to one oxygen, two nitrogen atoms of the BDMAE ligand and three oxygen atoms of coordinated water molecules. The complex exhibits a 3D supramolecular structure through a variety of intermolecular and intramolecular hydrogen bonding interactions. In addition, the complex has been investigated for catalytic properties towards the Henry reaction of nitromethane with p-nitrobenzaldehyde, and the results indicated that the 1-p-nitrophenyl-2-nitroethanol product was obtained in excellent yield under optimum conditions with the complex as the catalyst.  相似文献   

6.
Reaction of 2-pyridone, copper acetate and terbium(or yttrium) perchlorate in acetone with the moleratio 6: 2: 1 results in the formation of heteronuclear complex Ln_2Cu_4L_8 (HL)_4 (OH)_2 (ClO_4)_4 (H_20)_(10)2CH_3COCH_3(Ln = Tb (1), Y (2)). By recrystallizing (1) in CHCl_3 single crystals were obtained and thestructure was determined by four-circle diffractometer. Data showed that the crystal is in space groupC2/m with a=27. 454(9)A, b=13, 608A, c=30. 556(11)A, β=99. 89(3)°, v=11245. 7(7. 5)A~3. Thestructure was solved by a combination of Patterson method and Fourier technique. The final R value is0. 103. In the structure, four copper and two terbium ions are bridged by 2-pyridone anions to form anessentially octahedral Cu_4Tb_2 core. The terbium atoms are each eight-coordinate and the copper atomsare five-coordinate.  相似文献   

7.
All attempts to prepare light lanthanide dicyclopeutadienyt chloride failed,due to the disproportionation reaction. The crystal complex of [(η~5-C_5H_5)_2NdCl.OC_4H_8]_2 was successfully prepared by the reaction of NdCl_3·2C_4H_8O with cyclopentadienyl sodium (molar ratio 1:1.8)in tetrahydrofuran at room temperatureThe composition of the title compound was determined by the methods of elemental analysis, infrared spectroscopy and photoelectron spectroscopy. The crystal structure of [(η~5-C_5H_5)_2NdCl·OC_4H_8]_2 was determined from single crystal X-ray diffraction. Data were collected at-60℃ under dry nitrogen atmosphere.The complex crystallizes in the monoclinic space group P2_1/c,with Z=2. Lattice parameters are: a=8.201(3), b=21.589(6),c=8.596(3),β=109.10(3)°.The structure was solved by Patterson and Fourier techniques and refined by least-squares to a final conventional R=0.0636 for 1680 reflections. There are two Nd atoms in the dimeric unit which are bridged asymmetrically by the two chlori  相似文献   

8.
A new complex Ir(ppy)_2(Hpda)(Hppy=2-phenylpyridine, H_2pda=pyridine-2,3-dicarboxylic acid) has been synthesized and characterized. According to single-crystal X-ray diffraction analyses, the title complex crystallizes in the monoclinic system, space group P21/n with a=8.5708(10), b=22.685(2), c=12.5722(15) ?, β=96.19(1)°, V=2430.2(5) ?~3, C_(29)H_(20)N_3O_4 Ir, Mr=666.22, Z=4, Dc=1.833 g/cm~3, F(000)=1304, μ=5.54 mm~(-1), λ(Mo Kα)=0.71073 ?, GOOF=1.02, the final R=0.049 and w R=0.119 for 4680 independent reflections with Rint=0.069. The title complex is of mononuclear structure. Intermolecular C–H···O hydrogen bonds and π-π stacking interactions result in the formation of a 3D supramolecular network. Photoluminescent spectra show that one intense emission band with the maximum of 516 nm can be observed in the title complex.  相似文献   

9.
A heterometal-organic framework {[Pr_2Ca(betc)_2(H_2O)_7]·H_2O}_n(1) was prepared by the hydrothermal reaction of 1,2,4,5-benzenetetracarboxylic acid(H4betc) with Pr(NO_3)_3 and CaCO_3, and further characterized by single-crystal X-ray structural analysis, elemental analysis, IR, thermal gravimetric, and X-ray powder diffraction. Complex 1 crystallizes in triclinic, space group P1 with a = 7.3668(12), b = 10.1726(14), c = 11.2264(15) ?, a = 100.404(2), b = 106.113(3), g = 109.158(3)o, V = 728.48(19) ?~3, Mr = 966.26, Z = 1, F(000) = 470, Dc = 2.203 g/cm~3, m(Mo Kα) = 3.585 mm~(-1), the final R = 0.0195 and w R = 0.0470(I 2s(I)). Complex 1 is a 3D network with pcu topology with 1D porosity and rich hydrogen-bonding interactions. The proton conductivity of complex 1 was also studied under ~97% relative humidity and the different temperature conditions.  相似文献   

10.
Two copper (Ⅱ) a-methacrylate complexes with benzimidazole, Cu [CH_2=C( CH_3)-COO]_2(C_7H_6N_2)_2(1) and Cu_2 [CH_2=C(CH_3)-COO]_4(C_7H_6N_2)_2 (2), have been prepared and characterized by elemental analyses, IR and electronic reflectance spectroscopies. The single crystal X-ray diffraction study of the two complexes shows that complex 1 has a square planar configuration, while complex 2 has a binuclear cage structure. The crystal structural analyses show that both complexes 1 and 2 are monoclinic, with space group P2_1/c, a=0.924 16(8) nm, b=1.233 02(13) nm, c =0.989 1(3) nm, β=91.912(13)°, D_c=1.386 g/cm~3, Z=2, R=0.033 9 for the former; and a=0.905 7(2) nm, b=2.252 1(5) nm, c=1.623 5(4) nm, β=90.11(2)°, D_c =1.411 g/cm~3 , Z=4, R=0.056 8, Cu-Cu=0.266 21 nm for the latter. Different structural types of complexes 1 and 2 were produced simultaneously in the reaction of copper (Ⅱ) α-methacrylate with benzimidazole in methanol solution. The forming mechanism of the complexes has been summarized.  相似文献   

11.
The crystal structure of one novel Mn(II) complex, [Mn(pmta)_3]_2[Mn(H_2O)_6]·4H_2O(1), is reported(Hpmta = 5-methyl-1-phenyl-1H-1,2,3-triazole-4-carboxylic acid). In the title compound, the asymmetric unit consists of a [Mn(pmta_)3]ˉ anion, half [Mn(H_2O)_6]~(2+) counter cation and two lattice H_2O molecules, and the intra- and intermolecular hydrogen bonds connect the complex into a supramolecular structure. The liquid-state fluorescence spectra of complex 1 have been determined. Hirshfeld surface analysis was also studied. The main intermolecular interactions in the complex are O···H and H···H contacts.  相似文献   

12.
A new tetranuclear silver(I) complex with the formula of [Ag_4(MMPzA)_2(dmPz)_4(H_2DPC)_2](H_2O)_4(1, MMPz A = mono(3,5-bimethyl-pyrazolmethyl)amine), dm Pz = 3,5-dimethylpyrazole, H_2DPC = pyridine-3,4-dicarboxylic acid) has been synthesized and characterized by single-crystal X-ray diffraction method. The title complex crystallizes in the triclinic system, space group P1 with a = 10.5532(13), b = 11.5071(18), c = 13.3951(17) ?, α = 97.3190(10), β = 106.7360(10), γ = 108.0770(10)o, V = 1438.3(3) ?3, Z = 1, Dc = 1.691 g/cm3, F(000) = 736, μ = 1.421 mm-1, the final R = 0.0400 and w R = 0.0942 for 5097 observed reflections(I 2σ(I)). The intermolecular hydrogen bonding interaction extends the complex into a 1D chain structure. In addition, the complex was tested in vitro for its antibacterial activity and it exhibited significant activity, especially against penicillium.  相似文献   

13.
The reaction of the reduced Schiff base HL(N-(4-hydroxybenzyl)-L-serine) with Zn(CH_3COO)_2·2H_2O in aqueous solution afforded [Zn(L)_2]·3H_2O(I). The complex has been characterized by elemental analysis, FT-IR, powder X-ray diffraction, electrospray ionization mass spectrometry and single-crystal X-ray diffraction. Complex I crystallizes in the orthorhombic system, space group P212121, with a=9.197(2), b=10.445(2), c=24.149(5) ?, V=2319.8(8) ?~3, Z=4, C_(20)H_(30)N_2O11 Zn, M_r=539.83, Dc=1.546 g·cm~3, μ=1.122 mm~(-1), F(000)=1128, GOOF=0.971, the final R=0.0206 and w R=0.0506 for 4346 observed reflections(I 2σ(I)). In complex I, each Zn(II) ion coordinates with three carboxyl oxygen atoms and two amine nitrogen atoms from three L-anions, forming a distorted five-coordinated trigonal bipyramidal geometry. Complex I exhibits a 1D wavy chain structure that is extended by hydrogen-bonding interactions to form a supramolecular network. The bioactivity of the complex as a potential PTPs inhibitor in vitro was investigated, displaying potent inhibition against PTP1B(IC_(50), 0.24 μM) and TCPTP(IC_(50), 0.53 μM) with a moderate selectivity.  相似文献   

14.
The compound(n-Bu_4N)_2[W_2Cu_4S_8(S_2CNC_4H_8)_2]was obtained by the reaction of Bu_4NBr,(NH_4)_2WS_4,NaS_2NCC_4H_8 and CuCl in CH_3CN and CH_3OH.It crystallizes in the monoclinicspace group P2_1/c with unit cell parameters:a=21.875(5),b=16.843(4),c=17.745(5),β=101.69(6)°,V=6402(6)~3,Z=4,D_o=1.718 g·cm~(-3).The final R and R_w values converged to 0.055and 0.060 respectively.The structure consists of two‘butterfly’units[WS_4Cu_2]linked togetherby two weak Cu—S bonds and two bridging S_2CNC_4H_8 ligands.Infrared spectra gave charac-teristic absorptions at 495 cm~(-1) for W=S and 450,435,412 cm~(-1) for W—μ-S.  相似文献   

15.
A new Zn(Ⅱ) complex [Zn(Phen)_2(C_(12)H_6O_4N_2)(H_2O)]·3H_2O with 2,2?-bipyridine-3,3?-dicarboxylic acid and 1,10-phenanthroline(Phen) as ligands was synthesized, and the crystal data are as follows: monoclinic, space group P2_(1/n), a=12.5581(11), b=17.3382(17), c=15.6687(14) ?, β=110.579(2)o, M_r=731.02, V=3193.9(5) ?~3, Dc=1.520 g/cm~3, Z=4, μ(Mo Kα)=0.833 mm~(-1), F(000)=1508, the final R=0.0431 and w R=0.0936. In the title complex, the central Zn(Ⅱ) ion is located in a distorted octahedral coordination environment. The electrochemical and fluorescent properties were studied. The title complex possesses irreversible electron transfer in the electrode reaction, and it has a strong emission peak in the range of 470~505 nm, with the excitation wavelength being 488 nm.  相似文献   

16.
A new complex, [Cu(HL)(phen)(H_2O)]·4H_2O(1, H_3L·HCl = 5-((4-carboxypiperidin-1-yl)methyl)isophthalic acid hydrochloride, phen = 1,10-phenanthroline), has been hydrothermally prepared and characterized by single-crystal X-ray diffraction, IR spectroscopy, elemental analysis and PXRD. Complex 1 crystallizes in monoclinic, space group P21/c with a = 14.5520(14), b = 12.6659(12), c = 15.5006(14) ?, β = 97.224(2)o, V = 2834.3(5) ?3, Z = 4, C27H33N3O11 Cu, Mr = 639.10, Dc = 1.498 g/cm~3, μ = 0.837 mm~(-1), S = 1.047, F(000) = 1332, the final R = 0.0423 and w R = 0.1118 for 18772 observed reflections(I 2σ(I)). The compound is a Cu(Ⅱ) centre mononuclear molecule in the asymmetric unit. The independent binuclear [Cu_2(HL)_2(phen)_2] units are bridged to form a three-dimensional(3D) supramolecular polymer by extensive hydrogen bonds and π-π non-covalent bonding interactions. Moreover, thermogravimetric(TG) analysis and gas adsorption property of 1 were also discussed.  相似文献   

17.
A new uranium(Ⅵ)-polycarboxylate framework with honeycomb(6,3) nets {[Zn(phen)_2(H_2O)_2][(UO_2)_2(BDC)_3]·2H_2O}n(1, BDC = benzene-1,4-dicarboxylate) was hydrotherrmally synthesized by the reactions of Zn(NO_3)_2·6H_2O with phenanthroine, UO_2(NO_3)_2·6H_2O and benzene-1,4-dicarboxylate. The complex was structurally characterized by FT-IR spectroscopy, powder XRD and X-ray single-crystal diffraction. Crystal data for 1: monoclinic, space group Cc with M_r = 1522.19, a = 14.9385(10), b = 20.4922(13), c = 15.9728(10) ?, β = 100.1240(10)°, V = 4813.5(5) ?~3, Z = 4, D_c = 2.100 g?cm~(–3), μ = 7.293 mm~(–1), F(000) = 2872, the final R = 0.0224 and w R= 0.0677 for 6522 observed reflections with I 2σ(I). Hydrogen bonds and π-π stacking interactions contribute to the structural extension and stabilization. Experimental band gap of about 3.57 e V indicates its broad gap semiconductor nature. UV-Vis spectra and solid-state luminescence were discussed in detail. The compound exhibits photocatalytic activities for the degradation of rhodamine B.  相似文献   

18.
QIN Bei 《结构化学》2012,31(8):1187-1193
A new asymmetric bidentate copper(Ⅱ) complex,CuL 2(HL=2-((E)-(4-bromophenylimino)methyl)-6-bromo-4-chlorophenol),has been synthesized and characterized by elemental analyses and single-crystal X-ray diffraction.The complex crystallizes in the monoclinic space group P2 1 /c with a=11.218(3),b=9.355(3),c=13.449(4),β=108.722(4)°,V=1336.8(6)3,Z=2,Dc=2.008 g/cm 3,μ(MoKα)=7.024 mm-1,F(000)=806,S=0.999,the final R=0.0342 and wR=0.0641for2611observed reflections (I>2σ(I)).The central copper(Ⅱ) is four-coordinate and bonds to two nitrogen and two oxygen atoms from two Schiff base ligands.The complex is linked into a two-dimensional supramolecular structure by weak intermolecular interactions.In addition,DNA-binding properties of the metal complex were investigated using spectrometric titrations and viscosity measurements.The results show that the complex binds with calf-thymus DNA(CT-DNA),presumably via a partial intercalative mode.The intrinsic binding constant of the Cu(Ⅱ) complex with DNA is 7.335×10 3 M-1.  相似文献   

19.
A novel copper(Ⅱ) complex derived from 1,4,7-triazacyclononane[CuL]_2(PF_6)_3×MeCN×H_2 O was synthesized and crystallographically characterized {L = 1,4-bis(2-carbamoylethyl)-7-benzimidazole-2-yl-methyl-1,4,7-triazacyclononane}. It crystallizes in triclinic, space group P1, with a = 13.2425(13), b = 14.0807(15), c = 17.6798(18), α = 86.296(2), β = 72.773(2), γ= 68.905(2)o, V = 2934.5(5) ?~3, Z = 2, D_c = 1.611 g/m~3, F(000) = 1456, M_r = 1423.09, m = 0.920 mm~(-1). The final R = 0.0671 and wR = 0.1874 for 6501 observed reflections with I 2σ(I). The structural analysis shows that the complex cation([CuL]_2~(3+)) was formed by two complex cations, namely([CuL~3]~(2+) and [CuL_(-H)~3]~+) through a hydrogen bond. In each complex cation, the Cu(Ⅱ) lies in a distorted square pyramidal geometry. The redox behavior was studied by cyclic voltammetry(CV) in aqueous solution which indicates a reversible one electron redox reaction. The result of UV absorption, ethidium bromide(EB) fluorescence spectra indicated that the complex binds to CT-DNA in an intercalative mode. Superoxide dismutase(SOD) activity of the complex was determined by photoreduction of NBT, and the value of IC_(50) is 5.22 μmol·L~(-1).  相似文献   

20.
Self-assembly reaction of 1,2,4,5-benzenetetracarboxylic acid(H_4 btc) with CuCl_2 in mixed N,N-dimethylformamide(DMF), methanol and aqueous solution at room temperature generated a 2D complex, [Cu(btc)_(0.5)(DMF)(H_2 O)]_n(1) which was further characterized by X-ray diffraction, IR spectrum, elemental analysis and TG-DTA experiments. The structure determination reveals that the fundamental unit of complex 1 contains one Cu(Ⅱ) ion, half a btc~(4–), one DMF molecule and one water molecule, forming a half paddlewheel-like building block [Cu_2(btc)(DMF)_2(H_2 O)_2] which is different from those previous Cu-btc(Ⅱ) polymers obtained either in water or other media without water. It crystallizes in monoclinic system, space group C2/c with a = 22.8209(14), b = 9.2244(6), c = 10.8876(7) ?, b = 117.5210(10)o, V = 2032.6(2) ?~3, Z = 2, C_8 H_(10) CuNO_6, M_r = 279.71, D_c = 1.828 g/cm~3, μ = 2.162 mm-1, F(000) = 1136, the final R = 0.0225 and wR = 0.0652 with I 2s(I). Furthermore, the thermal stability of complex 1 is observed to be dependent on the polymeric structure nature. And the luminescent measurements show that complex 1 produces strong emission at room temperature.  相似文献   

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