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1.
A binuclear zinc(Ⅱ) complex with 2-carboxycinnamic acid (2-ccm) and dipyrido- [3,2-a:2',3'-c]phenazine (DPPZ), {[Zn2(2-ccm)2(DPPZ)2]·2H2O}n, was synthesized and characterized by elemental analysis, IR, single-crystal X-ray diffraction, thermal gravimetry and fluo- rescent emission. It crystallizes in monoclinic, space group P21/c with a = 13.409(4), b = 25.530(7), c = 13.952(4) A, β = 99.554(3)°, V= 4710(2) A3, Z= 4, C56H36N8O10Zn2, Mr= 1111.67, Dc = 1.568 g/cm3, μ(MoKα) = 1.093 mm^-1, F(000) = 2272, R = 0.0422 and wR = 0.0895. In the crystal, the basic unit of 1 is a binuclear Zn2 entity which is linked by 2-ccm ligand to form a 1D double chain along the a axis. The O-H...O hydrogen bonding and π-π interactions lead to a 3D supramolecular motif. In addition, thermal and luminescent properties of complex 1 have also been investigated.  相似文献   

2.
A new binuclear copper complex, [Cu2L2(pht)2]2·H2O(Hpht = 5,5-diphenylhydantoin, i.e. phenytoin; L = 2-diethylaminoethanol), has been synthesized by the solvothermal method, and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group C2/c with a = 31.918(3), b = 12.9222(15), c = 19.868(2) , β = 98.762(2)o, V = 8098.8(16) 3, Dc = 1.429 Mg/m3, Z = 4, F(000) = 3640, μ = 1.107 mm-1, R = 0.0560 and wR = 0.1276(I 2(I)). Each copper(Ⅱ) in a molecule is coordinated with N and O atoms from ligand L and N atom from ligand Hpht in a tetradentate manner. Moreover, two copper(Ⅱ) centers are bridged by two O atoms of hydroxyl groups from two L ligands to form a slightly distorted binuclear {Cu2O2} diamond configuration. In addition, the interaction of this complex with calf thymus DNA(CT-DNA) was investigated by UV-vis spectrum and viscometry, and the complex may bind to DNA through intercalation.  相似文献   

3.
LI Wen-Hui   《结构化学》2007,26(9):1053-1056
The title azide-bridged dinuclear Schiff base zinc(Ⅱ) complex [Zn2(C12H16N3O3)2-(μ1,1-N3)2] was prepared and characterized by elemental analysis, IR spectrum, and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group F21/n with a = 8.736(2), b = 14.850(3), c = 11.775(2) (A), β = 102.42(3)°, V= 1491.8(5) (A)3, Z= 2, Dc = 1.593 g/cm3, Mr = 715.36, λ(MoKα) = 0.71073 (A), μ = 1.669 mm-1, F(000) = 736, the final R = 0.0338 and wR = 0.0789. A total of 3411 unique reflections were collected, of which 2777 with Ⅰ>2σ(Ⅰ) were observed. The molecule of the complex is located on a crystallographic inversion centre. Each Zn atom in the complex is five-coordinated by one Schiff base ligand and two bridging azide groups, forming a trigonal bipyramidal configuration. The Zn…Zn distance is 3.328(2) (A). In the crystal structure, molecules are linked through intermolecular C-H…N hydrogen bonds, forming layers parallel to the bc plane. The complex shows low cytotoxic property to both normal and carcinoma cells.  相似文献   

4.
A novel metal-organic framework, namely [Zn(C20H13O5P)]n(1), has been hydrothermally synthesized through the reaction of 5-(oxidediphenylphosphino)isophthalic acid(H2L) with Zn(Ⅱ) salt. The title compound crystallizes in monoclinic, space group P21/c with a = 11.0966(10), b = 14.5651(14), c = 14.7311(15), β = 130.022(6)o, C20H13O5 PZn, Mr = 429.64, V = 1823.3(3) 3, Dc = 1.565 g/cm3, F(000) = 872, μ = 1.463 mm-1, S = 1.054 and Z = 4. The final R = 0.0270 and wR = 0.0739 for 2769 observed reflections with I 2σ(I). In the title complex, the Zn2(CO2)2 binuclear clusters are linked by L2- ligands to result in a pillared layer structure in the bc plane, which is a(4,4)-net composed of helical chains with opposite chirality by sharing Zn2(CO2)2 units. Adjacent layers are further associated together through Zn–O bonds involving the metal center and the oxygen atom of P=O group to achieve a 3D architecture, in which one-dimensional quadrangled channel displays the interweaving of two pairs of coaxial double-helical chains with opposite chirality. The luminescence property and thermogravimetric analysis of the title complex were investigated.  相似文献   

5.
韩晶  李婷  李冰 《结构化学》2015,(2):253-259
A new energetic complex, Ni(3,4'-Hbpt)2(Hoba)2(H2O)2(3,4'-Hbpt = 3-(3-pyridyl)-5-(4'-pyridyl)-1-H-1,2,4-triazole and H2 oba = 4,4'-oxybis(benzoic acid)), has been synthesized by hydrothermal reaction and characterized by elemental analysis, IR spectroscopy, single-crystal X-ray diffraction, thermogravimetric analyses and X-ray powder diffraction. Single-crystal X-ray diffraction analysis indicates that the complex belongs to the monoclinic system, space group P21/c with a = 10.2357(9), b = 24.594(2), c = 10.4225(9) A, β = 114.0110(10)°, V = 2396.7(4) A3, Dc =1.460 g/cm3, μ = 0.482 mm-1, Mr = 1053.63, F(000) = 1088, Z = 2, the final R = 0.0358 and wR =0.0973 with I 2σ(I). Both 3,4'-Hbpt and H2 oba ligands adopt monodentate modes linking one Ni(II)ion to form a 0D motif. Furthermore, the 0D motifs are linked into a 3D supramolecular architecture with hydrogen bonds. In addition, the catalytic performance for thermal decomposition of the efficacy of ammonium perchlorate(AP) is explored by differential scanning calorimetry(DSC),which indicates that the complex is a good candidate for a promoter of the thermal decomposition of ammonium perchlorate.  相似文献   

6.
One binuclear sodium(Ⅰ) complex [Na2(2-benzoylbenzoato)4(Phen)2(H2O)2]·H2O has been synthesized with 2-benzoylbenzoic acid and 1,10-henanthroline as ligands. The crystal structure was determined by X-ray diffraction. The crystal belongs to the triclinic system with space group P , a = 1.08096(8), b = 1.09619(8), c = 1.09740(8) nm, α = 79.0600(1), β = 71.0450(1), γ = 62.0540(1)o, V = 1.08533(1) nm3, Dc = 1.421 g/cm3, Z = 2, F(000) = 484, GOOF = 1.036, the final R = 0.0363 and wR = 0.0961. The crystal structure shows that two neighboring sodium(Ⅰ) ions are linked together by two bridging water molecules, and each end position is coordinated with one 1,10-phenanthroline molecule and one 2-benzoylbenzoato to form a binuclear structure. Each sodium(Ⅰ) ion in the molecule is coordinated with five atoms to give a distorted trigonal bipyramid. The fluorescence property of the title complex is also discussed.  相似文献   

7.
TANG  Shi-Di DENG  Yuan-Fu FU  Zhi-Yong 《结构化学》2010,(11):1666-1671
A new heterobimetallic nitrilotriacetatoperoxotitanate complex with the formula of [Mn(H2O)5]2[Ti(O2)2O(nta)2]·7H2O (1, C6H6O6N = H3nta) has been isolated in pure crystals. It was characterized by elemental analyses, IR, thermal analysis (TGA) and single-crystal X-ray diffraction. Complex 1 crystallizes in monoclinic, space group C2/c with a = 15.088(3), b = 13.311(3), c = 17.741(4) , β = 100.92(3)°, Z = 4, V = 3498.6(12) 3, Mr = 968.19, Dc = 1.838 g/cm3, μ = 1.266 mm-1, F(000) = 1992, R = 0.0337 and wR = 0.0819. Single-crystal X-ray analysis reveals that the titanium atom is N,O,O',O'-chelated by the nitrilotriacetate and O,O'-chelated by the peroxo group, and is coordinated to the bridging O atom in an overall pentagonal-bipyramidal geometry. The manganese ions in the compound are both 6-coordinated by five water molecules and one bridged carboxylato oxygen atom. A decameric water cluster consisting of a cyclic water hexamer in a boat fashion is also found in complex 1. The TGA and XRD results prove that 1 undergoes facile thermal decomposition to form the mixture of Mn2O3 and TiO2 at 600~800 ℃, and pure MnTiO3 at 900 ℃.  相似文献   

8.
A new Co(II) metal-organic coordination polymer based on flexible bis(imidazole) and aromatic dicarboxylate co-ligands, namely [Co(bix)(nph)]n(H2nph = 3-nitrophthalic acid, bix = 1,4-bis(imidazole-1-ylmethyl)benzene), has been hydrothermally synthesized and characterized by elemental analyses, TG, IR spectroscopy and single-crystal X-ray diffraction. It crystallizes in the triclinic space group P1 with a = 9.3767(14), b = 10.1451(15), c = 12.1488(17), α = 102.6450(10), β = 108.856(2), γ = 98.807(2)°, V = 1035.3(3)3, Z = 2, C22H17 Co N5O6, Mr = 506.34, Dc = 1.624 g/cm3, μ = 0.882 mm-1 and F(000) = 518. In the complex, the nph2- ligands connect neighbouring cobalt atoms to form binuclear [Co(nph)]2 subunits, which are linked by pairs of bix ligands to form a 2D honeycomb-like(6,3) network. In addition, the compound is further extended into a 3D supramolecular architecture by π···π stacking interactions. Moreover, the luminescence and catalytic properties of the complex are investigated.  相似文献   

9.
The title phenolic oxygen bridged dinuclear Schiff base zinc(Ⅱ)complex [Zn2Br2-(C15H14BrN2O)2]was synthesized and characterized by elemental analysis and single-crystal X-ray diffraction.The crystal belongs to the trielinic system,space group P-1 with a=9.2279(17),b=12.096(2),c=16.286(3)(A),α=75.402(3),β=87.464(3),γ=72.746(3)°,V=1679.1(5)(A)3,Z=2,Dc=1.833 g/cm3,Mr=926.94,λ(MoKα)=0.71073(A),μ=6.221 mm-1,F(000)=904,the final R=0.0601 and wR=0.1155.A total of 7453 unique reflections were collected,of which 3425 with Ⅰ>2σ(Ⅰ)were observed.One Zn atom is six-coordinate in an octahedral geometry,and the other one is four-coordinate in atetrahedral geometry.The Zn…Zn distance is 3.106(2) (A).In the crystal structure,molecules are linked through intermolecular hydrogen bonds typed N-H…Br and C-H…Br,forming zigzag chains running along the b axis.The complex shows potent cytotoxic property to both normal and cardnoma cells.  相似文献   

10.
A new coordination polymer, namely [Zn(pdc)(bbi)]n {H2 pdc = 2,3-pyridine dicar- boxylic acid, bbi = 1,1-(1,4-butanediyl)bis(imidazole)}, has been prepared under hydrothermal conditions and characterized by elemental analysis, IR, and single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21 /n with a = 8.436(3), b = 16.988(5), c = 12.106(4), β = 92.204(5)°, V = 1733.6(9)3, Z = 4, C17 H17 N5 O4 Zn, Mr = 420.73, Dc = 1.612 g/cm3, F(000) = 864, μ(MoKa) = 0.452 mm-1, the R = 0.0672 and wR = 0.1645. In the mononuclear complex, each Zn(II) is five-coordinated by one carboxylate O and one pyridyl N atoms from one pdc anion, one carboxylate O atom from another pdc anion, and two N atoms from two bib ligands. The Zn(II) ions are connected by pdc ligands to form skeleton chains, and bbi ligands further link them to construct a 2D framework. The thermal and luminescence properties of the complex were also investigated.  相似文献   

11.
A novel NiⅡ complex {[Ni(IBG)(μ-H2O)(H2O)2]·2H2O}n 1(H2IBG = isophthaloylbisglycine) has been synthesized and characterized by single-crystal X-ray diffraction,elemental analysis,IR spectra,and thermogravimetric analysis.It crystallizes in monoclinic,space group P2/c with a = 15.40(2),b = 6.960(10),c = 7.865(11) ,β = 90.32(3)o,V = 843(2) 3,Z = 2,C12H18NiN2O11,Mr = 424.99,Dc = 1.675 g/cm3,F(000) = 440,μ(MoKα) = 1.214 mm-1,the final R = 0.0514 and wR = 0.1247 for 1078 observed reflections with I 2σ(I).In the structure,each NiⅡcenter is situated in the center of a rather regular octahedron.Moreover,thermal stability has been studied and magnetic measurements show antiferromagnetic interactions for this complex.  相似文献   

12.
A new tetranuclear zinc(II) complex [Zn4(SO4)2(DPPZ)4(HSal)2(OH)2] 1 (DPPZ = dipyrido[3,2-a:2',3'-c]phenazine, H2Sal = salicylic acid) was prepared by using hydrothermal synthesis and characterized by elemental analysis, IR spectrum, thermal gravimetry (TG), fluorescent emission and single-crystal X-ray diffraction. Its crystal structure is of monoclinic, space group P2 1/c with a = 9.8897(8), b = 14.2506(12), c = 26.384(2) ,A, β = 94.8940(10)°, V = 3704.8(5) A3 Z = 2, C86H52N16O16S2Zn4, Mr = 1891.04, Dc = 1.695 g/cm^3, μ= 1.423 mm^-1, F(000) = 1920, GOOF = 1.039, the final R = 0.0358 and wR = 0.0872 for 6038 observed reflections with I 〉 2σ(I). In 1, "cage-like" tetranuclear clusters of [Zn4(SO4)2(DPPZ)4(HSal)2(OH)2] are further stacked through π-π interactions to generate a 3D supramolecular network.  相似文献   

13.
A new mixed-ligand nickel(Ⅱ) complex, [Ni(L)(DCA)(H2O)]·2H2O (L = C8H9N3, 2-aminomethyl-benzimidazole, DCA2- = 7-oxabicyclo[2,2,1]heptane-2,3-dicarboxylate, demethylcantharate, C8H8O5), has been synthesized and characterized. The structure of the complex was determined by single-crystal X-ray diffraction. It is of monoclinic system, space group P21/c with a = 7.7211(7), b = 12.0799(12), c = 19.7867(19), β = 100.390(6)°, V = 1815.2(3) nm3, Dc = 1.625 g·cm-3, Ζ = 4, F(000) = 928, R = 0.0314 and wR = 0.0822. In addition, the interaction between the complex and DNA was studied by means of fluorescence spectra and viscosity. The results indicate that the complex binds to DNA by the mode of partial intercalation with the Stern-Volmer constants Ksv of 3.81 × 104 mol·L-1.  相似文献   

14.
A new Schiff base Dibenzoyl-bissemicarbazone C15H16N6O2(L) and its complex with neodymium(Ⅲ ) perchlorate [NdL2(H2O)2](ClO4)3 were synthesized. The crystal and molecular structure of the title complex were determined by single crystal X-ray diffraction. The crystal is monoclinic and conforms to space group P. with cell constants a=10. 893(2) A, b= 12. 118(3) A , c=22. 494(5) A , β=89. 86(3)% V = 2969.19A3. The final standard deviation R=0. 0919. In the complex Nd is coordinated by four nitrogen and six oxygen atoms, of which four nitrogen and four oxygen atoms are provided by two neutral ligands L, and the other two oxygen atoms are provided by two water molecules, forming a ten-coordinated complex cation, which the perchlorate groups exist in the outer sphere. The coordination polyhedron takes a bicapped anti-square prism arrangement. That the average bond length of Nd-N is 2. 735 A indicates that the coordination of N in groups to Nd( Ⅲ ) is very weak.  相似文献   

15.
The title azide-bridged dinuclear Schiff base zinc(Ⅱ) complex [Zn2(C12H16N3O3)2-(μ1,1-N3)2] was prepared and characterized by elemental analysis, IR spectrum, and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group F21/n with a = 8.736(2), b = 14.850(3), c = 11.775(2) (A), β = 102.42(3)°, V= 1491.8(5) (A)3, Z= 2, Dc = 1.593 g/cm3, Mr = 715.36, λ(MoKα) = 0.71073 (A), μ = 1.669 mm-1, F(000) = 736, the final R = 0.0338 and wR = 0.0789. A total of 3411 unique reflections were collected, of which 2777 with Ⅰ>2σ(Ⅰ) were observed. The molecule of the complex is located on a crystallographic inversion centre. Each Zn atom in the complex is five-coordinated by one Schiff base ligand and two bridging azide groups, forming a trigonal bipyramidal configuration. The Zn…Zn distance is 3.328(2) (A). In the crystal structure, molecules are linked through intermolecular C-H…N hydrogen bonds, forming layers parallel to the bc plane. The complex shows low cytotoxic property to both normal and carcinoma cells.  相似文献   

16.
The title complex, [Ce(BA)3phen]2 (BA = benzoate, phen = 1,10-phenanthroline),was prepared by the reaction of Ce(NO3)3·6H2O, benzoic acid and 1,10-phenanthroline. The complex was characterized by single-crystal X-ray diffraction, elemental analysis, IR spectra and TG-DTG techniques. The results show that the crystal is of triclinic, space group P(1) with a =10.912(2), b = 11.962(3), c = 12.474(3)(A), a = 104.889(3), β = 93.523(3), γ = 113.332(3)°,C66H46Ce2N4O12, Mr = 1366.90, V= 1420.2(6) (A)3, Z = 1, Dc = 1.598 g/cm3,μ = 1.652 mm-1, S =1.024 and F(000) = 682. The final R = 0.0391 and wR = 0.0947 for 4878 observed reflections with I > 2σ(1). The structure of the title complex consists of two Ce(C6H5COO)3(C12H8N2) units,forming a binuclear molecule. Each Ce(Ⅲ) is coordinated by two O atoms of one bidentate chelating carboxylate group, five O atoms of two bidentate bridging and two tridentate chelating-bridging carboxylate groups, and two N atoms of one 1,10-phenanthroline molecule to complete a distorted monocapped square antiprism geometry. Its thermogravimetric analysis was determined by TG-DTG techniques.  相似文献   

17.
A novel binuclear Cu(Ⅱ)complex[Cu(paba)C1](pabaH=2-(2-pyridylmethylimine)benzenesulfonic acid)has been synthesized and characterized by elemental analysis,IR andsingle-crystal X-ray diffraction.The crystal of the title complex crystallizes in a monoclinie system,space group P21/n,with a=6.8165(7),b=15.3073(16),c=12.3795(13)(A),β=95.0160(10)°,V=1286.8(2)(A)3,Mr=360.26,Dc=1.860 g/cm3,μ=2.074 mm-1,F(000)=724,Z=4,the final R=0.0252 and wR=0.0675 for 2395 observed reflections with I>2σ(I).The title complex is centrosymmetric and a pair of chlorides act as μ2-bridges to link two Cu(Ⅱ)ions forming a binuclear complex.Every Cu(Ⅱ)ion is five-coordinated by pyridyl N,imine N and sulfonate O atoms of the tridentate paba ligand as well as two bridging Cl-,constructing the distorted square-pyramidal geometry.In the structure extensive hydrogen bonds and weak π-π stacking stabilize the solid structures,through which the complex builds its 3-dimensional supramolecular structure.  相似文献   

18.
A new coordination polymer [Ni(L)(m-bix)(H2O)]n(1, H2L = 5-iodo-isophthalic acid, m-bix = 1,3-bis(imidazol-1-ylmethyl)-benzene) has been synthesized by the hydrothermal method and characterized by IR, elemental analysis, powder XRD and single-crystal X-ray analysis. The crystal is of triclinic, space group P1 with a = 9.1638(3), b = 10.2319(3), c = 13.2463(4) ?, α = 80.1710(10), β = 83.671(2), γ = 70.3790(10)o, C22H19NiIN4O5, Mr = 605.02, V = 1150.85(6) ?3, Dc = 1.746 g/cm3, F(000) = 600, μ = 2.225 mm-1, S = 1.045 and Z = 2. The final R = 0.0388 and wR = 0.1257 for 5089 observed reflections with I 2σ(I). In the title complex, the M and P layers are arranged alternately to give a double-layer structure by the symmetry related hydrogen bonds, and these double-layers are further joined together to achieve a 2D supramolecular architecture through I···π interaction involving iodine atoms and imidazole rings. The thermal stability of the title complex was studied by thermal gravimetric(TG) and differential thermal analysis(DTA).  相似文献   

19.
A new energetic compound based on the tetrazole-1-acetic acid (tza) and potassium(I) salt, K2(tza)2(H2O), was synthesized and characterized by elemental analysis and FT-IR spectrum. Its crystal structure was determined by single-crystal X-ray diffraction analysis. The results show that the crystal belongs to the orthorhombic system, space group Pna21 with a = 1.11972(17) nm, b = 0.46647(7) nm, c = 2.5158(4) nm, V = 1.3140(3) nm3, K2C6H8N8O5, Mr = 350.40 g·mol-1, Dc = 1.771 g·cm-3, μ(MoKα) = 0.759 mm-1, F(000) = 712, Z = 4, R = 0.023 and wR = 0.0527 for 2961 observed reflections (I > 2σ(I)). The K(I) cation is six-coordinated with four O atoms from three carboxylate groups, one O atom from one H2O molecule and one N atom from tetrazolyl ring, in which each tza is coordinated in a tridentate chelating bridging coordination mode. The thermal decomposition mechanism of the title complex was studied by DSC and TG-DTG techniques. Under nitrogen atmosphere at a heating rate of 10 K·min-1, the thermal decomposition of the complex contains one main exothermic process between 191.7 and 243.8 ℃ in the DSC curve. Its combustion heat was mensurated by oxygen bomb calorimetry. The non-isothermal kinetics parameters were calculated by the Kissinger's method and Ozawa-Doyle's method, respectively. The sensitivity properties of K2(tza)2(H2O) were also determined with standard methods, which was very sensitive to flame.  相似文献   

20.
One novel binuclear copper(Ⅱ) complex [Cu 2 (Hpt) 2 (CO 3) 2 (H 2 O) 2 ]·H 2 O with copper carbonate and 3-(pyridin-2-yl)-1,2,4-triazole (Hpt) was hydrothermally synthesized and characterized by IR and X-ray diffraction analysis.The complex crystallizes in triclinic,space group P2 1 /n with a=0.6862(1),b=0.7805(1),c=1.1983(2) nm,α=72.03(2),β=107.72(3),γ=75.28(2)o,V=0.5884 nm 3,D c=2.105 g/cm 3,Z=1,F(000)=357,GOOF=1.041,the final R=0.01859 and wR=0.04348.The whole molecule is composed of two cooper ions,two Hpt molecules,two carbonate and three water molecules,forming a binuclear structure.The crystal structure shows that the cooper ion is coordinated with three nitrogen atoms from two Hpt molecules,two oxygen atoms from one carbonic acid and one water molecule,forming a distorted square pyramidal geometry.The TG analysis result shows that the title complex is stable under 131.0 ℃.  相似文献   

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