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1.
郁有祝  申艳红  吕垒  高盼  赵春普  李大成 《结构化学》2011,30(10):1393-1396
A new Mn2Ni2 cubane complex has been synthesized and characterized by single-crystal X-ray diffraction,FT IR spectra and elemental analysis.The title compound [MnIII2NiII2(hmp)4(N3)4(O2CR)2](hmp-is the anion of 2-pyridinemethanol and O2CR-is α-na-phthaleneacetate)crystallizes in the monoclinic system,space group P21/c with a = 10.519(5),b = 22.109(10),c = 23.235(9),β = 106.096(17)o,C48H42Mn2N16Ni2O8,Mr = 1198.28,V = 5192(4)3,Dc = 1.533 g/cm3,F(000)= 2448,μ = 1.258 cm1,Z = 4,the final R = 0.0875 and wR = 0.2020 for 3398 reflections with I > 2σ(I).X-ray diffraction analysis reveals that each Mn(III)center is octahedrally coordinated by two nitrogen atoms of azide anions and three oxygen atoms from three 2-pyridinemethanol anion ligands together with one oxygen atom from naphthaleneacetate.Each Ni(II)is octahedrally coordinated by two nitrogen atoms of 2-pyridinemethanol anion ligands as well as three oxygen atoms from three 2-pyridinemethanol anion ligands and one oxygen atom from naphthaleneacetate.  相似文献   

2.
A new Ni(II) complex, [Ni(ftsc)2NO3]NO3 (Hftsc=furan-2-carbaldehyde thiosemicarba-zone), has been synthesized and characterized by IR, UV spectra and single-crystal X-ray diffraction analysis. It crystallizes in a monoclinic system, space group P21/n, with a=10.5203(13), b=9.2094(11), c=20.829(3), β=91.518(2)°, V=2 017.3(5)3, Z=4, F(000)=1064, Dc=1.716 g/cm3, and wR= 0.0800. The complex contains a six-coordinated nickel(II) center which is bound to two imine nitrogen atoms and two thiolato sulfur atoms of two ligands as well as two oxygen atoms from a nitrate anion to assume a distorted octahedral coordination geometry. In addition, intermolecular N-H···O and C-H···O hydrogen bonds between adjacent molecules link the molecules together to form a three-dimensional structure.  相似文献   

3.
王凤武  魏亦军  朱其永 《结构化学》2007,26(11):1327-1331
A Schiff base zinc(Ⅱ) complex [Zn(C12H16BrClN2O)2(NCS)2] was prepared and characterized by elemental analysis,IR and single-crystal X-ray diffraction. The crystal belongs to the triclinic system,space group P1 with a=8.414(1),b=9.124(1),c=22.212(3),α=79.177(2),β=86.296(2),γ=89.899(2)o,V=1671.3(4)3,Z=2,Dc=1.631 g/cm3,Mr=820.79,λ(MoKα)= 0.71073,μ=3.444 mm-1,F(000)=824,R=0.0646 and wR=0.1179. A total of 7371 unique reflections were collected,of which 3904 with I > 2σ(I) were observed. The complex crystallizes with two half-molecules per asymmetric unit and each mononuclear molecule is centrosymmetric. The Zn atom lying at the inversion centre is six-coordinated in a slightly distorted octahedral geometry by two phenolate O atoms and two imine N atoms from two Schiff base ligands,as well as two N atoms from two thiocyanate anions. In the crystal structure,the combination of π-π stacking interactions and intermolecular hydrogen bonds (N–H…Br,N–H…O,N–H…N,C–H…O,C–H…S and C–H…Cl) leads to a three-dimensional network.  相似文献   

4.
A new kind of Schiff base HL(HL= 1-phenyl-3-methyl-4-(p-methylbenzoyl)-5-pyrazolone with L-Leucine methyl ester) and complexes Ni L′_2·0.75C_2H_5OH·0.25H_2O,Cu L′′2(L′ = 1-phenyl-3-methyl-4-(p-methylbenzoyl)-5-pyrazolone with L-leucine ethyl,L′′ = 1-phenyl-3-methyl-4-(p-methylbenzoyl)-5-pyrazolone with L-leucine) have been synthesized and structurally determined by X-ray diffraction. For HL: crystal structure determination indicates that there are two independent HLs with different conformations in one asymmetric unit. For complex 1: the Ni(Ⅱ) ion is six-coordinated by two carbonyl oxygen atoms from pyrazolone ring,two nitrogen atoms from different HL′ and two oxygen atoms from L-Leucine ethyl ester to form a distorted octahedral geometry. For complex 2: the Cu(Ⅱ) ion is four-coordinated by one carbonyl oxygen atom from the pyrazolone ring,one nitrogen atom from HL′′,and two different carboxylic oxygen atoms from L-leucine with the same conformation to form a distorted quadrilateral geometry.  相似文献   

5.
A new complex has been synthesized with o-methylbenzoyl-benzoic acid(HL) and 1,10-phenanthroline(phen) in the mixture of water and ethanol. It crystallizes in monoclinic, space group C2/c with a = 13.6328(18), b = 17.7876(18), c = 19.998(2), β = 104.720(4)o, C54H48N4O11Zn, Mr = 994.33, V = 4690.2(9)3, Dc = 1.408 g/cm3, Z = 4, F(000) = 2072, μ(MoKα) = 0.59 mm-1, R = 0.0736 and wR = 0.2029. The crystal structure shows that the zinc ions are coordinated with two oxygen atoms from two HL molecules and four nitrogen atoms from two phen molecules, forming distorted octahedral coordination geometry. The fluorescent and thermal stability properties of the complex are studied. The result shows that it has one fluorescent emission band at around 412 nm. In addition, the complex is stable under 210 ℃.  相似文献   

6.
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   

7.
A new metal-organic complex [Pb2(PDB)2(phen)]n·nH2O (H2PDB=pyridine-3,4-dicarboxylic acid,phen=1,10-phenanthroline) 1 has been hydrothermally synthesized and structurally characterized by elemental analysis,IR spectrum,TG and single-crystal X-ray diffraction.The compound crystallizes in triclinic,space group P1 with a=7.2472(5),b=10.6966(8),c=16.2376(12),α=98.2960(10),β=91.6430(10),γ=97.4810(10)o,V=1233.53(16)3,C26H16O9N4Pb2,Mr=942.81,Dc=2.538 g/cm3,μ(MoKα)=13.697 mm-1,F(000)=872,Z=2,the final R=0.0247 and wR=0.0654 for 3886 observed reflections (I 2σ(I)).In the crystal structure,the Pb(1) atom is six-coordinated with four carboxylate oxygen atoms from three different PDB ligands and two nitrogen atoms from phen ligand,showing a distorted octahedral geometry;the Pb(2) atom is four-coordinated with four carboxylate oxygen atoms from four different PDB ligands,showing a distorted tetrahedral geometry.It exhibits a three-dimensional supramolecular network structure formed by hydrogen bonds and π-π interactions.  相似文献   

8.
The crystal structure of Ni(Ⅱ) complex with 3-hydroxyl-1, 5-diazacycloheptane-N, N'-diacetate was determined by X-ray diffraction method. Crystal data for Ni2 (C9H14N2O5)2·2H2O: monoclinic, space group P21/n, a = 1.1717(5), b = 0.9794(3), c = 1.2971(2) nm, β= 96.62(3), V= 1.4786(7) nm3, Dc = 1.377 g/cm3, Z = 2,μ=13.321 cm-1 (Mo-Kα), F(000)=640. The final R and Rw are 0.075 and 0.089 respectively. The Ni(Ⅱ) ion forms 2:2 complex with ligand. Two ligands are bridged by two Ni(Ⅱ) atoms which are bridged by two O atoms. Every Ni(Ⅱ) is coordinated by two N atoms and four 0 atoms. The coordination polyhedron of the Ni(Ⅱ) ion is a distorted octahedron.  相似文献   

9.
The title complex Co(L)2Cl·4H2O I has been achieved via self-assembly by incorporating cobalt into 2-benzoylpyridine thiosemicarbazonate ligand, and characterized by elemental analysis, infrared spectra, mass spectra and single-crystal X-ray diffraction study. The crystal crystallizes in monoclinic, space group P21/n, with a=10.227(3), b=17.363(4), c=17.459(4), β=100.408(4)o, V=3049.2(13)3, Z=4, Mr=677.08, Dc=1.475 g/cm3, μ(MoKα)=0.834 mm-1, F(000)=1400, the final R=0.0747 and wR=0.0896 for 1663 observed reflections with I > 2σ(I). The complex contains one six-coordinated cobalt ion connected by two thiosemicarbazone ligands which act as a tridentate ligand to coordinate with the center metal atoms via two pyridyl nitrogen atoms, two imine nitrogen atoms and two sulfur atoms giving rise to a mononuclear structure. Hydrogen bonds existing in the complex link the different com-ponents to stabilize the crystal structure. The antitumor activity of the title complex was tested against A549 lung cancer cell line. Complex I exhibits antitumor activity.  相似文献   

10.
徐涵  李一志 《结构化学》2010,(11):1606-1611
A novel NiII complex [{Ni(IBG)(4,4'-bipy)(H2O)2}·3H2O]n 1 (H2IBG = isophthaloylbisglycine and 4,4'-bipy = 4,4'-bipyridine) has been synthesized and characterized by singlecrystal X-ray diffraction, elemental analysis, IR spectra and thermogravimetric analysis. It crystallizes in monoclinic, space group P2/c with a = 15.5420(7), b = 22.4344(1), c = 8.3455(5), β = 101.538(3)o, V = 2670.1(7)3, Z = 4, C22H32N4NiO13, Mr = 619.23, Dc = 1.443 g/cm3, F(000) = 1296.0, μ(MoKα) = 0.750 mm-1, the final R = 0.0570 and wR = 0.1445 for 2296 observed reflections with I 2σ(I). In the structure, the NiII metal center is coordinated in an octahedral environment arranged by two water molecules, two carboxylate oxygen atoms and two nitrogen atoms from two 4,4'-bipy ligands. Thermal decomposition and powder X-ray diffraction results indicate that the transformation from the crystal form, [{Ni(IBG)(4,4'-bipy)(H2O)2}·3H2O]n, to the amorphous powder, Ni(IBG)(4,4'-bipy)(H2O)2, is reversible, so the latter form may be utilized as an absorbing agent for water and water vapor.  相似文献   

11.
Two complexes CuLCl(H2O) 1 and Ni(L)2 2 (HL = 2-carboxy-1,10-phenanthroline) have been synthesized and characterized by single-crystal X-ray crystallography. The structure of 1 has a monoclinic space group P21/n with a = 7.985(2), b = 16.067(3), c = 9.694(2) A, β = 98.189(30)°, V= 1231.0(4) A^3, Z = 4, Dc = 1.836 g/cm^3,μ =1.998 mm^-1, F(000) = 684, the final R = 0.0301 and wR = 0.0810. The structure of 2 (C26H14N4NiO10) adopts an orthorhombic system, space group Pbea with a = 9.410(2), b = 23.2410(5), c = 23.8680(5) A, V = 5219.9(18) A^3, Z = 8, Mr = 601.12, Dc = 1,530 g/cm^3,μ = 0.809 mm^-1, F(000) = 2448, the final R = 0.0448 and wR = 0.1427. The Cu center of complex 1 exhibits a square pyramidal coordination environment with one oxygen and two nitrogen atoms from deprotonated 2-carboxy-1,10-phenanthroline, one oxygen atom from water and one chloride ion. The Ni center of complex 2 assumes a distorted octahedral coordination geometry consisting of two oxygen atoms and four nitrogen atoms of two deprotonated 2-carboxy-1,10-phenanthroline molecules. Supramolecular assembly has been found via noncovalent bonds, such as hydrogen bonds and π-π stacking interactions.  相似文献   

12.
A new metal-organic complex Co2(cbba)4(phen)2(μ2-OH2)(H2cbba=2-(4'-chlorine-benzoyl)benzoic acid,phen=1,10-phenanthroline) 1 has been hydrothermally synthesized and struc-turally characterized by single-crystal X-ray diffraction,elemental analyses,TG and IR spectroscopy.The compound crystallizes in triclinic,space group P1 with a=10.7659(7),b=17.1856(11),c=19.2022(13),α=83.8120(10),β=84.9930(10),γ=87.2070(10)°,V=3515.8(4)3,C80H50Cl4Co2N4O13,Mr=1534.90,Dc=1.450 g/cm3,μ(MoKα)=0.693 mm-1,F(000)=1568,Z=2,the final R=0.0490 and wR=0.1092 for 8216 observed reflections(Ⅰ > 2σ(Ⅰ)).In the crystal structure,the cobalt atom is six-coordinated with three carboxylate oxygen atoms from three different cbba ligands,one oxygen atom from coordinated water molecule and two nitrogen atoms from phen ligand,showing a distorted octahedral geometry.Furthermore,it exhibits a 3D supramolecular network through π-π and hydrogen bonding interactions.  相似文献   

13.
A new complex [Pb(phen)2(4-NBA)]2·2(NO3)·H2O(phen = 1,10-phenanthroline,4-NBA = 4-nitrobenzoate) has been hydrothermally synthesized and structurally determined by single-crystal X-ray diffraction,elemental analyses and IR spectroscopy.The complex crystallizes in monoclinic,space group P21/c with a = 13.416(3),b = 14.065(3),c = 16.845(3) ,β = 110.55(3)o,V = 2976.5(10)3,Z = 2,Dc = 1.796 g/cm3,F(000) = 1564,GOOF = 0.962,the final R = 0.0686 and wR = 0.1746.The crystal structure shows that the lead ion is coordinated with two carboxylate O atoms from the 4-NBA anion,and four N atoms from two phen molecules,forming a slightly distorted pentagonalbipyramidal coordination geometry.It is further extended by various supramo-lecular interactions to form a three-dimensional supramolecular network.The TG analysis result shows that this complex begins decomposing at 30 ℃ and decompounding completely at 733 ℃.  相似文献   

14.
许玉敏  赵小亮  胡拖平 《结构化学》2011,30(10):1442-1446
One cadmium(Ⅱ)coordination polymer [Cd(phen)(4,6-dimethyl-5-nitro-isophtha-lic acid)]n(1)has been synthesized with 4,6-dimethyl-5-nitro-isophthalic acid,phen(phen = 10-phenanthroline),and cadmium nitrate in the mixture of DMSO:H2O(V:V = 2:1).Crystallogra-phic data for this complex:monoclinic,space group P21/c,with a = 11.668(2),b = 11.841(6),c = 14.446(2),β = 102.440(4)°,V = 1.9491(8)3,Dc = 1.805 g/cm3,Z = 1,F(000)= 1056,GOOF = 0.999,R = 0.0280 and wR = 0.0662.The crystal structure analysis indicates that the cadmium ion is coordinated with two nitrogen atoms of one 1,10-phenanthroline molecule and five oxygen atoms from three 4,6-dimethyl-5-nitro-isophthalic acid molecules.The curve of TGA shows that 1 is stable up to 380.0 ℃.  相似文献   

15.
李薇  李玉林  李昶红  谭雄文 《结构化学》2011,30(9):1279-1282
The nickel complex {Ni(2,2-bipy)(H2O)3[C8H11O2(COO)]}(H2O)3 with bicycle-[2.2.1]-2-hepten-5,6-dicarboxylic acid [C7H8(COOH)2] and 2,2'-bipyridine (bipy) as ligands has been synthesized and characterized. It crystallizes in monoclinic, space group P , with a = 0.74975(3), b = 1.20309(4), c = 1.30593(4) nm, α = 109.861(2), β = 98.519(2), γ = 90.575(2)o, V = 1.09337(7) nm3, Dc = 1.552 g/cm3, Z = 2, F(000) = 524, the final GOOF = 1.064, R = 0.0397 and wR = 0.1171. The crystal structure shows that the nickel ion is coordinated with four oxygen atoms from one bicycle[2.2.1]-2-hepten-5,6-dicarboxylic acid molecule and three water molecules and two nitrogen atoms from the 2,2′-bipyridine molecule, forming a distorted octahedral coordination geometry. The result of TG analysis shows that the title complex is stable under 200.0 ℃.  相似文献   

16.
A new copper complex [Cu(pdc)(bpy)]·H2 O(1, H2 pdc = 3,5-pyridinedicarboxylic acid, bpy = 2,2-bipyridine) has been solvothermally synthesized and characterized by single-crystal X-ray diffraction, elemental analysis, IR spectroscopy, UV-vis spectroscopy and magnetic measure- ments. Complex 1 crystallizes in monoclinic system, space group P21 /c, a = 10.893(2), b = 7.3641(15), c = 1.9921(4), β = 92.16(3), V = 1596.9(6)3, Dc = 1.676 g/cm3, Mr = 402.84, Z = 4, F(000) = 820, μ = 1.404 mm-1, the final R = 0.0237 and wR = 0.0693. The Cu(II) ion is five-coordinated by two O atoms from two pdc ligands, one N atom from another pdc ligand and two N atoms from the bpy ligand. The pdc anion, which acts as a tridentate ligand, links three Cu ions, forming(3,3)-connected two-dimensional(2D) sheets. We also studied the electronic structure and orbital energies of complex 1 by DFT methods, and the results are consistent with UV-vis spectrum.  相似文献   

17.
A new dinuclear complex [Zn(dpa)(bipy)(H2O)]2 (dpa = 2,2'-diphenic acid, bipy = 2,2'-bipyridine) 1 has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, fluorescence spectrum and single-crystal X-ray diffraction. The complex crystallizes in monoclinic, space group P21/c with a = 10.960(2), b = 9.4841(18), c = 20.599(4), β = 104.452(3)o, V = 2073.4(7)3, C48H36N4O10Zn2, Mr = 959.55, Dc = 1.537 g/cm3, μ(MoKα) = 1.225 mm-1, F(000) = 984, Z = 2, the final R = 0.0364 and wR = 0.0843 for 2788 observed reflections (I > 2σ(I)). In the crystal structure, the zinc atom is five-coordinated with two carboxylate oxygen atoms from different dpas, one coordinated water molecule and two nitrogen atoms from bipy ligands, showing a slightly distorted triangular bipyramidal geometry. Furthermore, it exhibits a zero-dimensional network structure with a sixteen-membered ring and shows yellow photoluminescent property at room temperature.  相似文献   

18.
A novel one-dimensional chain coordination polymer [Mn(NAA)2(4,4’-bipy)(H2O)4]n has been synthesized with α-naphthaleneacetic acid, 4,4’-bipy and manganese(II) sulfate as raw ma-terials. Crystal data for this complex: monoclinic, space group P21/c, a = 1.1421(2), b = 1.6337(3), c = 0.94177(19) nm, β = 112.15(3)o, V = 1.6275(6) nm3, Dc = 1.407 g/cm3, Z = 2, μ(MoKα) = 0.467 mm-1, F(000) = 722, S = 1.007, R = 0.0412 and wR = 0.1022. The crystal structure shows that two neighboring manganese(II) ions are linked together by one 4,4?-bipy molecule, and the whole complex molecule forms a one-dimensional chain structure. Each manganese(II) ion is coordinated with two oxygen atoms of two α-naphthaleneacetic acid molecules, two nitrogen atoms of two 4,4?-bipy molecules and two oxygen atoms from two water molecules, giving a distorted octahedral coordination geometry. The electrochemical properties were also analyzed.  相似文献   

19.
A one-dimensional chain coordination polymer [Co(II)(C6H5CH=CHCOOH)2(4,4′- bipy)(H2O)5]n has been synthesized with cinnamylic acid, 4,4′-bipy and cobaltous chloride as raw materials. Crystal data for this complex: monoclinic, space group P21/c, a = 1.1481(3), b = 1.1230(2), c = 1.1759(3) nm, β = 97.054(4)o, V = 1.5046(6) nm3, Mr= 617.50, Dc = 1.363 g/cm3, Z = 2, μ(MoKα) = 0.627 mm-1, F(000) = 646, S = 1.062, R 0.0443 and wR = 0.1178. The crystal structure shows that two neighboring cobalt(II) ions are linked together by one 4,4′-bipy, and the whole complex molecule adopts a one-dimensional chain structure. Each cobalt(II) ion is coordinated with two nitrogen atoms from two 4,4′-bipy molecules and four oxygen atoms from four water molecules, giving a distorted octahedral coordination geometry. The electrochemical properties were analyzed by combining with the crystal structure.  相似文献   

20.
李静  王玉红  宋瑞峰 《结构化学》2014,33(10):1488-1494
A novel two-dimensional lead(II) coordination polymer 1, [C11H7Cl2NO3Pb]n, has been prepared by solvothermal reaction of new bridging ligand(5-chloro-quinolin-8-yloxy)acetic acid(HL) with PbCl2, and its structure was characterized by IR, elemental analysis, TG-DTA and single-crystal X-ray diffraction analysis. The crystal is of monoclinic system, space group P21/c with a = 16.7603(7), b = 8.6907(4), c = 8.4745(3), β = 101.1110(11)°, C11H7Cl2NO3 Pb, Mr = 479.27, V = 1211.25(9)3, Z = 4, Dc = 2.628 g/cm3, F(000) = 880, μ = 14.367 mm-1, R = 0.0173 and wR = 0.0508. The asymmetric unit contains one lead(II) cation, one(5-chloro-quinolin-8-yloxy)acetate(L) ligand and a chloride ion. The PbII center is hepta-coordinated in a distorted pentagonal bipyramidal geometry. The coordination sphere of the Pb atom is completed by two oxygen atoms and one nitrogen atom of the same L ligand, two bridging chloride ions and two bridging oxygen atoms of two adjacent L ligands. Two PbII centers are linked by the two L ligands to form a C2-symmetric dimer unit with a planar [Pb2O2] ring. Each dimer unit acts as a secondary building unit(SBU) and links adjacent four dimer units by the chloride atoms and oxygen atoms of carboxylate groups of L, forming a two-dimensional array. Such two-dimensional layers are packed through intermolecular C–H···Cl hydrogen bonds into a three-dimensional supramolecular structure. When the dimer unit is viewed as a 4-connected node, 1 is simplified as a 4-nodal 2-D network with square lattices of the diagonal lengths to be 6.079(1). The fluorescence emission peak of complex 1 appears near 407 nm.  相似文献   

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