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1.
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   

2.
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   

3.
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   

4.
郭锋 《结构化学》2010,29(2):187-190
A coordination polymer [Ni(pbc)2(H2O)]n(Hpbc = 3-pyrid-4-ylbenzoic acid) has been prepared by hydrothermal synthesis and characterized by single-crystal X-ray diffraction,IR and elemental analysis.The crystal is of monoclinic,space group C2/c with a=19.624(5),b=12.029(5),c=19.452(5),β=104.45(5)°,C24H18NiN2O5,Mr=473.11,V=4447(2)3,Dc=1.413 g/cm3,F(000)=1952,μ = 0.91 cm-1,Z = 8,the final R=0.0424 and wR=0.0871 for 3757 reflections with I2σ(I).X-ray diffraction analysis reveals that the pbc-ligands act as diconnectors to link two Ni(Ⅱ) centers and adopt two coordination modes of μ2-N,O and μ2-N,O,O to form infinite wavy nickel-carboxylate chains along the bc plane.The topological analysis of compound [Ni(pbc)2(H2O)]n reveals that it is a typical CdS framework.  相似文献   

5.
Two macrocyclic zinc(II) complexes {[ZnL(VO3)2]·0.33H2O}n(1) and [ZnL(H2O)2][Ni(CN)4](2)(L = 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane) have been obtained from the reactions of [ZnL](ClO4)2 with NH4VO3 and K2[Ni(CN)4], respectively, and structurally characterized by elemental analysis, IR, XRPD, TG and X-ray diffraction. Single-crystal X-ray diffraction analyses indicated that the Zn(II) atom lies on an inversion center and is octahedrally coordinated by four nitrogen atoms of the tetradentate macrocyclic ligand in the equatorial plane and two oxygen atoms of [VO4] tetrahedra in the axial positions in 1, and two oxygen atoms of two water molecules in 2. Complex 1 shows a three-dimensional structure, which is constructed by the links of [VO3]nn- chains with [ZnL]2+, forming one-dimensional channels occupied by guest water molecules. The monomers of [ZnL(H2O)2]2+ and [Ni(CN)4]2- are connected through the intermolecular hydrogen bonds to form a two-dimensional sheet in complex 2.  相似文献   

6.
A new coordination compound [Ba(OBPT)2(H2O)2]·H2O was obtained at room temperature by the reaction of 4,6-bis(2-pyridyl)-1,3,5-triazin-2-ol(HOBPT) with BaCl2.It was characterized by elemental analysis,FTIR,TG analysis,powder X-ray diffraction analysis and single-crystal X-ray diffraction analysis.The complex crystallizes in the monoclinic P21/n space group,with a = 16.325(1),b = 6.7977(5),c = 24.164(2) ,β = 104.009(1),V = 2601.8(3) 3,Z =4,C26H22BaN10O5,Mr = 691.88,Dc = 1.766 g/cm3,F(000) = 1376 and μ(MoKα) = 1.587 mm-1.The final R = 0.0282 and wR = 0.0724 for 5095 observed reflections with I > 2σ(I) and R = 0.0312 and wR = 0.0744 for all data.In the complex,the barium ion is ten-coordinated with six nitrogen atoms from two ligands,two deprotonated hydroxyl oxygen atoms from another two ligands and two coordinated water molecules to form a double stranded chain.The extensive supramolecular interac-tions lead to the formation of an infinite 2D framework.  相似文献   

7.
李邦玉  姚英明  王耀荣  张勇  沈琪 《结构化学》2011,30(10):1459-1463
The treatment of the mixture of n-BuLi with 1 equiv.8-aminoquinoline in THF in situ,which reacted further with 1/3 equiv.of YbCl3 in THF,to give the homoleptic lanthanide amide ate complex Yb(NH-C9H6N)4Li(C4H8O)2(1).The crystal structure was determined by X-ray diffraction and the following crystallographic data were obtained:C44H44N8O2YbLi,Mr = 896.85,monoclinic,space group C2/c,a = 7.8384(16),b = 22.294(5),c = 22.668(5),β = 97.614(5)°,V = 3926.3(14)3,Z = 4,Dc = 1.517 g/cm3,F(000)= 1812,μ(MoKα)= 2.431 mm-1,R = 0.0542 and wR = 0.1523 for 3372 observed reflections with I > 2σ(I).The structure of molecule 1 consists of one ytterbium atom,one lithium atom,four 8-aminoquinoline ligands and two THF molecules.The ytterbium atom is coordinated by eight nitrogen atoms of four 8-aminoquinoline ligands,forming a distorted dodecahedral geometry.  相似文献   

8.
A new energetic organic potassium salt bis(dinitromethyl)difurazanyl ether potassium salt [K2(BDFE)] was synthesized, and structurally characterized by elemental analysis, IR spectra, 13 C NMR and single-crystal X-ray diffraction. K2(BDFE) crystallizes in monoclinic system, space group C2/c with a = 17.342(3), b = 12.6943(17), c = 8.0972(11), β = 110.630(2)°, V = 1668.3(4)3, Z = 4, Dc = 2.000 g/cm3, F(000) = 1000, μ = 0.675 mm-1, S = 1.058, the final R = 0.0499 and wR = 0.1452. The K ion is eight-coordinated with eight O atoms from one water molecule and four bis(dinitromethyl)difurazanyl ethers(BDFE), forming a distorted dodecahedral structure. Thermal decomposition of the title complex was studied by using DSC and TG-DTG. There are primarily two exothermic decomposition processes between 200 and 370 ℃.  相似文献   

9.
One novel organically templated zincophophate(C5N2H14)·[Zn3(OH2)(PO4)2(HPO4)] has been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction together with elemental analysis, infrared spectroscopy, thermogravimetric analysis, and powder X-ray diffraction. The title compound crystallizes in the monoclinic space group P21/n, with a = 9.7904(11), b = 14.0287(14), c = 11.8651(13) , β = 104.690(3), V = 1576.4(3) 3, Z = 4, T = 296(2) K, Mr = 601.31 and Dc = 2.533 g/cm3. The compound consists of a macroanionic [Zn3(OH2)(PO4)2(HPO4)]2- framework and(C5N2H14)2+ cations, and its structure is built up from ZnO3(OH2), ZnO4, HPO4 and PO4 tetrahedral units that result in 4, 8 and 10-ring channels.  相似文献   

10.
Reaction of bis(4,6-dimethyl-2-pyrimidinethiolato)methane(bpytm) with CuCl2·4H2O in a mixed methanol/dichloromethane solution gave a one-dimensional coordina-tion polymer [CuCl2(μ-bpytm)]n which was characterized by single-crystal X-ray diffraction.It crystallizes in monoclinic,space group P21/c with a=16.9433(5),b=13.6986(4),c=7.8434(2),β=100.371(2)°,V=1790.71(9)3,Z=4,Mr=426.86,Dc=1.583 g/cm3,μ(MoKα)=1.751mm-1,F(000)=868,S=1.025,the final R=0.0399 and wR=0.0924 for 2538 observed reflections with Ⅰ2σ(Ⅰ) and 206 variables.The neutral coordination polymer is constructed by the bidentate thioether ligands to link adjacent copper atoms.Each copper atom is bridged by two adjacent nitrogen atoms of bpytm ligands and terminally bonded by two chloride atoms to form a squareplanar coordination geometry.The average Cu-N and Cu-Cl bond lengths are 2.025(2) and 2.234(1),respectively.  相似文献   

11.
A novel coordination polymer {[Zn(ts-gln)(bipy)]3H2O}n (ts-glnH2=N-p-toly-sulfonyl-glutamine,bipy=2,2-bipyridine) has been prepared and structurally characterized by X-ray diffraction method. It crystallizes in orthorhombic,space group P212121 with a=8.2622(5),b=16.6244(10),c=18.2807(10) ,V=2510.9(3) 3,C22H28N4O8SZn,Mr=573.91,Z=4,Dc= 1.518 g/cm3,μ(MoKa)=1.115 mm-1,F(000)=1192,the final R=0.0262 and wR=0.0662 for 5691 independent reflections with Rint=0.0240. The zinc(Ⅱ) atom is coordinated by N(3) and N(4) atoms of a bipy molecule,two carboxylate O(1) and O(2A) and amino N(1) atoms of ts-gln ligands,resulting in a square-pyramidal geometry. The title complex consists of an infinite zigzag chain of zinc(Ⅱ) ions linked by the carboxylate of N-p-tolysulfonyl-glutamine.  相似文献   

12.
The title compound, [InCl(C4H5NO4)]n, has been synthesized via the hydrothermal method and characterized by IR, elemental analysis, UV-Vis-Nir spectra and single-crystal X-ray diffraction analysis. Single-crystal X-ray analyses show that it is a carboxylate-bridged two-dimensional layer network indium(III) polymer, catena-poly[[chloroindium(III)]-μ-(iminodiacetate к4N,O,O':O':O'']. The crystal is of orthorhombic system, space group Pnma with a = 13.5970(13), b = 8.7671(10), c = 6.0427(5), C4H5ClInNO4, Mr = 281.36, V = 720.33(12)3, Z = 4, Dc = 2.594 g/cm3, F(000) = 536, μ = 3.613 mm-1, R = 0.0245 and wR = 0.0570. The In(III) ion exhibits an approximately octahedral InClNO4 coordination environment, with the two O donor atoms of iminodiacetate and two O atoms belonging to the carboxylate group of two adjacent iminodiacetates occupying the basal positions, and the chlorine ion and one nitrogen atom of iminodiacetate in the apical sites. Carboxylate groups are mutually cis oriented, and each syn-anti carboxylate group bridges two indium(III) ions via two different basal positions, resulting in the formation of a 2-D network with rhombus (4, 4) grids. Each rhombus grid unit is formed from four indium atoms and four iminodiacetate units with the diagonal lengths of 8.767(1) and 6.043(1).  相似文献   

13.
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   

14.
孙海燕 《结构化学》2014,33(10):1467-1471
The novel crystal of the title compound 2-(((5-(((5,7-dimethyl-[1,2,4]triazolo-[1, 5-a]-pyrimidin-2-yl)thio)methyl)-4-phenyl-4H-1,2,4-triazol-3-yl)thio)methyl)-4H-chromen-4-one methanol solvate(C27H25N7O3S2, Mr = 559.66) has been prepared and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monocline system, space group P21/c with a = 11.9879(9), b = 14.0743(10), c = 15.9706(11), β = 98.509(2)°, V = 2664.9(3)3, Z = 4, Dc = 1.395 g/cm3, F(000) = 1168, μ = 0.116 mm-1, MoKa radiation(λ = 0.71073), R = 0.0652, and wR = 0.1425 for 5220 observed reflections with I 2σ(I). X-ray diffraction analyses reveal that the molecule adopts a C-shape. The planes of the benzopyrone and triazolopyrimidine were nearly parallel to each other, with a dihedral angle of 1.21(3)°. Intramolecular and intermolecular hydrogen bonds together with π-π interations are found to exist in the structure. The results of MTT assay indicate that the title compound displays excellent antiproliferative activity against two human cancer cell lines.  相似文献   

15.
The new title compound 8-((4-((2,3-diaminopyridin-4-yl)-oxy)-3-fluorophenyl)-amino)-2-(4-fluorophenyl)-3-methyl-2,7-naphthyridin-1(2H)-one(C26H20F2N6O2, Mr = 486.48) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 15.365(3), b = 13.144(2), c = 11.863(2), β= 108.882(3)°, Z = 4, V = 2267.0(7)3, Dc = 1.425 g/cm3, F(000) = 1008, μ = 0.105 mm-1, MoKa radiation(λ = 0.71073), R = 0.0480 and wR = 0.1294 for 3197 observed reflections with I 2σ(I). X-ray diffraction analysis reveals that the region C(substituents of 8-amino group and 3-methyl group on the 2,7-naphthyridin-1(2H)-one ring) of compound 6 are effectively planar. Intramolecular and intermolecular hydrogen bonds together with π···π interations are found in the structure. In addition, compound 6 shows potent c-Met and c-Kit kinase inhibition activities.  相似文献   

16.
A novel supramolecular mixed ligand complex of formula [Cu(PTS)2(Him)2(H2O)2] (C20H26CuN4O8S2,PTS=p-toluenesulfonate,Him=imidazole) has been synthesized in aqueous solution and characterized by elemental analysis,IR and single-crystal X-ray diffraction.The compound crystallizes in the monoclinic system,space group P21/n,Z=2,a=5.650(2),b=14.671(3),c=14.638(3),β=100.10(3)°,V=1194.60(4)3,Dc=1.607 g/cm3,μ(MoKα)=1.143 mm-1,F(000)=598,R=0.0615 and wR=0.1503 for 1752 observed reflections with I 2σ(I).The copper(II) ion in the complex adopts a slightly distorted octahedral coordination geometry and is six-coordinated with N2O4 donor set consisting of two nitrogen atoms and four oxygen atoms provided by the ligands of two imidazole molecules,two water molecules and two p-toluenesulfonate ions.The sulfonate group of the PTS ligand remains weak-coordinated and forms a number of hydrogen bonds with water molecules and imidazole ligands.X-ray structural analysis reveals that the coordination molecules are connected to form a 3-D supramolecular framework by electrostatic interaction,weak van der Waals forces,hydrogen bonding and π-π interaction.The thermal behaviour of the title complex was investigated by using DSC and TG-DTG techniques.  相似文献   

17.
黄统辉  陈华  陈杰  张爱东 《结构化学》2014,33(10):1455-1459
Two 5-pyrimidinyl-1,2,4-oxadiazoles were synthesized through two different routes and their structures were characterized by single-crystal X-ray diffraction, NMR and MS. Compound 3, 5-(2-chloro-4-methyl-6-phenylpyrimidin-5-yl)-3-phenyl-1,2,4-oxadiazole, crystallizes in orthorhombic, space group Pbca with a = 19.1575(11), b = 8.2115(5), c = 21.2035(12), V = 3335.6(3)3 and Z = 4. Compound 6, 5-(2,6-dichloropyrimidin-4-yl)-3-phenyl-1,2,4-oxadiazole, crystallizes in monoclinic space group Pn with a = 8.4275(13), b = 5.4088(8), c = 13.493(2), β = 99.768(3)o, V = 4658.6(6)3 and Z = 8. Preliminary bioassay indicated that the two title compounds had good herbicidal activities.  相似文献   

18.
A novel coordination polymer {[Zn(ts-gln)(bipy)]3H2O}n (ts-glnH2=N-p-toly-sulfonyl-glutamine,bipy=2,2-bipyridine) has been prepared and structurally characterized by X-ray diffraction method. It crystallizes in orthorhombic,space group P212121 with a=8.2622(5),b=16.6244(10),c=18.2807(10) ,V=2510.9(3) 3,C22H28N4O8SZn,Mr=573.91,Z=4,Dc= 1.518 g/cm3,μ(MoKa)=1.115 mm-1,F(000)=1192,the final R=0.0262 and wR=0.0662 for 5691 independent reflections with Rint=0.0240. The zinc(Ⅱ) atom is coordinated by N(3) and N(4) atoms of a bipy molecule,two carboxylate O(1) and O(2A) and amino N(1) atoms of ts-gln ligands,resulting in a square-pyramidal geometry. The title complex consists of an infinite zigzag chain of zinc(Ⅱ) ions linked by the carboxylate of N-p-tolysulfonyl-glutamine.  相似文献   

19.
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   

20.
The title tetranuclear complex,(μ4-oxo)-hexakis(μ2-chloro)-tetrakis(2-amino-1,3-thiazole-N)-tetra-copper(ii) [Cu4(μ4-O)(μ-Cl)6L4](1,L=2-amino-1,3-thiazole) was synthesized by the reaction of CuCl2·2H2O with 2-amino-1,3-thiazole in methanol and characterized by IR spectra and X-ray diffraction.Complex 1 crystallizes in triclinic,space group P1 with a=9.7137(2),b=10.7005(2),c=14.6505(2),α=83.9550(10),β=82.0930(10),γ=67.1640(10)°,V=1387.84(4)3,Mr=883.43,Z=2,μ=3.927 mm-1,Dc=2.1144 g/cm3,F(000)=868,R=0.0332 and wR=0.0814.The complex contains a tetrahedron of four CuII atoms coordinating to a central μ4-O atom,with the six edges of the tetrahedron bridged by six Cl atoms.The Cu-O bond distances range from 1.910(2) to 1.918(2),Cu-Cl from 2.3501(11) to 2.5924(10),and Cu-Cu from 3.1003(6) to 3.1663(6).The coordination geometries of the four coppers distort from trigonal bipramid to tetragonal pyramid with different distortion factors.The free animo groups of the ligands result in a lot of N-H···Cl and N-H···N intra-and intermolecular hydrogen bonds.  相似文献   

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