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1.
The mononuclear complex, Cu(H2SIP-O)(bpy)(H2O) (H4SIP-O = 4-hydroxyl- 5-sulfoisophthalic acid and bpy = 2,2'-dipyridyl), has been synthesized by the hydrothermal reaction of Cu(OH)2 with NaH2SIP and bpy at 160 ℃, and characterized by single-crystal X-ray diffraction, elemental analysis and IR spectrum. The new ligand 4-hydroxyl-5-sulfoisophthalic acid derived from 5-sulfoisophthalic acid ligand under an in situ hydrothermal condition. The crystal of the complex crystallizes in a triclinic system, space group P1, with a = 7.757(4), b = 10.663(6), c = 11.727(7)A, α = 94.272(4), β = 104.067(7), γ = 97.400(7)°, V= 927.4(9)A^3, Z = 2, C18H14N2O9SCu, Mr= 497.93, Dc= 1.783 g/cm^3,μ = 1.350 mm^-1, F(000) = 506, the final R = 0.0518 and wR = 0.1513 for 4180 observed reflections with I 〉 2σ(I). The central Cu(II) ion is five-coordinated by two oxygen atoms from the H2SIP-O^2- ligand and two nitrogen atoms of bpy ligand in a distorted square-planar geometry as well as a water oxygen atom in the apical position to complete a distorted square-pyramidal coordination geometry. The mononuclear copper molecules are linked by hydrogen bonds between coordinated water molecules and sulfonate groups to form a one-dimensional double-chain structure. The chains are further held together through extensive π-π stacking interactions between the aromatic rings to form a three- dimensional supramolecular structure.  相似文献   

2.
银秀菊  欧阳淼  刘旭辉  蒋毅民 《结构化学》2009,28(10):1251-1256
A novel coordination polymer [Na2Cd(2,6-pyda)(N3)2(H2O)6]n (2,6-H2pyda = 2,6- pyridinedicarboxylic acid) has been synthesized 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 = 24.416(4), b = 10.7638(17), c = 6.9224(11) A^°, β= 106.124(2)A^°, V = 1747.7(5) A^°3, Mr = 515.64, De= 1.960 g/cm^3,μ = 1.365 mm^-1, F(000) = 1024, Z = 4, the final R = 0.0426 and wR = 0.1320. In the title complex, there exist two kinds of metal centers in the structure, cadmium ions and sodium ions. The Cd(Ⅱ) atom shows a distorted pentagonal-dipyramidal geometry defined by two O and one N atoms from one deprotonated pyda ligand and four N atoms from four μ-1,1,3 azido groups. The adjacent cadmium atoms are bridged via two μ-1,1,3 azido groups, along the c axis to afford an extended chain. There is also a 2D network which is comprised of binuclear subunits [NaE(H2O)6] connected by O atoms from coordinated water between the adjacent Cdn(pyda)n(Na)2n infinite chains. Furthermore, each cadmium atom is connected with four adjacent sodium atoms through the bridging N3- ligand in μ-1,3 patterns. Thus, the title complex exhibits a novel three-dimensional network structure.  相似文献   

3.
The coordination polymer [Zn(p-pdoa)4(bbp)]n 1 (p-pdoa = p-phenylenedioxydiacetate dianion and bbp = 2,6-bis(benzimidazol-2-yl)pyridine) has been synthesized by hydrothermal method and characterized by elemental analysis, IR and X-ray single-crystal diffraction. The title complex crystallizes in the triclinic system, space group P1^- with a = 7.8383(2), b = 12.6610(4), c = 13.1792(5)A, a = 84.433(2),β = 74.2980(1), γ = 87.4290(1)°, V = 1252.93(7)A^3, Z = 2, Dc = 1.593 g/cm^3,/z = 1.038 mm^-1, F(000) = 616, the final R = 0.0361 and wR = 0.1139. The Zn(Ⅱ) atom assumes a distorted trigonal bipyramidal geometry, involving two carboxyl O atoms from two different p-pdoa ligands and three N atoms from the bbp ligand. The Zn(Ⅱ) atom is alternately interlinked by p-pdoa ligands in a bismonodentate mode into a helical chain with a long pitch of 12.661 A and the adjacent Zn…Zn distance of 11.056 and 12.245 A. There exists a 2D supramolecular framework linked by π-π stacking (3.312 A) between adjacent benzimidazoles of bbp ligands and intermolecular hydrogen-bonding interactions between the uncoordinated carboxylate oxygen atoms (O(2), 0(5)) and the uncoordinated imidazolyl N atoms (N…O distances 2.706 and 2.786 A). There also exist two interlayer π-π stacking interactions of 3.299 A between adjacent central pyridines of bbp ligand and 3.176 A between the phenyl groups of p-pdoa ligand. Such π-π stacking interactions extend the two-dimensional layers into a 3D supramolecular network.  相似文献   

4.
A novel binuclear Cu(Ⅱ) complex [Cu(paba)Cl] (pabaH = 2-(2-pyridylmethylimine)benzenesulfonic acid) has been synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal of the title complex crystallizes in a monoclinic 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/cm^3,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 〉 20(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   

5.
The title complex [Co(L)2]Cl·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 P2 1/n, with a = 10.227(3), b = 17.363(4), c = 17.459(4) A, β= 100.408(4)°, V= 3049.2(13) A^3, Z = 4, Mr = 677.08, Dc = 1.475 g/cm^3, 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 components to stabilize the crystal structure. The antiturnor activity of the title complex was tested against A549 lung cancer cell line. Complex ! exhibits antitumor activity.  相似文献   

6.
A one-dimensional chain coordination polymer [Cu(phen)(2,4,6-TMBA)2(H2O)]n has been synthesized by reacting 2,4,6-trimethyl-benzoic acid, 1,10-phenanthroline and Cu(Ⅱ) perchlorate and its structure was characterized. Crystal data for this complex: tetragonal, space group I41, a = 2.0293(3), b = 2.0293(3), c = 1.3758(2) nm, α =β= γ = 90°, V= 5.6657(13) nm3, Dc= 1.379 g/cm3, Z = 8, μ(MoKa) = 0.815 mm-1, Mr = 588.14, F(000) = 2456, S = 1.047, R = 0.0459 and wR = 0.1053. The crystal structure shows that two neighboring Cu(Ⅱ) ions are linked together by one bridging-chelating 2,4,6-trimethyl-benzoic group, forming a one-dimensional chain structure. Each Cu(Ⅱ) ion is coordinated with two nitrogen atoms from one 1,10-phenanthroline molecule, three oxygen atoms from three 2,4,6-trimethyl-benzoic acid molecules and one oxygen atom from one water molecule, giving a six-coordinate distorted octahedral coordination geometry. The cyclic voltammetry behavior of the complex was also investigated.  相似文献   

7.
Reaction of AgAc with bzdmpymtH in MeOH resulted in the title compound [Ag(bzdmpymt)]6-2MeOH (1.2MeOH), which was structurally characterized by elemental analysis, IR, and single-crystal X-ray diffraction analysis. 1.2MeOH belongs to the triclinic system, space group Pi, with a = 10.930(2), b = 11.646(2), c = 16.794(3)A, a = 103.97(3), β = 97.07(3), γ = 97.94(3)°, V = 2027.2(7) A3, Z = 1, μ = 1.629 mm^-1, Dc = 1.710 mg/m3, T = 193(2) K, CsoH86Ag6N12O2S6, Mr = 2087.25, F(000) = 1044, S = 1.034, R = 0.0355 and wR = 0.0709. In 1.2MeOH, six silver(I) atoms are held together by six bzdmpymt ligands through N and S atoms to form a water-wheel-shaped structure. Each Ag atom is coordinated by two S atoms from two bzdmpymt ligands and one N atom from the third bzdmpymt ligand, giving a trigonal planar coordination geometry. Interactions between the CH3 group of bzdmpymt ligand and one pyrimidyl nitrogen atom in an adjacent molecule afford a one-dimensional hydrogen-bonding chain running along the b axis. The luminescent property of 1.2MeOH was also investigated.  相似文献   

8.
杨燕  曾明华  张来军  梁宏 《结构化学》2009,28(7):785-788
A novel tetranuclear zinc(H) coordination polymer [Zn4(o-bda)a(p-pbim)4]n 1 (p-pbim = 4-pyridylbenzimidazole, o-bda2 = o-phenylenediacetic acid dianion) has been synthesized by a hydrothermal method and characterized by elemental analysis, IR and X-ray singlecrystal diffraction. The title complex crystallizes in monoclinic, space group of P21/n with α = 14.231(1), b = 16.257(1), c = 16.794(1) ]k, β = 100.26(1)°, V = 3823.1(2)A3, Z = 8, Dc = 1.573 g/cm^3,β = 1.321 mm^-1, F(000) = 1856, R = 0.0420 and wR = 0.111. The Zn(1) atom assumes a distorted trigonal bipyramidal geometry, involving three carboxyl O atoms from two different o-bda ligands and two N atoms from two p-pbim ligands. The Zn(2) atom is coordinated by two oxygens from two distinct bda2- anions and two nitrogen atoms from two p-pbim ligands to form a distorted tetrahedral geometry. The Zn(Ⅱ) atoms are alternately interlinked by o-bda ligands in bis-monodentate or chelating-bidentate and monodentate modes into one-dimensional undulate chains along axis c with the adjacent Zn…Zn distances of 8.32 and 8.47 A. Such neighboring chains are further extended into a 1D bi-chain structure with two different subrings A and B, which are 32- and 14-membered rings through interchain p-pbim ligands. There exists a 2D supramolecular network linked by intermolecular hydrogen-bonding interactions between the uncoordinated carboxylate 0(4) atom or coordinated carboxylate 0(7) atom and the uncoordinated imidazolyl N(2) and N(5) atoms with the O...N distances to be 2.695 and 2.807A.  相似文献   

9.
ZHAO Xiao-Fan 《结构化学》2008,27(7):853-857
A novel end-to-end azido-bridged polynuclear Schiff-base copper(II) complex, [Cu(C12H15Br2N2O)(N3)]n, was prepared and characterized by elemental analysis, IR spectra, and single-crystal X-ray diffraction. The crystal belongs to the orthorhombic system, space group Pbcn with a = 24.588(5), b = 10.377(2), c = 13.022(3) A, V= 3322.6(12) A^3, Z = 8, Dc = 1.874 g/cm^3, Mr = 468.65, λ(MoKa) = 0.71073 A,μ = 6.130 mm^-1, F(000) = 1832, R = 0.0637 and wR = 0.1176. The Cu atom in the complex is five-coordinated in a square pyramidal geometry by three donor atoms of the Schiff-base ligand, and two N atoms from two bridging azide ligands. The [2,4-dibromo-6-[(3-dimethylaminopropylimino)methyl]phenolato]copper(II) units are linked by the bridging azide ligands, giving zigzag polymeric chains with backbones of the [--Cu-N-N-N--Cu]n type running along the b axis.  相似文献   

10.
A new dinuclear copper complex, [Cu(C9H11N3)Cl2]2(C18H22Cl4Cu2N6), has been synthesized and characterized by X-ray structure determination. It crystallizes in the triclinic P1^- space group with a = 7.526(3), b = 9.473(4), c = 9.535(3)A, α = 117.214(10), β = 108.251(9), γ = 91.560(6)°, V = 562.3(4)A^3, Z = 1, Mr = 591.30, F(000) = 298, Dc = 1.746 g/cm^3, μ(MoKα) = 2.385 mm^-1, the final R = 0.0577 and wR = 0.1248 for 2188 unique reflections with 1629 observed ones (Ⅰ〉 2σ(Ⅰ)). In the title complex, each copper(Ⅱ) atom is located at the center of a distorted trigonal bipyramid of five coordination atoms (two nitrogen and three chlorine atoms). Two copper(Ⅱ) atoms were bridged by two chlorine anions (Cl(2) and Cl(2a)) to form a Cu(Ⅱ)-Cu(Ⅱ) binuclear entity with the distance between two copper(Ⅱ) atoms of 3.398 (A).  相似文献   

11.
A new La(Ⅲ) complex, {[La(L)(NO3)(H2O)3]·H2O}n (L = 1,10-phenanthroline- 2,9-dicarboxylate), has been synthesized and structurally determined by X-ray diffraction analysis. The complex crystallizes in the monoclinic system, space group P21/c with a = 7.7358(17), b = 8.1664(18), c = 28.271(6) A, β= 95.184(4)°, V= 1778.6(7) A3, Z = 4, C14H14LaN3O11, Mr = 539.19, Dc = 2.014 g/cm^3, μ= 2.471 mm^-1, F(000) = 1056, the final R = 0.0350 and wR = 0.0659. In this complex, each metal center adopts a ten-coordination geometry formed by two N atoms from a ligand L and eight O atoms from three H2O molecules, a nitrate ion and carboxylates of two ligands. Each ligand adopts a N2,O3-pentdentate coordination mode using two N and two O atoms chelating a La(Ⅲ), and using another O atom of carboxylate to bridge another La(Ⅲ) center resulting in a 1D helical chain molecule. Intermolecular strong O-H…O and weak C-H…O hydrogen bonds extend the 1D chain structure into a 3D supramolecular architecture.  相似文献   

12.
The synthesis and molecular structure of a new dinuclear copper(Ⅰ) complex [Cu(dppb)(NO 3)] 2 are reported.The compound crystallizes in the monoclinic system,space group P2 1 /n with a=12.830(3),b=10.899(2),c=19.666 (4),β=104.69(3)°,V=2660.1(9)3,Z=4,D c=1.378 g/cm 3,F(000)=1144,the final R=0.0600 and wR=0.0668 for 2951 observed reflections with I > 2σ(Ⅰ).The complex contains a folded Cu 2 P 4 core structure,with two Cu(Ⅰ) atoms being bridged by a pair of dppb ligands to form a 14-membered Cu 2 P 4 C 8 zigzag ring.The ligand sphere of each metal center is completed by a nitrate anion in a chelating fashion.  相似文献   

13.
O-(p-tolyl)dithiophosphato nickel complex [Ni(S2P{O}OC6HaCH3-p)(dppv)] has been synthesized by the treatment of (dppv)NiCl2 (dppv = Ph2PCH=CHPPh2) with (p-CH3C6HaO)2P{S}SH'Et2NH in THF. The new complex was fully characterized by elemental analysis, IR, 1H NMR, 31p NMR spectroscopies and thermo-gravimetric analysis. The molecular structure of the complex was established by X-ray crystallography. The crystal crystallizes in monoclinic, space group P21/c with a = 9.2739(5), b = 17.8803(8), c = 20.1879(12) A, fl = 93.269(5), V = 3342.1(3) A3, Z = 4, C33H29NiO2P3S2, Mr = 673.30, Dc = 1.338 g/cm3, F(000) = 1392 and #(MoKa) = 0.877 rnm-l. The final R = 0.0578 and wR = 0.1045 for 4138 observed reflections with 1 〉 20(/) and R = 0.1050 and wR = 0.1204 for all data. The Ni centre atom adopts a NiP2S2 square-planar geometry with two phosphorus atoms from the dppv ligand and two sulfur atoms from the O-(p-tolyl)dithiophosphate ligand. The most interesting structural feature of the title complex resides in its 1D helical chain structure constructing via intermolecular C-H'"O secondary interactions along the b-axis. The adjacent helical chains running in opposite directions are connected into a 1D double-stranded helical chain and further linked into a 2D supramolecular network by weak C-H.--C interaction.  相似文献   

14.
A mixed-ligand metal-organic complex [Cd(C7H3N3O2)(C12H8N2)]n was synthesized by cadmium(Ⅱ) nitrate, 1,10-phenanthroline(phen) and benzotriazole-5-carboxylate acid(H2btca). Single crystal X-ray analysis indicates that complex 1 has a two-dimensional layer structure and crystallizes in an orthorhombic space group(Pbca), with cell parameters, a=1.7422(6) nm, b=0.9264(3) nm, c=2.0729(7) nm, α=90°, β=90°,γ=90°, V=3.346(2) nm^3, Z=8. Each central Cd(Ⅱ) is six-coordinated by four N atoms, two of which are from 1,10-phenanthroline, and the other two from two different triazole nitrogen atoms and two O atoms from benzotriazole-5-carboxylate, forming a distorted octahedral geometry. Adjacent Cd(Ⅱ) centers are bridged by benzotriazole-5-carboxylate molecules to form a one-dimensional chain, which is further connected by the nitrogen atoms of btca^2- to form an extended two-dimensional wave-like layer, with OFF(offset face-to-face) stacking interactions between phen ligands in adjacent layers, which are helpful to forming the three-dimensional supramolecular structure.  相似文献   

15.
A new metal-organic complex Mn2(cbba)4(phen)2 (Hcbba = 2-(4'-chlorine-benzoyl)- benzoic acid, phen = 1,10-phenanthroline) 1 has been hydrotherrnally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses and IR spectroscopy. The compound crystallizes in orthorhombic, space group Pbcn with α = 12.154(5), b = 18.166(7), c = 31.197(13) A, V = 6887(5) A^3, C80H48Cl4Mn2N4O12, Mr= 1508.90, Dc = 1.455 g/cm^3, μ(MoKα) = 0.591 mm^-1, F(000) = 3080, Z = 4, the final R = 0.0408 and wR = 0.0873 for 4033 observed reflections (I 〉 2σ(I)). In the crystal structure, the manganese atom is six-coordinated with four carboxylate oxygen atoms from three different cbba ligands and two nitrogen atoms from phen ligands, showing a distorted octahedral geometry. Furthermore, it exhibits a 3D supramolecular network through π-π interactions.  相似文献   

16.
The complex [Cu(phen)2(POAc)3]ClO·4H2O has been synthesized and investigated by elemental analysis, IR spec-troscopy and X-ray diffraction methods, where phen = 1,10-phenanthroline, POAc = phenylacetate group). The complex crystallizes in the triclinic space group PI with two molecules in a unit cell of dimensions a = 1.0579(2) nm, b = 1.2423(3) nm, c = 1.9190(4) nm, α = 71.84(1)°, β = 80.50(2)°, γ = 88.60(1)°, V = 2.3625(9) nm3, R = 0.0407 and Rw = 0.0656. The complex results from bridging of two Cu(phen)2 units by three carboxylate groups, and each Cu2 ion is in a distorted square pyramidal geometry with two nitrogen atoms of phen and three carboxylate oxygen atoms of POAc. It has been showed that intramolecular stacking interactions occur between the phenyl moieties of POAc and aromatic rings of phen, leading to a novel molecule structure with two coordinating modes of carboxylate ligands, of which two phenylacetates are μ2-carboxylate-O-bridging ligands, and the other is a μ2-carboxylate-  相似文献   

17.
A mixed-valence dinuclear manganese complex, [MnⅡMnⅢL](ClO4)·1/2MeOH, where L is a macrocyclic ligand derived from the cyclocondensation of sodium 2,6-diformyl-4-methylphenolate with N,N-bis(2-aminoethyl)-2-hydroxybenzyl amine, was obtained and its structure was determined by X-ray diffraction. The orange crystal is a monoclinic system with space group P21/c and lattice parameters a=1.1617(4), b=1.4005(3), c=1.4641(3) nm, β=113.03(2)°, and Z=2. The crystal structure shows that each pendant-arm is bonded in a bidentate fashion to the adjacent metal atom and that both the arms are on the same side of the macrocycle. The two Mn atoms are bridged by two μ2-phenoxy oxygen atoms of the tetra-imine macrocycle, and each Mn atom, locating in a trigonal prismatic coordination environment(N3O3), is six-coordinated by the two imine nitrogen atoms, one tertiary nitrogen atom and a pendant phenol moiety apart from the two oxygen atoms.  相似文献   

18.
A new mononuclear Cu(II) complex, [Cu(L)] (H2L = 4,4′,6,6v-tetrabromo-2,2′- [ethylenedioxybis(nitrilomethylidyne)]diphenol), has been synthesized and structurally characterized. X-ray crystal structure of the complex reveals that the Cu(Ⅱ) ion is four-coordinated by two oxygen atoms and two nitrogen atoms from L2- unit. Crystallographic data: monoclinic, space group P21/n with a = 14.076(2), b = 6.9801(14), c = 19.858 (2) A, β= 107.613(2)°, C16n10Br4CuN2O4, Mr = 677.44, V = 1859.6(5) A3, Dc = 2.420 g/cm3,μ = 9.796 mm^-1, F(000) = 1284, Z = 4, the final R = 0.0516 and wR = 0.0938 for 1879 observed reflections with I 〉 2σ(/). The dihedral angel between the two coordination planes of Cu(1)-N(2)--O(4) and Cu(1 )-N( 1 )-O(3)) is 30.08(6)°.  相似文献   

19.
A new metal-organic coordination polymer [Cd(5-hip)(phen)]n·nH2O 1 has been hydro- ermally synthesized and characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. The crystal of the complex crystallizes in monoclinic, space group P2/n with a = 8.8071(17), b =12.386(2), c = 16.981(3) A, β = 100.182(2)°, V = 1823.2(6) A^3, Mr=. 490.73, Dc =1.788 g/cm^3,μ(MoKa) = 1.240 mm^-1, F(000) = 976, Z= 4, the final R = 0.0458 and wR = 0.1373 for 2864 observed reflections (I 〉 2σ(I)). The Cd atoms are coordinated by two N atoms from the phen ligands and four O atoms from 5-hydroxyisophthalate ligands in a highly distorted octahedral geometry.  相似文献   

20.
ABSTRACT A new 4-chlorobenzoic acid bridge Co(Ⅱ ) complex [[Co2(2,2'-bpy)2(μ-L)e(L)2(μ-H2O)] (HL = 4-chlorobenzoic acid) has been obtained by hydrothermal synthesis, and X-ray single-crystal diffraction analysis shows that it crystallizes in the monoclinic system, space group C2/c with a = 22.537(5), b = 16.212(3), c = 15.306(3) A, β= 124.37(3)°, V= 4616.1(16)A3, Mr = 1070.45, Dc = 1.540 g/cm3, Z = 4, p = 1.012 mm-1, F(000) = 2176, the final R = 0.0338 and wR= 0.0810. The title complex is composed of dinuclear [Co2(2,2'-bpy)2(μ-L)2(L)2(μ-HaO)] molecules. Each Co(Ⅱ ) atom is coordinated by two nitrogen atoms from one 2,2’-bipyridine ligand, three oxygen atoms from three 4-chlorobenzoic ions and another oxygen atom from one water molecule. The two Co(Ⅱ) atoms are connected by two 4-chlorobenzoic ions and one bridged water molecule. The dinuclear molecules are interlinked by hydrogen bond and π-π stacking interactions into a three-dimensional supramolecular network.  相似文献   

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