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1.
A new copper(H) complex [Cu2(DMF)(H2O)(C7H4NO4)2(C7H3NO4)]2-3.5DMF has been synthesized and its structure was determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1^- with a = 10.722(3), b = 18.170(4), c = 20.923(7)A,α = 105.297(9), β = 101.701(10), γ = 105.74(1)°, V= 3615(1)A^3, Z = 2, C58.50H64.50Cu4N1l.50O3150, Mr = 1686.90, Dc = 1.550 g/cm^3,μ= 1.255 mm^-1, F(000) = 1728.00, T = 150(2) K, the final R = 0.0640 and wR = 0.173 for 11310 observed reflections with I 〉 2σ(I). In the crystal, each formular unit consists of two dinuclear copper(H) compounds, between which the O-H…O hydrogen bonds exist. Each Cu^Ⅱ cation is six-coordinated in an octahedral geometry. The intermolecular hydrogenbonding interaction leads to a 3-D framework of the title compound.  相似文献   

2.
The title compound has been synthesized by the addition reaction of N-(4-cyanopyrazole-3-yl)-3,5-difluorophenyl-imine and diisopropyl phosphate. Its structure was confirmed by means of IR, ^1H NMR and elemental analysis. The single-crystal structure of the title compound was determined by X-ray crystallography. The compound crystallizes in monoclinic, space group C2/c with a = 18.9959(14), b = 9.2212(7), c = 22.1108(16)A^°, β= 90.1540(10)°, V = 3873.0(5) A^°^3, Dc = 1.366 g/cm^3, Z = 8, μ = 0.185, F(000) = 1664, and the final R = 0.0503 and wR = 0.1539 for 2996 observed reflections (I 〉 2σ(I)). The results demonstrate that the dihedral angle between the pyrazole and benzene rings is 105.5°, and there is a full delocalized pyrazole system with sp^2 hydridization of N(3). The crystal structure is stabilized by two intermolecular hydrogen bonds of N(1)-H(1)…O(3) and N(3)-H(3A)…N(4). The preliminary biological test shows that the title compound has a moderate antifungal activity.  相似文献   

3.
The new title compound N-(5-(4-chloro-2-(trifluoromethyl)phenyl)furan-2-carbon-yl)- N'-(4,6-dimethylpyrimidin-2-yl)thiourea (C19H14C1F3N4O2S) has been synthesized, and its crystal structure and biological behaviors were studied. The title compound crystallizes in the monoclinic system, space group P21/c with a = 7.932(5), b = 33.46(2), c = 7.556(5) A, β = 98.058(9)°, V = 1986(2) A^3 Mr = 454.85, Z = 4, Dc = 1.521 g/cm^3, μ = 0.349 mm^-1 and F(000) = 928. The structure was solved by direct methods and refined to R = 0.0724 and wR= 0.1429 for 3494 observed reflections (I 〉 2σ(I)). Intermolecular hydrogen bonds along the b axis together with the continuous π-π interactions construct the three-dimensional architecture of the title compound. The preliminary biological tests show definite herbicidalactivity for the title compound.  相似文献   

4.
A new infinite three-dimensional framework structure of the title compound [H6Mo^VI8O27]·3C4N2H10 has been synthesized under mild hydrothermal conditions and characterized by elemental analyses, IR, fluorescent spectra and single-crystal X-ray diffraction. C12H36Mo8N6O27 crystallizes in the triclinic system, space group P1^- with a = 8.820(3), b = 9.534(3), c = 10.993(4)A, α= 99.985(17), β = 106.65(2), γ= 101.650(14)°,V = 840.6(5)A^3, Mr = 1463.99, Z = 1, Dc = 2.892 g/cm^3,μ = 2.993 mm^-1, F(000) = 702, the final R = 0.0676, wR = 0.1920 and S = 1.074 for 2196 observed reflections with I 〉 2σ(I). The title compound exhibits a novel infinite three-dimensional (3D) framework composed of a [H6Mo^VI8O27] subunit and three dissociated piperazine fragments. The complex exhibits two strong fluorescent emission bands at ca. 417 and 440 nm (λex = 378nm) in the solid state at room temperature.  相似文献   

5.
The reaction of VO(acac)2 with 2-hydroxyl-1-naphthaldehyde isonicotinyl hydrazone and amines (ethylenediamine or diethylenetriamine) in CH3OH yields crystals of novel vanadium compounds characterized by IR, NMR spectroscopic methods and X-ray single-crystal structure determination. Two different vanadium units exist in the crystal cell of [VO2(C17H11N3O2)][VO- (C4H13N3)(C6H5N3O)](C2H5OH) which crystallizes in the triclinic system, space group P1 with a = 8.0104(17), b = 13.898(3), c = 14.955(3)A, α = 89.103(4), β = 79.551(4), γ = 78.352(4)°, V = 1603.3(6)A^3, Mr = 723.54, Dc = 1.499 g/cm^3, Z = 2, λ(MoKα) = 0.71073 ]A,μ= 0.644 mm^-1, F(000) = 748, the final R = 0.0547 and wR = 0.0997 for 8920 observed reflections with I 〉 2σ(I). According to structure analysis, two different molecules are arranged in the lattice and the two vanadium atoms adopt octahedral and square pyramidal coordination geometries, respectively. The interactions between DNA and vanadium complexes have been investigated by UV-Vis absorption spectro- photometry.  相似文献   

6.
The novel mixed-ligand neutral compound [Mo3O4(C2O4)2bipy-(H2O)3]·EtOH·2H2O(bipy = 2,2′-bipyridine) has been prepared by the reaction of oxalic acid elution of Mo(IV) and bipy, and characterized by single-crystal X-ray diffraction analysis and IR. The crystal is of triclinic, space groups P1^- with a = 9.5520(2), b = 10.3730(1), c = 13.5722(2)A, a = 74.940(12),β = 80.772(14),γ= 69.898(11)°, V = 1215.73(11)A^3, Z = 2, C16H24Mo3N2O18, Mr = 820.19, Dc = 2.241 g/cm^3,μ = 1.616 mm^-1, F(000) = 808, T = 293(2) K, the final R = 0.0424 and wR = 0.0939 for 4119 observed reflections with I 〉 2σ(I). The trinuclear unit is coordinated by mixed ligands of oxalate and bipy. The intermolecular hydrogen bonding interactions among adjacent [Mo3O4(C2O4)2·bipy(H2O)3] extend the compound into a three-dimensional supramolecular framework. The uncoordinated water molecules and ethal molecules act as space-fillers and consolidate the whole architecture through hydrogen bonding interactions.  相似文献   

7.
The title compound, N,N'-bis-[3-chloro-5-S-(l-menthyloxy)-2(5H)-4-furanon-yl]- propane-l,3-diamine (C31H48Cl2N2O6, Mr = 615.61), has been synthesized and characterized by IR, 1H NMR, MS, elemental analysis and single-crystal X-ray diffraction. The crystal crystallizes in the monoclinic system, space group C2 with a = 16.1091(4), b = 11.1880(3), c = 19.2854(5) A, β = 106.297(2)°, V = 3336.12(15) A3, Z = 4, Dc = 1.226 mg/m3,μ = 0.237 mm^-1, F(000) = 1320, the final R = 0.0531 and wR = 0.0700 for 2760 observed reflections (I 〉 2σ(I)). X-ray analysis reveals that the title compound possesses four rings: two chiral five-membered furanone rings and two six-membered cyclohexane rings with chair conformation, containing eight chiral centers: C2(S), C3(R), C5(R), C10(S), C18(S), C21(R), C22(S) and C25(R). The structure is stabilized by N-H…O hydrogen bonding interaction.  相似文献   

8.
A supramolecular compound (C6H6NO2)3(C6H5NO2)(PW12O40)·2H2O including the Keggin-type [PW1O40]3- polyanion, [HC6H5NO2]+ (protonated pyridine-4-carboxylic acid molecule), C6H5NO2 (pyridine-4-carboxylic acid molecule) and two free H20 molecules has been synthesized by the hydrothermal method and characterized by elemental analysis, IR spectra, single-crystal X-ray diffraction and powder X-ray diffraction. The crystal belongs to orthorhombic, space group Pnnm with a = 1.0483(3), b = 1.4368(6), c = 2.0526(7) nm, V= 3.0918(18) nm3,Z = 2, F(000) = 3004, Mr= 3406.07, Dc= 1.757 g.m-3,μ = 41.241 mm-1, the final R = 0.0387 and wR = 0.1089 for 2091 observed reflections withI〉 2σ(I). A total of 30431 reflections were collected, of which 3083 were independent (Rint = 0.0605). S is 1.182. The title compound presents a 3-D structure via intermolecular hydrogen bonds among [PW12O40]3- polyanions and pyridine-4-carboxylic acid ligands. The ultraviolet and luminescence spectra have been studied at room temperature, of which the purple fluorescent emission is located at 363 nm when excited at 264 nm. Fluorescent emission of the compound derives from the π-π* transitions in the pyridine-4-carboxylic acid ligands.  相似文献   

9.
A new heteropolyoxotungstate [(C2H4N2)4(P4Co3W4O28H6)(H2C2O4)]n with a three-dimensional framework was hydrothermally synthesized.The compound crystallizes in a tetragonal system,space group I41/a with a = 17.1006(17),b = 17.1006(7),c = 10.7525(5),V = 3144.2(2)3,Z = 4,Dc = 3.795 g·cm-3,F(000) = 3300,MoKα(λ = 0.71073 ),μ = 16.460 mm-1,the final R = 0.0335 and wR = 0.0776.In the heteropolyoxotungstate,tungsten-oxygen octahedra are linked by sharing two cis-vertexes into an infinite helical chain extending along the c axis.Cobalt atoms in the octahedral geometry act as the linkers of these chains,forming a three-dimensional framework.The cobalt and phosphorus atoms in the tetrahedral geometry play a role in stabilizing the three-dimensional framework.Ethylenediamine molecules are polymerized into organic chains which locate in the interspaces of the framework in the way of interwinding with the W-O chains.  相似文献   

10.
Under hydrothermal condition, the reaction of 2-naphthoxyacetic acid with ZnCl2 and 4,4′-bipyridine (4,4′-bipy) has afforded a new Zn(Ⅱ) compound, [Zn(C12H9O3)2(C10H8N2)]n·nH2O1, which was structurally characterized by single-crystal X-ray diffraction analysis. The crystal is of monoclinic, space group P21/c with a = 7.7335(2), b = 19.3834(4), c = 20.1707(4) A, β = 104.9830(10)°, V = 2920.82(11) A^3, C34H28ZnN2O7, Mr = 641.95, Z = 4, Dc = 1.460 g/cm^3,μ = 0.895 mm^-1, F(000) = 1328, R = 0.0406 and wR = 0.0876 for 4417 observed reflections (I〉 2σ(I)) Complex 1 consists of one-dimensional zigzag chains deriving from Zn(C12H9O3)2 units linked by 4,4′-bipy ligands, and lattice water molecules decorate between the chains. Non-covalent interactions, such as hydrogen-bonding and aromatic π-π interactions, lead to the formation of a 3D network structure. The thermogravimetric analysis (TGA) and luminescent property for 1 have also been studied in this paper.  相似文献   

11.
王永净  徐立 《结构化学》2008,27(3):297-300
A new bismuth compound Bi(Hsal)3(1,10-phenanthroline) (Hsal = O2CC6H4-2-OH) has been synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in the triclinic system, space group P1, with a = 10.243(2), b = 11.905(3), c = 12.934(3) A, α= 76.780(6), β= 68.683(6),γ= 80.930(7)°, V = 1425.6(5) A^3, Dc = 1.865 g/cm^3, Mr = 800.51, F(000) = 780, μ= 6.247 mm^-1, Z = 2, R = 0.0456 and wR = 0.1131 for 5612 observed reflections (I 〉 2σ(I)). In this compound, three salicylate ligands coordinate to the Bi atom through the carboxylate groups to form a four-membered chelate ring, and phenanthroline ligand chelates the metal through two N atoms. The structure of the title compound manifests a possible coordination mode between bismuth subsalicylate and N atom containing amino acid in the biological system.  相似文献   

12.
李正义  来源  石嵩  韩辰  陈亮  孙小强 《结构化学》2013,(9):1387-1391
The title compound 5,17-diformyl-11,23-di(tert-butyl)-25,26,27,28-tetrapropoxycalix[4]arene has been synthesized by selective formylation of 5,11,17,23-tetra(tert-butyl)25,26,27,28-tetrahydroxycalix[4]arene in three steps and characterized by1H NMR and X-ray single-crystal diffraction.The crystal belongs to the monoclinic system,space group C2/c with a = 25.760(3),b = 10.9952(10),c = 18.630(2),β = 119.985(4)°,V = 4570.4(9)3,Z = 4,Dc = 1.106 g/cm3,Mr = 761.01,F(000) = 1648,μ = 0.071 mm-1,MoKa radiation(λ = 0.71073),R = 0.0710 and wR = 0.2411 for 3234 observed reflections with I 2σ(I).X-ray analysis reveals that the title compound adopts a pinched cone conformation which leads to an open cavity.Intermolecular C–H O weak interactions link the molecules along the bc plane,which are effective in the stabilization of the crystal structure.  相似文献   

13.
段文增  冯帅  孙斌  吴仁涛 《结构化学》2009,28(10):1290-1295
The title compound [2-(2,6-dioxacyclohexyl)-5-methoxylphenols]2 was synthesized by the reaction of 2-hydroxyl-3-methoxylbenzaldehyde and 1,3-propanediol in the presence of DMF-DMS adduct and characterized by IR spectrum, UV-Vis spectrum and X-ray crystallography. The title compound belongs to monoclinic, space group P21 with a = 9.8967(10), b = 8.2240(9), c = 13.3654(14) A^°, β= 90.016(2)°, C11H14O4, Mr = 210.22, V = 1087.8(2)A^°3, Z = 4, Dc = 1.284 Mg/m^3, F(000) = 448,μ = 0.098 mm^-1, the final R = 0.0300 and wR = 0.0761 for 2070 observed reflections with I 〉 2σ(I). The molecules are connected via intermolecular O-H…O hydrogen bonds into a 2D network structure. Moreover, theoretical investigations of the title compound with HF/6-31G(d) method were performed, and its stability, frontier molecular orbital composition and Mulliken charge distribution were also discussed. The compound is a bis-molecule. The two molecules stay together and could not be separated. Two crystallographically independent molecules exist in an asymmetric unit. The bond lengths and bond angles of the two molecules are slightly different with each other.  相似文献   

14.
A novel ionic compound [Fe(CN)6·(PhCHeNC9H7)4]·12H2O
(C70H80FeN10O12, Mr = 1309.29) has been synthesized and its structure was characterized by I-R, elemental analysis and X-ray diffraction. The compound crystaUizes in triclinic, space group P1, with a = 10.968(7), b = 11.466(7), c = 14.077(8)A, α= 87.014(7), β= 78.124(7), γ = 72.708(7)°, V = 1654.1(17)A3, Z = 1, Dc = 1.314 g·cm^-3, F(000) = 692, p = 0.298 mm^-1, the final R = 0.0519 and wR = 0.1355. The building unit of the title compound consists of four (PhCH2N+C9H7) ions, one [Fe(CN)6]4- anion, and a dozen water molecules. According to the structural analysis, [Fe(CN)6]4- ions are linked together by O-H…O and O-H…N hydrogen bonds, while (PhCH2N+C9HT) and [Fe(CN)6]4- ions interact with each other by electrostatic force to form an ionic compound.  相似文献   

15.
YANG  Ying-Qun ZHANG  Shao-Hua LI  Wei 《结构化学》2013,(11):1663-1666
A new Cd(II) complex [Cd(C12H6OaN2)(Phen)ffH2O)]'3H2O with 2,2"-bipyridine- 3,3"-dicarboxylic acid as a ligand has been synthesized. Crystal data for the title complex are as follows: monoclinic, space group P2dn, a = 12.8458(5), b = 17.9131(7), c = 15.2960(6) A, β = 111.7430(10)°, V = 3269.3(2) A3, Dc = 1.581 g/cm3, Z = 4,/a(MoKa) = 0.731 mm-1, F(000) = 1580, the R = 0.0244 and wR = 0.0605. In the title complex, the central Cd(ll) ion is located in a distorted octahedral coordination environment. The electrochemical and fluorescent properties of the title complex were studied. The results show that the electron transfer of the title complex is irreversible in the electrode reaction and it has a broad emission peak in the range of 470-508 nm with the excitation wavelength of 488 nm.  相似文献   

16.
The title compound, [Cu3(dmpzm)4(μ-1,3-dca)2(dca)4]·2H2O (dmpzm = 1,1'-methylenebis(3,5-dimethyl-lH-pyrazole), dca = dicyanamide) 1·2H2O, was synthesized via the reaction of CuCl2·2H2O with dmpzm and Na(dca), and characterized by elemental analysis and IR spectra. 1·2H2O crystallizes in the monoclinic system, space group C2/m with a = 13.578(3), b = 16.769(3), c = 14.769(3) A, β = 104.10(3)° V = 3261.4(11) A^3, Z = 2, Dc = 1.466 g/cm^3, T = 153(2) K, C56H68N34O2Cu3, Mr = 1440.09, F(000) = 1490,μ(MoKa) = 1.040 mm^-1, S = 1.150, R = 0.0553 and wR = 0.1123 for 2744 observed reflections with I 〉 2σ(I). The central copper atom is chelated by two dmpzm ligands and coordinated by two bridging dca anions, forming a slightly distorted octahedral geometry. The two external copper atoms adopt a square-pyramidal coordination geometry, coordinated by one chelating dmpzm ligand and one bridging and two terminal dca anions. Two intermolecular hydrogen bonding interactions result in the formation of a 2D (4,4) hydrogen-bonded network.  相似文献   

17.
The title compound 3,3'-(2,2'-(ethane-1,2-diylbis(oxy))bis(ethane-2,1-diyl))bis(2- (4-chlorophenylamino)quinazolin-4(3H)-one) 3 (C34H30CI2N604, Mr = 657.54) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in space group P1 with a = 9.9185(8), b = 10.6124(9), c = 15.4064(13) A, α = 92.896(2),β = 103.813(2), γ= 94.635(2)°, V= 1565.5(2) A3, Z = 2, Dc = 1.395 g/cm^3,μ = 0.257 mm^-1, F(000) = 684, the final R = 0.0580 and wR = 0.1284 for 3400 observed reflections (I〉 2σ(I). It remains triclinic in the crystal. Intra- and intermolecular N(3)-H(3A)…O(2), N(6)-H(6A)…O(3) and C(19)-H(19A)…O(4) #1 (#1: 1-x, 1-y, -z) hydrogen bonds are observed in the title compound. A two-dimensional chain network is formed from the dimmers and intermolecular π-π interactions in the crystal structure. This open network has solvent-accessible voids (10A3).  相似文献   

18.
The title compound (E)-2-[(4-tert-butyl-5-(4-methoxybenzyl)thiazol-2-ylimino)methyl]phenol was synthesized by the reaction of 5-(4-methoxybenzyl)-4-tert- butylthiazol-2-amine with salicylaldehyde, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 5.9362(8), b = 11.5070(15), c = 29.460(4)A, β= 97.326(3)°, V = 1995.9(5) A^3, Z = 4, F(000) = 808, C22H24N2O2S, Mr= 380.49, De= 1.266 g/cm^3, S = 1.031,μ = 0.181 mm^-1, the final R = 0.0474 and wR = 0.1441 for 4327 observed reflections (I 〉 2σ(I)). Intramolecular O-H…N hydrogen bond is observed in the crystal. The preliminary bioassay showed that the title compound exhibits 95% inhibition rate against Rhizoctonia solani at the test concentration of 500 mg/L.  相似文献   

19.
The title compound (Z)-1-(3-fluorobenzyl)-5-((3-fluorobenzylimino)(2-hydroxy-4- methoxyphenyl)methyl)pyridin-2(1H)-one (C27H22F2N2O3,Mr = 460.47) was synthesized and crystallized. The crystal belongs to the triclinic system,space group P1 with a = 9.951(6),b = 10.059(6),c = 12.927(7)A,α = 109.828(7),β = 102.304(7),γ = 104.898(7)°,Z = 2,V = 1110.2(11)A^3,Dc =1.377 Mg/m^3,μ(MoKα) = 0.102 mm^-1,F(000) = 480,the final R = 0.0449 and Rw = 0.1250 for 4595 observed reflections (I 〉 2σ(I)). X-ray analysis reveals that both m-fluorobenzyl groups are diorientationally disordered because of the rotation of C–C single bond which was represented as F(1),F(2) and F(1'),F(2'). The diorientational disorder was refined and gave the occupancies of 0.665(4) and 0.335(4) for F(1) and F(1'),0.631(3) and 0.369(3) for F(2) and F(2'). Hydrogen bonds existing in the cell link different components to stabilize the crystal structure. The active data proved that the title compound has good anti-HBV activity.  相似文献   

20.
The title Schiff base compound 4-bromo-2-[(3-methylpyridin-2-ylimino)methyl]phenol was prepared and structurally characterized by elemental analysis, IR spectrum, and single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P2 1/n, with a = 4.4870(9), b = 19.953(4), c = 13.860(3)A, β = 93.13(3)°, V = 1239.0(4)A3 Z = 4, Dc = 1.561 g/cm3, C13H11BrN2O2 , Mr = 291.15, p = 3.302 mm-1 and F(000) = 584. The final refinement gave R = 0.0608 and wR = 0.1377 for 1329 observed reflections with I 〉 2σ(I). X-ray diffraction reveals that the non-hydrogen atoms in the compound are nearly coplanar, with the mean deviation of 0.0197A from the plane. The molecule adopts an E configuration about the central C=N functional bond. The compound possesses moderate antimicrobial property.  相似文献   

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