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1.
Single crystals of 1-cyclohexylpiperazine-1,4-diium dichromate(VI), (C10H22N2)[Cr2O7], were obtained by slow evaporation at room temperature from an aqueous solution of potassium dichromate, hydrochloric acid and 1-cyclohexylpiperazine. (C10H22N2)[Cr2O7] is triclinic (P\(\bar 1\)) with a = 10.351(2) Å, b = 12.766(3) Å, c = 6.111(1) Å, α = 91.50(2)°, β = 104.26(3)°, γ = 94.91(2)°, V = 778.8(3) Å3, and Z = 2. The structure determination performed from single crystal X-ray diffraction data leads to R1/wR2 reliability factors of 0.032/0.078. The asymmetric unit of the title salt C10H22N22+·Cr2O72?, consists of one 1-cyclohexylpiperazine-1,4-diium dication and one dichromate dianion. These entities are linked together by N–H···O hydrogen bonds to form {(C10H22N2)[Cr2O7]}n infinite chains lying parallel to the (100) plane and running along the c axis. The intermolecular N–H···O hydrogen bonds link these chains into a two-dimensional network structure consolidated through C–H···O weak interactions.  相似文献   

2.
Oxidation of N-aminophthalimide with lead tetraacetate in the presence of 1,5-diaryl-3-[(E)-2-arylethenyl]-1H-pyrazoles, as well as of 1,3-diphenyl-5-[(E)-2-phenylethenyl]-1H-pyrazole, gives adducts at the exocyclic C=C bond, the corresponding phthalimidoaziridinylpyrazoles. From 1,5-diphenyl-3-[(1E,3E)-4-phenyl-1,3-butadienyl]-1H-pyrazole, only product of addition at both exocyclic C=C bonds was obtained. In the reaction with 1-phenyl-3-[(1E, 3E)-4-phenyl-1,3-butadienyl]-5-[(E)-2-phenylethenyl]-1H-pyrazole, the adduct at the styryl C=C bond was isolated. Analogous 4,5-dihydropyrazoles, 1,5-diphenyl-3-[(1E, 3E)-4-phenyl-1,3-butadienyl]-4,5-dihydro-1H-pyrazole and 1-phenyl-3-[(1E, 3E)-4-phenyl-1,3-butadienyl]-5-[(E)-2-phenylethenyl]-4,5-dihydro-1H-pyrazole, turned out to be inert in oxidative addition of N-aminophthalimide.  相似文献   

3.
The synthesis, IR spectroscopic study, and X-ray diffraction analysis (CIF file CCDC no. 1574078) are carried out for 1,3-diamino-2-hydroxypropane-N,N,N′,N′-tetraacetic acid (I). The structural units of a crystal of compound I are (H4.5HPdta)0.5– anions, (H5.5HPdta)0.5+ cations, and molecules of water of crystallization joined by a branched network of hydrogen bonds: strong intermolecular O–H…O and intramolecular N–H…O bonds.  相似文献   

4.
According to the data of quantum-chemical calculations and IR spectroscopy the trifluoro-N-(2-phenylacetyl)methanesulfonamide CF3SO2NHC(O)CH2Ph in the isolated state and in inert media exists in the form of two conformers with the syn- and antiperiplanar orientation of the C=O and N-H bonds. Its self-associates in the CCl4 solution and in molecular crystals constitute cyclic dimers formed by the NH···O=S bonds and chain dimers with the NH···O=C bonds. As a hydrogen bond donor, trifluoro-N-(2-phenylacetyl)methanesulfonamide is stronger than N-methyltrifluoromethanesulfonamide. Its pK a in methanol is 5.45, that is 5 pK units lower than for amides CF3SO2NHR and 2 pK units higher than for imide (CF3SO2)2NH.  相似文献   

5.
A new coordination polymer, [Cd(HMal)(Bipy)(H2O) · 2H2O (I) (H3Mal is malic acid, Bipy is 4,4′-bipyridine), has been synthesized from H3Mal and Bipy under hydrothermal conditions and characterized by elemental analysis, IR, TG, and single-crystal X-ray diffraction. The X-ray diffraction analysis reveals that I (C14H16N2O7Cd) crystallizes in the orthorhombic system, space group Ibam. The adjacent cadmium(II) atoms were first interconnected by the HMal ligands via carboxylate oxygen atoms and its adjacent hydroxyl group to generate an infinite zigzag [Cd(HMal)] n chain, which are further linked by Bipy ligands to form a 2D wavelike layer. Interestingly, the adjacent layers are further connected via hydrogen bonds, giving rise to a 3D porous framework with a cross-sectional area of 11.690 × 9.326 Å2. The unit cell parameters for I: a = 8,457(1), b = 22.030(7), c = 23.066(7) V = 4297(2) Å3, Z = 4.  相似文献   

6.
A one-dimensional zinc(II) polymer, {[Zn2((p-FPhHIDC)(p-FPhH2IDC)2)(Phen)2] · H2O} n (I) (p-FPhH3IDC = 2-(p-fluorophenyl)-1H-imidazole-4,5-dicarboxylicacid (Phen = 1,10-phenanthroline), has been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction (CIF file CCDC no. 1063532), elemental analyses, and IR spectra. In polymer I, these 1D wave chains were joined through the π–π interactions and intermolecular hydrogen bonds to give a 2D architecture. The thermal properties of I have been determined in air.  相似文献   

7.
A new copper(II) complex of 1,10-phenanthroline (C12H8N2) and the meta-aminobenzoate ion (m-amb; C7H6NO 2 ? ), having the formula Cu(C12H8N2)(C7H6NO2)Cl?0.5H2O, is prepared and characterized by elemental analysis, IR spectroscopy, and single crystal X-ray diffraction. The structure is built up from monomeric units in which the coordination environment around the metal ion is a square plane arising from a bidentate 1,10-phenanthroline molecule, a monodentate m-amb anion, and a chloride ion. A very long (Cu–N = 2.856(5) Å) bond to the nitrogen atom of an adjacent m-amb ion generates [101] polymeric chains in the crystal. The crystal structure is consolidated by N–H???O and O–H???O hydrogen bonds and C–H???O, C–H???Cl, and aromatic π–π stacking interactions. Crystal data: C19H15ClCuN3O2.5, M r = 424.33, monoclinic, P21/n (No. 14), a = 9.8200(5) Å, b = 10.9291(7) Å, c = 16.3803(9) Å, β = 105.293(3)°, V = 1695.74(17) Å3, Z = 4, R(F) = 0.043, wR(F 2) = 0.122.  相似文献   

8.
The methods of IR spectroscopy and quantum chemistry (B3LYP/DGDZVP) were applied to investigation of the types of self-associates formed in solutions of N-(2-hydroxy-3,8-diiodocyclooctyl)trifluoroacetamide and N-(4-iodo-2,2,5,5-tetramethyltetrahydrofuran-3-yl)trifluoroacetamide in CCl4 by means of hydrogen bonding. The ОН group of N-(2-hydroxy-3,8-diiodocyclooctyl)trifluoroacetamide participates in the formation of intramolecular hydrogen bond ОH···О=С, while chain dimers are formed due to interactions between the NH and С=О groups of the neighboring molecules. Due to the formation of the intramolecular bond, the dimers of N-(2-hydroxy-3,8-diiodocyclooctyl)trifluoroacetamide are energetically less stable than the chain dimer of N-(4-iodo-2,2,5,5-tetramethyltetrahydrofuran-3-yl)trifluoroacetamide.  相似文献   

9.
A new zinc(II) complex Zn(H3Pimda)2] · H2O (I), where H3Pimda = 2-Propyl-1H-imidazole-4, 5-dicarboxylic acid, has been synthesized and characterized by elemental analysis, IR spectroscopy and X-ray single-crystal diffraction. It crystallizes in the triclinic system, space group P \(\bar 1\), with a = 8.397(3), b = 11.271(4), c = 12.312(5)Å, α = 70.432(5), β = 70.984(5), γ = 74.897(5)°, V = 1022.9(7) Å3, M r = 475.71, Z = 2, ρ c = 1.695 g/cm3, F(000) = 488, μ = 1.151 mm?1, R = 0.0659 and Rw =0.1525 for 3769 observed reflections. The hydrogen bonding derived from the coordinated waters connects the mononuclear zinc complex units into a one-dimensional chain, and these chains are further linked by intermolecular hydrogen bonds into a 2D supramolecular network. Complex I also displays strong photoluminescence properties in the liquid state at room temperature.  相似文献   

10.
A novel coordination polymer [Co5(OH)2(dnbpdc)4(H2O)6]·16H2O (1) (dnbpdc = 6,6′-dinitro-4,4′-biphenyldicarboxylic acid) is obtained from a hydrothermal reaction. The structure of complex 1 is characterized by elemental analysis, IR spectroscopy, and single crystal X-ray diffraction analysis. The title compound (C56H70Co5N8O56, M r = 2045.85) crystallizes in the triclinic space group P-1 with a = 11.9349(2) Å, b = 12.1895(2) Å, c = 15.420(2) Å, α = 109.390(7)°, β = 94.786(1)°, γ = 108.027(9)°, V = 1968.4(4) Å3, Z = 1, D c = 1.726 g/cm3, F(000) = 1045, μ(MoK α) = 1.154 mm–1, T = 133(2) K, the final R = 0.0316 and wR = 0.0692 for 7032 observed reflections with I > 2σ(I). The coordination polymer is built of a pentanuclear Co(II) cluster, four dnbpdc ligands, two hydroxyl groups, six coordination water and sixteen crystal water molecules. Ligand oxygen atoms exhibit three types of coordination modes (monodentate, syn-syn bridging bidentate and bridging tridentate). Moreover, the infinite three-dimensional supramolecular network is generated by coordination and hydrogen bonds. The thermal stability of complex 1 is evaluated by differential scanning calorimetry and thermogravimetric analysis.  相似文献   

11.
The reaction of CuCl2 · 2H2O with N-(pyridine-3-sulfonyl amino)-acetate (H2L) in ethanol, water and 4,4′-Bipy under solvothermal conditions leads to the formation of a dinuclear copper polymer {[Cu2(L)2(4,4′-Bipy)(H2O)2] · H2O · CH3OH} n (I). The polymer was characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis, and X-ray single-crystal diffraction (CIF file CCDC no. 1543747). The results showed that polymer belongs to the triclinic system, \(P\bar 1\) space group. TG curve shows that polymer I first removes water molecules, and then the ligand split for polymers I, and the remained residue is CuO. The magnetic measurement reveals the N-(pyridine-3-sulfonyl amino)-acetate as bridge ligand can mediate the antiferromagnetic coupling interaction between magnetic centers.  相似文献   

12.
A novel organic-inorganic hybrid compound based on weak intermolecular interactions formulated as Ni(H2Bibzim)3Cl2 · 2H2O (H2Bibzim = 2,2-bibenzimidazole, formula, C14H10N4) has been synthesized under hydrothermal conditions and characterized by elemental analysis, single-crystal X-ray diffraction analyses, and IR spectra. It crystallizes in the orthorhombic system, space group Pbcn, Z = 2, a = 20.8530(19), b = 15.7838(14), c = 12.3159(11) Å, V = 4053.7(6) Å3, M r = 1736.84, ρc = 1.423g/cm3, λ = 0.71073 Å, μ(MoK α) = 0.664 mm?1, F(000) = 1792, R = 0.0283 and wR = 0.0707 for 3746 observed reflections with I > 2σ(I). The complex is composed of mononuclear cations [Ni(H2Bibzim)3]2+, chlorine anions, and lattice water molecules, which are linked into a two-dimensional supramolecular architectures via hydrogen bonds and π-π-stacking interactions.  相似文献   

13.
A new cobalt(II) coordination polymer, namely [Co(L)(Ndc)] n (I), where L = 1,5-bis(5,6- dimethylbenzimidazole)pentane, H2Ndc = 2,6-naphthalenedicarboxylic acid, was synthesized and characterized by elemental analysis, IR spectra, powder X-ray diffraction and single-crystal X-ray diffraction (CIF file CCDC no. 1548044). Complex I displays a 2D (4,4) layer which further extended into a 3D supramolecular framework via weak C–H···O hydrogen bondings. The luminescence explorations demonstrated that I exhibits highly selective and sensitive sensing for Cr2O 7 2? with high quenching efficiency Ksv value of 9.87 × 103 L mol?1 and low detection limit (0.24 μM (S/N = 3)). Meanwhile I also exhibits highly selective and sensitive sensing for Fe3+ with quenching efficiency Ksv = 3.6 × 104 L mol–1 and low detection limit (0.32 μM (S/N = 3)). Complex I exhibits higher photocatalytic activities for the degradation of methylene blue under UV irradiation. Additionally, the thermal behavior and electrochemical properties of the compound are also presented.  相似文献   

14.
Potassium peroxypentafluorotantalate monohydrate K2TaO2F5 · H2O was synthesized by the introduction of hydrogen peroxide and potassium chloride into highly pure tantalum-containing fluoride solutions at 70°C followed by cooling of the mixture to room temperature at a rate of 10–15 K/h. The X-ray diffraction analysis revealed that K2TaO2F5 · H2O crystallized in the monoclinic crystal system with the following unit cell parameters: a = 8.965(2) Å, b = 8.966(2) Å, c = 9.257(2) Å, β = 99.78(3) °, Z = 4, V unit cell = 733.3(5) Å3, ρcalcd = 3.681 g/cm3, FW = 404.13, space group C 2 3 = C2(5). The thermolysis of K2TaO2F5 · H2O was studied at 160–1000°C, and the phases formed under specified conditions were determined.  相似文献   

15.
The crystal structure of an antimony(III) fluoride complex of the composition (C5H12NO2)SbF4·H2O (I) involving a cation of α-amino isovaleric acid (DL-valine, Val) is determined. Crystals are monoclinic: a = 12.2024(2) Å, b = 6.1636(1) Å, c = 15.5167(3) Å, Z = 4, space group P21/c. The structure is formed of DL-valinium (C5H12NO2)+ cations, complex [SbF4]nn? anions having a polymeric chain structure, and crystallization water molecules. The [SbF4]nn? complex anions consist of trigonal SbF4E bipyramids joined together by asymmetric bridging Sb–F(3)···Sb bonds. The structural units are organized into a threedimensional framework via N–H···F, N–H···O, and O–H···F hydrogen bonds.  相似文献   

16.
A coordination polymer “[Mn(PDB)(H2O)2] · H2O” n (I) (H2PDB = pyridine-3,4-dicarboxylic acid) was hydrothermally synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal of complex I are triclinic: C7H9NMnO7, M = 274.09; a = 7.2389(18), b = 8.045(2), c = 9.157(2) Å, α = 75.421(12)° β = 68.092(9)°, γ = 76.021(12)°, V = 1472.3(2) Å3, Z = 2, ρ c = 1.927 g/cm3, μ = 1.420 mm?1, space group P \(\bar 1\) F(000) = 278, R = 0.0253 and wR = 0.0621 for 1709 observed reflections (I>2σ(I)). X-ray diffraction structure analyses reveal that two-dimensional layers were formed as bridged by PDB, and further assembled into the three-dimensional framework supramolecular structure via hydrogen bonding interaction. Magnetic susceptibility measurements reveal an antiferromagnetic interaction in I.  相似文献   

17.
Two novel μ-oxo-di-μ-carboxylato-bridged iron(III) complexes of [Fe2(bpea)2(PhCO2)2(μ-O)] (ClO4)2·C2H5OH (1) and [Fe2(bpma)2(ClCH2COO)2(μ-O)](ClO4)2· H2O (2) (bpea = N,N-bis(2-pyridylmethyl)ethylamine, bpma = N,N-bis(2-pyridylmethyl)methylamine), have been synthesized and determined by X-ray diffraction. Complex (1) crystallizes in the Orthorhombic space group P nma with d(Fe···Fe) of 3.094 Å and average d(Fe–Obbridge) of 1.805 Å; Complex (2) crystallizes in the Monoclinic space group C 2/c, with d(Fe···Fe) of 3.109 Å and average d(Fe–Obbridge) of 1.794 Å. The magnetic studies indicate a stronger antiferromagnetic interaction between iron(III) ions through μ-oxo-di-μ-carboxylato-bridge for complex (1), with J = ? 141.6 cm?1.  相似文献   

18.
Two crystalline polymorphic forms of α-(N-benzoxazolin-2-one)acetic acid (BAA) are prepared by changing the temperature of its crystallization from solution in ethanol. Crystallographic data of the α-form are determined: a = 12.7769(17) Å, b = 8.2574(9) Å, c = 16.7390(19) Å, β = 105.087(13)°, space group C2/c, V = 1705.2(4) Å3, and Z = 8, while those of β form are a = 5.2854(4) Å, b = 5.9880(4) Å, c = 13.4509(5) Å, β = 94.666(4)°, space group P21, V = 424.30(4) Å3, and Z = 2. It is found that BAA molecules of the α form combine into infinite one-dimensional chains arranged along axis b by means of O?H···O and C?H···O hydrogen bonds, and these chains are crosslinked via C?H···O hydrogen bonds to form a threedimensional structure. The β form has another system of hydrogen bonds, one of which is bifurcated (O4···O2, O4···O3), and the π–π-interactions between the benzoxazolinone fragments of BAA molecules combined into a chain also arranged along axis b are observed. Calorimetric analysis shows that the polymorphic transition from the α form to the β form occurs at 129°C.  相似文献   

19.
The X-ray analysis of a single crystal of Mg(C12H13N4O4S)2·11H2O, where (C12H13N4O4S)? is the anion of 4-p-aminobenzenesulfamido-2,6-dimethoxypyrimidine (sulfadimethoxine) is carried out. Unit cell parameters are: a = 19.753(4) Å, b = 34.031(7) Å, c = 13.859(3) Å; β = 125.37(3)°, C2/c, Z = 8, R(F) = 0.042. The structure is built of [Mg(OH2)6]2+, (C12H13N4O4S)?, and water molecules and corresponds to the formula [Mg(OH2)6](C12H13N4O4S)2·5H2O. The IR bands of νasymSO2 and νsymSO2 are bathochromically shifted as a result of their participation in hydrogen bonding, and not because of any direct coordination of sulfadimethoxinate anion to the complexing atom through oxygen.  相似文献   

20.
One new trinuclear nickel(II) cluster with a Ni3(μ 3-OH) core was synthesized by the method of in situ one pot synthesis. The complex [Ni3(μ 3-OH)(cpza)3]Cl2·H2O (1) (where Hcpza is N-(4-cyano-1H-pyrazol-3-yl)acetamide) was characterized by single-crystal X-ray diffraction methods, elemental analyses, IR spectroscopy and Hirshfeld surface analysis. For complex 1, the crystal structure is extended into 3D structure through N–H···O and O–H···Cl hydrogen bonds. According to the 3D Hirshfeld surface and 2D fingerprint plots, the main interactions in the cluster are the H···H, N···H and O···H contacts.  相似文献   

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