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1.
A novel europium(III) complex, [Eu(C7H5O2)2(C7H6O2)2(C12H8N2)2Cl], was synthesized and characterized by elemental analysis and single-crystal X-ray determination. It crystallizes in the monoclinic system, space group Cc with a = 17.2814(16), b = 17.9421(17), c = 14.9971(14) Å, β = 101.6510(10)°, Z = 4, ρ c = 1.508 g/cm3, μ = 1.496 mm?1, the final R = 0.0516 and wR = 0.1267 for 6435 observed reflections with I > 2σ(I). Structural analysis shows that the Eu(III) atom is nine-coordinated by one chlorine atom, four N atoms of two 1,10-phenanthroline (Phen) ligands, and four O atoms from four carboxybenzene ligands, to form a distorted tricapped trigonal prism. The luminescence spectrum of the complex indicates that the intensity of the emission wavelength at 612 nm is strongest among all emission wavelengths and the second phen ligand shows an enhancement effect on the luminescence of the complex.  相似文献   

2.
New compounds of sparfloxacin (C19H22F2N4O3, SfH) and levofloxacin (C18H20FN3O4, LevoH) with mineral acids, namely, sparfloxacinium bromide (SfH · HBr, I) and levofloxacindium diperchlorate (LevoH · 2HClO4, II), have been synthesized and characterized by X-ray diffraction. Crystallographic data are a = 7.7151(7) Å, b = 26.109(3) Å, с = 10.008(1) Å, β = 103.556(1)°, V = 1959.7(3) Å3, space group P21/n, Z = 4 for I and a = 9.727(6) Å, b = 20.440(12) Å, с = 12.286(7) Å, β = 104.327(8)°, V = 2367(2)Å3, space group P21, Z = 4 for II. The structures of these compounds are stabilized by intra- and intermolecular hydrogen bonds and π–π interaction between SfH2+ or LevoH32+ ions.  相似文献   

3.
The trans(O)-cis(C)-bis(pyridine-2-carboxylato)dicyanocobaltate(III) ions, [Co(Pic)2(CN)2]?, crystallize from acid medium with three water molecules per two crystallographically nonequivalent complexes whose charge is compensated by protons. One of the water molecules forms an oxonium ion (H3O+) with a proton. The other two water molecules bound to each other through a short hydrogen bond O-H…O (2.403(2) Å) and thus forming (H5O2)+ cations is another proton site. The (H3O)(H5O2)[Co(Pic)2(CN)2]2 crystals are monoclinic: a = 10.7027(7) Å, b = 25.786(1) Å, c = 11.4865(8) Å, β = 91.411(9)°, Z = 4, space group P21/n.  相似文献   

4.
A complex [Zn(C8H7O3)2(H2O)2] (C8H8O3 is vanillin) has been synthesized and characterized by IR, elemental analysis, and X-ray diffraction single-crystal analysis. The crystals are monoclinic, space group C2/c, a = 22.236(8) Å, b = 10.594(2) Å, c = 7.8190(16) Å, α = 89.90(3)°, β = 106.87(4)°, γ = 89.99(3)°, V = 1762.6(8) Å3, Z = 4, F(000) = 832, S = 1.079, ρ c = 1.521g cm?3, R = 0.0221, R w = 0.0604, μ = 1.433 mm?1. The Zn2+ ion is six-coordinated with a distorted octahedron geometry. The complex forms a three-dimensional network through intermolecular hydrogen bonds. The thermal decomposition kinetics of the complex for the second stage was studied under non-isothermal conditions by the TG and DTG methods. The kinetic equation can be expressed as dα/dt = Ae?E/RT 2(1 ? α)[1 ? ln(1 ? α)]1/2. The kinetic parameters (E, A), activation entropy ΔS , and activation free-energy ΔG were also gained.  相似文献   

5.
A new mixed-ligand one-dimensional copper(II) coordination polymer [Cu(en)(sal)Cl] n where en = ethylenediamine(C2H8N2) and Hsal = 2-hydroxybenzoic acid (salicylic acid; C7H6O3) is synthesized and characterized by FTIR spectroscopy and single crystal X-ray diffraction. The structure contains Cu2+ ions in two different distorted octahedral coordination environments: an axially extended CuN4Cl2 moiety arising from a pair of bidentate en ligands and a CuO4Cl2 moiety arising from a pair of asymmetrically coordinated sal anions. The chloride ions bridge the copper ions into a zigzag chain propagating in [001]. The structure is consolidated by N–H???O and N–H???Cl hydrogen bonds which generate a layered network. Crystal data: C9H13ClCuN2O3, M r = 296.20, monoclinic, P21/c, a = 13.9179(10) Å, b = 10.4900(8) Å, c = 8.5181(6) Å, β = 105.518(4)°, V = 1198.30(15) Å3, Z = 4, R(F) = 0.026, w R(F 2) = 0.068.  相似文献   

6.
The atomic structure of ((C2H5)4N)2TeBr6 crystals (a = 17.930(8) Å, b = 11.133(5) Å, c = 15.022(7) Å, β = 109.28(9)°, space group C2/c, Z = 4, ρcalcd = 2.036 g/cm3) has been studied by X-ray diffraction. The ((C2H5)4N)2TeBr6 crystal structure consists of isolated [TeBr6]2? anions and ((C2H5)4N)+ cations. The electronic and geometric aspects that influence the luminescence and thermochromic properties of the complex have been considered.  相似文献   

7.
Two complexes with derivatives of pyridine as ligands were synthesized and characterized. From the reaction of 2-pyridinecarboxaldehyde oxime with Cu(OAc)2 · H2O afforded the complex C20H30N6O12Cu3 (I), and the use of 3-hydroxy-2-pyridinecarboxylic acid with anhydrous MnCl2 · 4H2O led to the formation of another complex C12H14N2OCl2Mn (II). They were characterized by X-ray diffraction (CIF files CCDC nos. 568718 (I) and 1568880 (II)), NMR, IR and elemental analysis. For I: terigonal, space group R\(\bar 3\)/H, a = 42.548(3), c = 10.2774(9) Å, V = 16113(2) Å3, Z = 18, ρcalcd = 1.367 Mg/m3, the final R factor was R1 = 0.0945, 6662 for reflections were observed with I > 2σ(I), wR = 0.162 for all data. For II: triclinic, Pī, a = 5.6174(9), b = 7.7259(13), c = 9.7160(16) Å, α = 70.444(3)°, β = 88.009(3)°, γ = 89.818(3)°, V = 397.09(11) Å3, Z = 1, ρcalcd = 1.840 Mg/m3, the final R factor was R1 = 0.0281, 4280 for reflections were observed with I > 2σ(I), wR = 0.0775 for all data.  相似文献   

8.
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   

9.
The crystal structure of (C2H5)4N)2TeCl6 was determined by X-ray diffraction (a = 14.130(2) Å, b = 14.547(2)Å, c = 13.296(2)Å, β= 90.356(3)°; space group C2/c, Z = 4, ρ(calcd) = 1.387 g/cm3). The crystal structure is composed of the [TeCl6]2? anions and tetraethylammonium cations ((C2H5)4N)+. The electronic and geometric aspects that determine the spectral luminescence and thermochromic properties of the complex are discussed.  相似文献   

10.
A terbium p-methyl benzoate complex with 1,10-phenanthroline, [Tb(p-MBA)3(Phen)]2 (p-MBA = p-methyl benzoate and Phen = 1,10-phenanthroline), has been prepared and structurally characterized by X-ray diffraction. It crystallizes in triclinic system, space group P \(\bar 1\) with a = 12.8064(12), b = 13.3589(12), c = 19.8277(19) Å, α = 91.668(2)°, β = 97.775(2)°, γ = 106.312(2)°, C72H58N4O12Tb2, M r = 1489.06, V = 3217.6(5) Å3, Z = 2, ρ c = 1.537 g/cm3, μ(MoK α) = 2.246 mm?1, F(000) = 1488, the final R = 0.0622 and wR = 0.0962 for 14128 independent reflections with R int = 0.0843. It consists of two types of crystallographically independent dimeric molecules [Tb(p-MBA)3(Phen)]2 noted as [Tb-1] and [Tb-2]. In the dimeric molecule [Tb-1], each Tb(III) is eight-coordinated with one Phen molecule, two bridging carboxylate groups, and two bidentate chelating carboxylate groups, while in [Tb-2] each Tb(III) is eight-coordinated with one Phen molecule, four bridging carboxylate groups, and one bidentate chelating carboxylate group. The title complex shows intense green luminescence under UV light at room temperature.  相似文献   

11.
Complexes of NiII with new ligands N′,N′′-bis(3-carboxy-1-oxoprop-2-enyl), 2-Amino-N-arylbenzamidine (C21H17N3O6), N′,N′′-bis(3-carboxy-1-oxopropanyl) 2-Amino-N-arylbenzamidine (C21H21N3O6) and N′,N′′-bis(3-carboxy-1- oxophenelenyl) 2-Amino-N-arylbenzamidine (C29H21N3O6) have been synthesized and characterized by elemental analyses, vibrational spectra, electronic spectra, TOF-mass spectra, magnetic susceptibility measurements, thermal studies and X-ray powder diffraction studies. Vibrational spectra indicate coordination of amide and carboxylate oxygen of the ligands along with two water molecules giving a MO6 weak field octahedral chromophore. Electronic spectra and magnetic susceptibility measurements reveal octahedral geometry for NiII complexes. The elemental analyses and mass spectral data have justified the ML complexes. Kinetic and thermodynamic parameters were computed from the thermal data using Coats and Redfern method, which confirm first order kinetics. The crystal data: C21H19N3O8 Ni is orthorhombic, space group Pmmm, a = b = 9.015360(Å), c = 10.554430(Å), V = 572.11A3; C21H23N3O8Ni is monoclinic, space group P2/m, a = 15.08206(Å), b = 5.358276(Å), c = 9.898351(Å), V = 671.58A3; C29H23N3O8Ni is tetragonal, space group P4/m, a = b = 6.328104(Å), c = 9.82213(Å), V = 393.33A3. Molecular structures of the complexes have been optimized by MM2 calculations and supported octahedral arrangements around Nickel(II) ions.  相似文献   

12.
A new lanthanum(III) complex of uracil-1-acetate (UA) and 1,10-phenanthroline (Phen), [La(Phen)(UA)3]n · nH2O, was synthesized and characterized by elemental analysis, IR spectroscopy, XRD powder diffraction, thermal analysis, and X-ray crystallography. The single crystal X-ray analysis shows that the compound is in the monoclinic system, space group P21/c with a = 14.645(6), b = 17.114(7), c = 14.141(6) Å, β = 117.206(6)°, V = 3152(2) Å3, Z = 4, final R 1 = 0.0455 and wR 2 = 0.0909. Each La3+ ion is coordinated by two N atoms from Phen, seven carboxylate oxygen atoms, and one carbonyl oxygen atom from UA, which results in ten-coordinate geometry, LaN2O8. The structural studies indicate that the title compound is two-dimensional coordination polymer, and self-assembly of the compound in the solid state is likely to occur due to N-H…O and O-H…O hydrogen bonds.  相似文献   

13.
The interaction of oxythiamine bromide hydrobromide with H2PtCl6 in a hydrochloric acid solution gives the salt of protonated oxythiamine (oxythiamine is the 4-methyl-3-[(2′-methyl-4′-oxo-3′,4′-dihydropyrimidinyl-5′)methyl]-5-(2-hydroxyethyl)thiazolium cation,C12H16N3O2S+) with a platinum(IV) mixed-ligand anion, (C12H17Br2.32Cl3.68N3O2PtS) (I). The crystals of salt I are monoclinic: a = 12.888(3), b = 10.835(2), c =15.898(4) Å, β = 113.03(2)°, Z = 4, space group P21/c. They are built of the [H2OT]2+ cations and [Pt(Cl/Br)6]2? anions joined by hydrogen bonds and electrostatic and π-π stacking interactions. In the cation, the planar thiazolium and pyrimidine rings are bound through the methylene bridge, form a dihedral angle of 90.0°, and exist in the F conformation. The cations are combined into centrosymmetric cyclic dimers flanked on both sides by centrosymmetrically arranged octahedral anions to form short contacts.  相似文献   

14.
Slow evaporation of solutions of Sc and Eu nitrates with macrocyclic cavitand cucurbit[6]uril gives crystals of isostructural complexes [Sc(NO3)(H2O)4(C36H36N24O12)](NO3)2 ? 8.5H2O (space group Pna21, a = 32.0065(18) Å, b = 14.7904(8) Å, c = 11.5774(6) Å, V = 5480.6(5) Å3, Z = 4) and [Eu(NO3)(H2O)4(C36H36N24O12)](NO3)2 ? 6.75H2O (space group Pna21, a = 31.9525(17) Å, b = 14.7203(8) Å, c = 11.8592(6) Å, V = 5578.0(5) Å3, Z = 4). The metal to ligand ratio in these complexes is 1 : 1; the complexes are obtained at 0.025–0.1 mol/l concentrations of the metals in solutions. With higher lanthanide concentrations (0.7–1 mol/l), the 2 : 1 complex with cucurbit[6]uril is formed of the composition [{ Gd(NO3)(H2O)5}2(C36H36N24O12)](NO3)4 ? 6.5H2O (space group \(P\bar 1\), a = 13.3972(6) Å, b = 14.4994(5) Å, c = 18.3290(8) Å, α = 73.5610(10)°, β = 87.2590(10)°, γ = 87.5540(10)°, V = 3409.4(2) Å3, Z = 2) and isotypical complex [{Gd(NO3)(H2O)5}2{(C5H5N) ? (C36H36N24O12)}](NO3)4 ? 8H2O with a pyridine molecule inside the cucurbit[6]uril cavity (space group P21/n, a = 14.8263(6) Å, b = 13.3688(7) Å, c = 18.5970(9) Å, β = 107.5860(10)°, V = 3513.8(3) Å3, Z = 2). According to X-ray diffraction data, the metal atoms of the title complexes coordinate the O atoms in portals of cucurbit[6]uril molecules.  相似文献   

15.
The electron impact mass spectra of 1-R-substituted 3-alkoxy-2-(propargylsulfanyl)- and 3-alkoxy-2-(allenylsulfanyl)-1H-pyrroles (R = Me, i-Pr, s-Bu, Ph) have been studied for the first time. These compounds give rise to stable molecular ions whose primary fragmentation follows three competing pathways: cleavage of the C–O bonds with expulsion of alkyl radical, cleavage of the C–S bonds with formation of [M–C3H3]+ ions, and cleavage of the C–N bonds with synchronous hydrogen transfer to give odd-electron [M–CnH2n]+ · ion. The main fragmentation pathway of 2-(propargylsulfanyl) derivatives is cleavage of the C–S bond with formation of [M–C3H3]+ ion.  相似文献   

16.
Three novel carboxylate complexes were synthesized: dimethylgold(III) trifluoroacetate [Me2Au(Tfa)]2 (I), trimethylacetate (pivalate) [Me2Au(Piv)]2 (II), and benzoate [Me2Au(OBz)]2 (III). The starting reagent was [Me2AuI]2. The procedure of its synthesis provides 60% product yield. Dimethylgold(III) carboxylates were identified from the IR and 1H NMR data. The title compounds were studied by X-ray diffraction. The unit cell parameters for I, C8H12Au2F6O4: a = 15.5522(13), b = 12.9398(11), c = 15.6555(14) Å, β = 104.308(2)°, Z = 8, ρ(calcd.) = 2.959 g/cm3, space group C2/c, R = 0.0779; for II, C14H30Au2O4: a = 10.3025(3), b = 15.5952(4), c = 12.6819(3) Å, β = 105.8270(10)°, Z = 4, ρ(calcd.) = 2.224 g/cm3, space group P21/c, R = 0.0229; for III, C18H22Au2O4: a = 12.8050(2), b = 19.7886(3), c = 7.60300(10) Å, Z = 4, ρ(calcd.) = 2.401 g/cm3, space group Pnma, R = 0.0144. Compounds I–III have the molecular structures; the structural units are the [(CH3)2Au(OOCR)]2 dimers (Au…Au 2.984–3.080 Å), R = CF3, tert-Bu, Ph. The gold atoms have the square coordination with two carbon atoms and two oxygen atoms (Au-O 2.120–2.173 Å). The molecules in compounds I–III are united into infinite unidimensional chains connected by van der Waals interactions.  相似文献   

17.
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   

18.
A new Schiff base ligand C19H13NO5(H2L) was synthesized using 2-aminoterephthalic acid and 2-hydroxy-1-naphthaldehyde. A complex of this ligand [Cu(C19H11NO5)(C2H6O)] n was synthesized and characterized by IR, UV, fluorescence spectroscopy and X-ray diffraction single-crystal analysis. The crystal crystallizes in the monoclinic system, space group Pbca with a = 8.7745(18), b = 18.613(4), c = 24.644(5) Å, V = 4024.9(14) Å3, Z = 8, F(000) = 1816, S = 1.009, ρ calcd = 1.462 g cm?3, μ = 1.122 mm?1, the final R = 0.0477 and wR = 0.1594 for 4609 observed reflections (I > 2σ(I)). The Cu(II) is five-coordinated by one N atom and two O atoms from the Schiff base ligand and two carboxylate O atoms from another two ligands to form a distorted square-pyramidal geometry. Each ligand serves as a bridging ligand to link Cu2+ ions, leading to a two-dimensional coordination polymer. The fluorescence properties of the ligand and complex were also studied. The ligand shows strong fluorescence, and the fluorescence intensity is weakened after the Cu(II) complex formed.  相似文献   

19.
Crystal structures are determined by X-ray crystallography for tetrafluoroantimonates(III) of single and double protonated 3-amino-1,2,4-triazolium cations of the composition (C2H5N4)SbF4 (I) (monoclinic: a = 4.7723(6) Å, b = 19.643(2) Å, c = 7.6974(9) Å, β = 97.239(2)°, Z = 4, Cc space group) and (C2H6N4)(SbF4)2 (II) (monoclinic: a = 4.7617(3) Å, b = 15.512(1) Å c = 7.4365(5)Å β = 107.706(1)°, Z = 2, P21/n space group). The structure of I is built from complex [SbF4]? anions and single charged (C2H5N4)+ cations; the structure of II is built from the same anion and double charged 3-amino-1,2,4-triazolium cation: (C2H6N4)2+. In the structure, weak interactions Sb…F join the anions in polymeric layers [SbF4] n n? that are assembled in a 3D framework by N-H…F hydrogen bonds. The formation of the double protonated 3-amino-1,2,4-triazolium cation (C2H6N4)2+, found in the crystal structure of II, is observed for the first time.  相似文献   

20.
A new coordination polymer, {[Cd(bbmb)(bdc)]} n (bbmb = 1,1′-(1,4-butanediyl)bis-(2-methylbenzimidazole), H2bdc = 1,3-benzenedicarboxylic acid) was synthesized under hydrothermal conditions. The complex was structurally characterized by single crystal X-ray diffraction analyses, infrared spectroscopy (IR), elemental analyses. The compound crystallizes in the monoclinic system, space group P21/c with a = 10.860(6) Å, b = 13.115(7) Å, c = 21.009(9) Å, β = 120.94(2)°, V = 2567(2) Å3, Z = 4, C28H26CdN4O4, M r = 594.93, D c = 1.540 g/cm3, μ = 0.893 mm–1. Each cadmium center is six coordinated with four O atoms from two bdc2– anions, and two N atoms of two bbmb ligands. The complex features a 4-connected 2D (4, 4) sheet with a point symbol {42.62}. Fluorescence properties of the title complex were investigated.  相似文献   

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