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1.
Abstract Single crystals of new open-framework lanthanide sulphate nitrite La(NO2)(SO4)(H2O) has been synthesized, in the presence of 2,6-diformyl-4-chlorophenol. His structure has been determined by X-ray diffraction data: the complex crystallizes in the tetragonal system, space group P43, with a = 7.0028(2) (?), b = 7.0028(2) (?), c = 11.8341(4) ?, V = 580.34(3) ?3, Z = 4, D c = 3.582 Mg m−3. The three-dimensional (3D) framework of this compound is built up by the linkages of lanthanide atoms and the oxygen atoms of the sulphate and nitrite groups. The lanthanum atom is 9-fold coordinated. The structure is unfamiliar in lanthanide chemistry and this compound represents the first example of nitrite lanthanide sulphate complex. Graphical Abstract An unfamiliar structure in lanthanide chemistry represented by the first example of nitrite lanthanide sulphate complex is described.   相似文献   

2.
Abstract The tridentate Schiff base carboxylate-containing ligand 2-pyridylmethylamino-3-butyric acid (Hpaba) reacts with copper(II) perchlorate to give the one-dimensional chain complex {[Cu(μ-paba)](ClO4)·H2O} n (1). The coordination geometry of each copper(II) ion is best described as a square-plane with two nitrogen atoms and one carboxylate oxygen atom of the ligand, and one carboxylate oxygen atom belong to another ligand. It crystallizes in the monoclinic system P21/c with a = 12.717(2), b = 7.9163(15), c = 14.981(2) ?, β = 111.14(1)°, V = 1406.8(4) ?3, Z = 4. Cyclic voltammogram of 1 undergoes the reversible one-electron oxidation to the Cu(III) and the reversible one-electron reduction to the Cu(I) state. Graphical Abstract Crystal structure of 1 reveals a syn-anti carboxylate-bridged one dimensional chain complex in which the coordination environment around each copper(II) ion exhibits a distorted square plane.   相似文献   

3.
Abstract A new complex [Co(H2pztc)(bpy)H2O] (H4pztc = pyrazine-2,3,5,6-tetracarboxylic acid, bpy = 2,2′-bipyridine) has been synthesized by hydrothermal reactions of Co(NO3)2 · 6H2O with H4pztc and bpy and characterized by IR and X-ray diffraction single crystal structure analysis. It belongs to monoclinic system, P21/c space group with a = 13.454(2) ?, b = 12.939(2) ?, c = 11.4993(19) ?, α = 90°, β = 111.640(3)°, γ = 90°. This complex is assembled into 3D supramolecular architecture by hydrogen bonds (O–H···O, C–H···O). Index Abstract A new complex of cobalt(II) with pyrazine-2,3,5,6-tetracarboxylic acid and 2,2′-bipyridine is assembled by intermolecular hydrogen bonds forming 2D layer and 3D supramolecular network.   相似文献   

4.
Abstract  The title compound, aquabis(5-methylisoazole-3-carboxylato-O,N)copper(II) monohydrate, [Cu(L2)(H2O)] · H2O is synthesized and characterized by X-ray diffraction, elementary analysis, and IR. The ligand coordinates to the copper center in a bidentate O,N fashion through the carboxylic acid moiety and the heteroaromatic nitrogen atom. The complex crystallizes in the triclinic space group with unit cell parameters a = 8.4080(12)?, b = 8.810(3), c = 10.318(2)?, α = 110.08(3)°, β = 104.81(2)°, γ = 103.149(16)°, V = 650.9(3)?3, Z = 2. In addition, the synthesis of the free acid 5-methylisoazole-3-carboxylic acid and pyridine containing complex bis(5-methylisoazole-3-carboxylato)bispyridinecopper(II) monohydrate is described. Index Abstract  Synthesis and crystal structure of aquabis(5-methylisoazole-3-carboxylato-O,N)copper(II)monohydrate. The first coordination compound of 5-methylisoxazole-3-carboxylic acid.   相似文献   

5.
Abstract  [Na(H2O)2(C18H15O6SO3)]2 was synthesized by sulfated 5-hydroxy-6,7,4′-trimethoxyisoflavone with concentrated sulfuric acid. Single-crystal X-ray diffraction study indicates that it is a dimeric centrosymmetric species. The coordination polyhedron of each Na(I) atom exhibits a distorted trigonal bipyramidal geometry. The dimeric units are linked by intermolecular hydrogen bonds C–H⋯π, C–H⋯O and O–H⋯O to result in a three-dimensional framework. Graphical Abstract  [Na(H2O)2(C18H15O6SO3)]2 was synthesized by sulfated 5-hydroxy-6,7,4′-trimethoxyisoflavone with concentrated sulfuric acid. The coordination polyhedron of each Na(I) atom exhibits a distorted trigonal bipyramidal geometry. The dimeric centrosymmetric units are linked by intermolecular hydrogen bonds C–H⋯π, C–H⋯O and O–H⋯O to result in a three-dimensional framework. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.  相似文献   

6.
Abstract These complexes have been characterized by X-ray crystallography, spectroscopic, and cyclic voltammetry. In 1, the copper(II) ion has a distorted square-pyramidal geometry with three nitrogen atoms of the dpa ligand and two oxygen atoms of the nitrate anions. The crystal structure of 2 shows that the copper(II) ions are bridged by tp anion to form a dinuclear complex, in which each copper(II) ion exhibits a distorted square-pyramid with three nitrogen atoms of the dpa ligand, water molecule, and the oxygen atom of the bridging tp ligand. Cyclic voltammetric data indicate that 1 undergoes irreversible one-electron oxidation to the CuIII and reversible one-electron reduction to the CuI, while 2 gives one reversible oxidation and two reversible and irreversible reduced processes. The electronic spectra and redox potentials of the complexes are influenced significantly by the anionic ligands. Graphical Abstract The reaction of [Cu(dpa)Cl2] with K(NO3)2 and Na2tp yields mononuclear and dinuclear copper(II) complexes [Cu(dpa)(NO3)2] (1) and [Cu2(dpa)2(H2O)2(μ-tp)](tp)·6H2O (2) (dpa = di-(2-picolyl)amine, tp = terephthalate).   相似文献   

7.
Abstract  The copper(II) complex [Cu(C5H4NCH2−N=CH–C6H3OCH3–O)Cl], (1) containing a new tridentate Schiff base ligand (LH), which is the 1:1 condensation product of 2-(aminomethyl)pyridine and o-vaniline, has been synthesised and characterized by IR and UV–Vis spectra. Structural investigation shows that 1 crystallizes to a monoclinic system, having space group P2(1)/c, a = 6.9634(7), b = 18.1209(19), c = 10.3448(11) ?, α = 90°, β = 103.97(2)°, γ = 90° and Z = 4. The coordination geometry around the copper atom is slightly distorted square planar, formed by the N2O donor set of the Schiff base and one Cl atom. The Cu–N(1), Cu–N(2), Cu–O(1) and Cu–Cl bond distances are 2.0114(14), 1.9414(14), 1.9147(12) and 2.2520(5) ?, respectively. Index Abstract  The copper(II) complex [Cu(C5H4NCH2−N=CH–C6H3OCH3–O)Cl], (1) containing a tridentate Schiff base ligand (LH), synthesised and characterized by IR and UV–Vis spectra. The central copper ion possesses a distorted square-planar geometry.   相似文献   

8.
Abstract 3-[(Naphthalen-2-yl) methyl]isocoumarin was synthesized by the reaction of homophthalic acid with 2-(naphthalen-2-yl)acetyl chloride at elevated temperature and its crystal structure has been determined (C20H14O2), Mr = 286.31, a = 13.704(3), b = 7.356(4), c = 7.042(7) ?, β = 99.21(3)°, space group Pc, Z = 2, and V = 700.7(8) ?3. The isocoumarin and the naphthalene ring systems are individually planar and the dihedral angle between the mean planes of these two ring systems is 70.05(8)°. Graphical Abstract Synthesis and crystal structure of 3-[(Naphthalen-2-yl)methyl]isocoumarin Aamer Saeed, Junmei Liang, Masood Parvez The synthesis and crystal structure of a novel isocoumarin, 3-[(naphthalen-2-yl)methyl]isocoumarin has been presented.   相似文献   

9.
Abstract The coordination chemistry of the ligand N-thiazol-2-yl-toluenesulfonamidate towards the copper(II) ion has been investigated using an electrochemical synthesis method. The X-ray structure of this complex was elucidated and is discussed. The compound crystallised in the monoclinic crystal system, P21/c space group with a = 17.3888(9), b = 16.3003(9), c = 18.3679(9) ? and β = 114.3640(10)°. Four bidentate sulfathiazolato anions bridge two metal centers in a paddle-wheel fashion, with the nitrogen atoms as donors to give a dimeric species with a Cu···Cu distance of 2.7859(5) ?. Graphical Abstract The coordination chemistry of the ligand N-thiazol-2-yl-toluenesulfonamidate towards the copper(II) ion has been investigated using an electrochemical synthesis method. The X-ray structure of the product has been elucidated and is discussed. Sulfathiazolato anions act as bridging ligands to give a dimeric species with a Cu···Cu distance of 2.7859(5) ?.   相似文献   

10.
Abstract  Two structures containing pseudo-tetrahedral Cu(II)N2Cl2 coordination complexes are reported. The first molecular structure (A) of the compound, 1,1′bis(1-ethylbenzimidazol-2-yl)propane copper(II) dichloride (triEtBBIM)Cu(II)Cl2, 1, is reported. The complex crystallized in the triclinic space group P-1 with a = 8.616(3) ?, b = 9.302(3) ?, c = 14.314(4) ?, α = 85.613(6)°, β = 85.170(6)°, γ = 66.117(6)° and V = 1044.1(5) ?3 with Z = 2. The second structure (B) contains 1 and (3,3′bis(1-ethylbenzimidazol-2-yl)pentane) copper(II) dichloride (tetEtBBIM)Cu(II)Cl2, 2, both of which, cocrystallize in an equal molar ratio with a nitromethane solvate molecule. The complex crystallized in the monoclinic space group P21/c with a = 18.876(4) ?, b = 14.975(3) ?, c = 18.344(4) ?, β = 116.75(3)°, and V = 4630.3(16) ?3 with Z = 4. The cocrystallization of such discrete complexes has been coined a chemical Janus. Graphical Abstract  The title complexes contain pseudo-tetrahedral Cu(II)N2Cl2 coordination. One of the structures is the result of an unusual cocrystallization, in which two different discrete Cu(II) molecules cocrystallize in an equimolar ratio with a nitromethane solvate molecule.   相似文献   

11.
Abstract The title compound trans-UO2(N(SiMe3)2)2(THF)2 (1) was synthesized and characterized by X-ray crystallography. The complex crystallizes in the monoclinic space group C2/c (#15) with lattice parameters a = 16.0771(5) ?, b = 13.1196(4) ?, c = 16.9391(6) ?, β = 116.853(1)°, V = 3187.61(18) ?3, Z = 4, D calc = 1.532 g cm-3. The six-coordinate uranium(VI) center adopts an all-trans octahedral geometry consisting of mutually trans oxo groups, silylamido ligands, and neutral THF donors. Structural comparisons of this uranyl(VI) bis(amido) complex with a related tris(amido) derivative within the series are made based on symmetry, charge, and coordination number. Graphical Abstract The X-ray crystal structure of the title complex is reported, providing comparisons based on symmetry, charge, and coordination number with a related uranyl(VI) amido derivative within this series.   相似文献   

12.

Treatment of [Fe2(CO)6(μ-S2C3H6)] (1) with triphenylstibine in a 1:1 molar ratio at room temperature in presence of Me3NO resulted compound [Fe2(CO)5(SbPh3)(μ-S2C3H6)] (2) in 88% yield as red crystals. When the reaction was carried out under a 1:5 molar ratio in presence of Me3NO, it resulted a monosubstituted compound [Fe2(CO)5(SbPh3)(μ-S2C3H6)] (2) in 63% yield along with a disubstituted compound [Fe2(CO)4(SbPh3)2(μ-S2C3H6)] (3) in low yield (8%) as red crystals. Reaction of 2 with triphenylstibine in a 1:5 molar ratio under same condition resulted 3 in moderate yield (46%). Compounds 2 and 3 were characterized by elemental analyses, IR, 1H NMR and 13C NMR spectroscopic data. Crystal structures of the compounds were unambiguously determined by single crystal X-Ray diffraction studies. Compound 2 crystalized as monoclinic crystal system with the space group P21/c, a?=?9.464(4) Å, b?=?16.902(7) Å, c?=?17.081(7) Å, β?=?101.216(13)° and Z?=?4. Compound 3 was triclinic, space group P-1, a?=?9.552(3) Å, b?=?13.985(5) Å, c?=?16.487(6) Å, α?=?78.372(16)°, β?=?89.976(14)°, γ?=?71.638(11)° and Z?=?2.

Graphic Abstract

Two new diiron propane-1,3-dithiolate complexes, [Fe2(CO)5(SbPh3)(μ-S2C3H6)] (2) and [Fe2(CO)4(SbPh3)2(μ-S2C3H6)] (3), were synthesized by the displacement of carbonyl groups from [Fe2(CO)6(μ-S2C3H6)] (1) with triphenylstibine, and the resulting complexes were structurally characterized.

Solid state molecular structure of compound 2 (left) and compound 3 (right)

  相似文献   

13.
Abstract The title compound, 3, 6-dihydroxy-2-[2-(4-hydroxy-phenyl)-vinyl]- benzene-1,3-dicarbaldehyde was synthesized by Vilslmeier reaction from resveratrol (trans-3,4′,5-trihydroxystilbene). Its structure was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic, space group P21/n with crystallographic parameters: a = 7.2950(15) ?, b = 14.781(3) ?, c = 12.202(2) ?, β = 96.57(3)°, μ = 0.108 mm−1, V = 1307.1(5) ?, Z = 4, Dx = 1.445 g/cm3, F(000) = 592, T = 293(2) K, 2.17°≤ θ ≤ 26.00°. The X-ray results demonstrated that the Vilslmeier reaction of resveratrol with DMF, POCl3 and CH3CN yielded 4,6-dhydroxy-2-[2-(4-hydroxy-phenyl)-vinyl]-benzene-1,3-dicarbaldehyde. Graphical Abstract In this article, a resveratrol derivative was prepared and structurally characterized by single crystal X-ray diffraction.   相似文献   

14.
Abstract The three complexes (pnH2)[Co(pydc)2]·4H2O 1, (pnH2)[Cu(pydc)2]·4H2O 2, and (pnH2)[Cd(pydc)2]·3.5H2O 3 (pn: propane-1,3-diamine, pydc: pyridine-2,6-dicarboxylate) were prepared using a proton transfer compound (pnH2)(pydc)·(pydcH2)·2.5H2O, LH 2 and corresponding metallic salts. The characterization was carried out using elemental analysis, IR and NMR spectroscopy, and single crystal X-ray diffraction. Complexes 1 and 2 crystallize in space group P , but complex 3 crystallizes in space group P2/c. Cell parameters of the complexes are a = 8.449(1) ?, b = 11.668(1) ?, c = 12.801(1) ?, α = 115.748(2)°, β = 93.038(2)°, γ = 97.867(2)° for 1; a = 7.973(2) ?, b = 16.632(2) ?, c = 25.280(5) ?, α = 94.178(6)°, β = 95.186(6)°, γ = 91.603(5)° for 2 and a = 20.055(1) ?, b = 13.8161(9) ?, c = 8.2418(5) ?, β = 100.086(1)° for 3. The three crystal structures illustrate that the metal ion is six-coordinated by two pydc’s. In structures of 2 and 3, it can be seen that propane-1,3-diaminium fragments have different conformations. The complexes have ion-pairing interactions, O–H···O, N–H···O and C–H···O hydrogen bonds, π–π stacking as well as van der Waals forces as the main factors in formation of their supramolecular structures. Index Abstract Supramolecular Cobalt(II), Copper(II) and Cadmium(II) Complexes Obtained from a Proton Transfer Compound including Pyridine-2,6-dicarboxylate and Propane-1,3-diaminium Ions; Synthesis, Characterization and Crystal Structure Hossein Aghabozorg, Mohammad Ghadermazi,Bahar Nakhjavan, Faranak Manteghi The synthesis, characterization, crystal structure and non-covalent interactions of three supramolecular complexes of Co(II), Cu(II) and Cd(II) obtained by the reaction of a proton transfer compound i.e. (pnH2)(pydc)·(pydcH2)·2.5H2O with the corresponding metallic salts are reported. Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.  相似文献   

15.
Abstract  The zinc(II) complex with 2-(2-hydroxyphenyl)benzimidazole, namely [Zn(2-(2-hydroxyphenyl)benzimidazolate)2]·C2H5OH (· C2H5OH) has been synthesized and characterized by X-ray crystallography and photoluminescent analysis. The complex crystallizes in monoclinic space group P21/c with cell parameters a = 10.156(1) ?, b = 25.771(3) ?, c = 9.674(1) ?, α = 90°, β = 103.641(2)°, γ = 90°, Z = 4, V = 2460.4(4) ?3. The central Zn(II) is four-coordinate and has a tetrahedral geometry. The steady-state and time-resolved photoluminescent spectra for the title compound have also been studied. The emission property can be ascribed to ligand-centered charge-transfer transition (LCCT) with π → π* property. Index Abstract   A new co-crystal of Zn(II) complex of 2-(2-hydroxylphenyl)benzimidazole with ethanol solvate has been prepared, characterized by X-ray crystallography and fluorescent studies.   相似文献   

16.
Abstract  Reactions of CuF2, CuCl2 · 2H2O and CuBr2 with 2,2′-dipyridylamine (HDPA) in water at room temperature using Cu:HDPA = 2:1 mol yield [Cu(HDPA)(H2O)2F]F · 3H2O (1), Cu(HDPA)Cl2 (2) and Cu(HDPA)Br2 (3) respectively. The structures of 2 and 3 are isostructural in spacegroup C2 with cell dimensions; for 2, a = 14.702(8), b = 7.726(2), c = 4.829(6) ?, β = 96.68(8)° and for 3, a = 14.2934(8), b = 7.9057(6), c = 5.1982(5) ?, β = 94.049(7)°. In the X-ray crystal structure, the complex 1 is found to contain tapes of water pentamers. Our DFT calculations at the B3LYP/LanL2DZ level show that the reaction Cu(HDPA)X2 + 2H2O = [Cu(HDPA)(H2O)2X]X is most exothermic in the gas phase when X = F, i.e., the tendency of water uptake is maximum for Cu(HDPA)F2. It seems that the exothermicities of the aquations of Cu(HDPA)Cl2 and Cu(HDPA)Br2 are not sufficient to stabilise the type of ribbons of water observed in 1 and consequently water is eschewed when X = Cl or Br. Graphical Abstract  Cu(2,2′-dipyridylamine)X2 takes up water to produce ribbons of water pentamer, as shown in the accompanied picture (red: O atom of a solvent water molecule), only when X is F but not when it Cl or Br. The results are rationalised by means of DFT calculations at the B3LYP/LanL2DZ level. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.  相似文献   

17.
Abstract The crystal structures of methyl 4-{(E)-2-(4-methylpiperazino)-1-diazenyl}benzoate (2a) and 1,4-di[(E)-2-(2-nitrophenyl)-1-diazenyl]piperazine (3a) have been determined by single crystal X-ray diffraction analysis. The bis-triazene (3a) adopts an unusual pseudo-boat conformation in the piperazine ring, with a dihedral angle of 52.20(0.06)° between the two planes defined within the piperazine ring. The crystal structures of 2a and 3a are compared with the structure of the triazene (4) and the closely related bis-triazene (5). The piperazine ring of 2a adopts a typical chair conformation, whereas the piperazine ring of 3a adopts an unusual boat conformation. Crystal data: 2a C13H18N4O2, monoclinic, space group P21 /n, a = 13.849(3) ?, b = 6.577(1) ?, c = 14.904(3) ?, α = 90°, β = 96.098(3)°, γ = 90° and V = 1,349.8(4) ?3, for Z = 4. 3a C16H16N8O4, triclinic, space group P-1, a = 7.6066(6) ?, b = 8.3741(7) ?, c = 14.507(1) ?, α = 78.673(1)°, β = 81.877(1)°, γ = 73.445(1)° and V = 865.0(1) ?3, for Z = 2. Index abstract The crystal structures of methyl 4-{(E)-2-(4-methylpiperazino)-1-diazenyl}benzoate (2a) and 1,4-di[(E)-2-(2-nitrophenyl)-1-diazenyl]piperazine (3a) have been determined by single crystal X-ray diffraction analysis.  相似文献   

18.
Abstract  A new complex [Cu(NCS)4 (N-Eim)4] [Cu(NCS)2 (N-Eim)2] (where N-Eim = N-ethylimidazole) has been synthesized and structurally characterized by single-crystal X-ray diffraction. The compound crystallizes in the Triclinic space group P−1 with the parameters: a = 8.7707(18) ?, b = 10.712(2) ?, c = 13.511(3) ?, α = 104.73(3)°, β = 104.84(3)°, γ = 102.52(3)°, V = 1131.54(3) ?3, with Z = 1 formula units. In the structure, the copper atoms all assume an elongated octahedral geometry with two distinct coordination environments; one is coordinated by four N-ethyl-imidazole ligands and two axial SCN groups, and another by two SCN groups and two N-ethyl-imidazole ligands. The two units form one infinite 1D zigzag chain along the [1 0 1] plane by two thiocyanate ligands from the [Cu(NCS)4 (N-Eim)4] units. Index Abstract  The title compound, tetrakis(1-ethyl-1H-imidazole)diisothio cyanatocopper(II) bis(1-ethyl-1H-imidazole)diisothiocyanatocopper(II) has been synthesized and structurally characterized by single-crystal X-ray diffraction. In the structure, the copper atoms all assume an elongated octahedral geometry with two distinct coordination environments. The two units form one infinite 1D zigzag chain along the [1 0 1] plane by two thiocyanate ligands from the [Cu(NCS)4 (N-Eim) 4] units.   相似文献   

19.
Index Abstract  In the dinuclear compound (HPhen)2[Sm2(Hsal)8(H2O)2] · 2H2O (Hsal = o-HOC6H4CO2 , Phen = 1,10-phenanthroline), intermolecular hydrogen bonds and π–π stacking interactions between parallel aromatic rings result in the formation of a two-dimensional supramolecular network.   相似文献   

20.
Abstract  The title compound, C16H22O4, synthesized by modified Knoevenagel condensation of protocatechualdehyde with monoheptyl-malonate and recrystallized from benzene, was confirmed by single-crystal X-ray diffraction (CCDC 272827). The compound crystallizes in triclinic space group Pī with cell parameters a = 5.296(3) ?, b = 10.711(13) ?, c = 13.870(4) ?, α = 98.84(7)°, β = 90.97(4)°, γ = 96.77(7)° and Z = 2. The structure is the E isomer and its packing is stabilized by intermolecular O–H···O and C–H···O hydrogen bonds. Index Abstract  The title compound, C16H22O4, synthesized by modified Knoevenagel condensation, was confirmed by single-crystal X-ray diffraction showing its structure is in E isomer and its packing is stabilized by hydrogen bonds.   相似文献   

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