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1.
Three new triphosphonate compounds, [Zn(APTPH4)(2,2′-bipy)(H2O)]?·?2H2O (1), [Cd(APTPH4)(2,2′-bipy)(H2O)]?·?2H2O (2), and [Zn(APTPH4)(phen)2]?·?phen?·?4H2O (3) (APTPH6?=?1-aminopropane-1,1,3-triphosphonic acid, 2,2′-bipy?=?2,2′-bipyridine, phen?=?1,10-phenanthroline), are synthesized by a low-temperature hydrothermal method. Compounds 1 and 2 are isomorphous, both one-dimensional (1D) coordination polymers expanded into three-dimensional (3D) supramolecular structures by hydrogen bonds and π–π stacking interactions. Compound 3 is a molecular complex and forms a 3D network through an S-shaped water hexamer. Crystal data for 1: Triclinic, space group P 1, a?=?6.6814(5)?Å, b?=?10.0929(7)?Å, c?=?15.438(2)?Å, α?=?81.544(2)°, β?=?79.066(2)°, γ?=?82.278(2)°, Z?=?2; for 2: Triclinic, space group P 1, a?=?6.9380(8)?Å, b?= 10.043(2)?Å, c?=?15.681(2)?Å, α?=?81.357(2)°, β?=?78.510(2)°, γ?=?81.902(2)°, Z?=?2; Crystal data for 3: Triclinic, space group P 1, a?=?12.540(2)?Å, b?=?12.596(2)?Å, c?=?14.997(2)?Å, α?=?100.795(2)°, β?=?113.328(2)°, γ?=?101.358(2)°, Z?=?2.  相似文献   

2.
The hydrothermal reaction of Co(COO)2?·?4H2O, MoO3, H3PO4 and 4,4′-bipyridine yields bipyridine-ligated cobalt dimolybdate [CoMo2O7(4,4′-bipy)1.5] (1) (4,4′-bipy?=?4,4′-bipyridine) in the triclinic system with space group of P 1 and cell parameters of a?=?7.1951(8)?Å, b?=?11.1708(17)?Å, c?=?11.4514(11)?Å, α?=?98.545(7)°, β?=?90.315(2)°, γ?=?105.777(5)°, V?=?874.88(19)?Å3, and Z?=?2. Its structure consists of Co/Mo/O bimetal oxide layers with {Mo2O7} building blocks, linked by the coordination of 4,4′-bipy ligand with Co and Mo atoms, into a 3D porous hybrid framework.  相似文献   

3.
Two new compounds, [Zn(phen)3]2[γ-As8V14O42(H2O)]?·?4H2O (1) and [Cd(phen)3]2[γ-As8V14O42(H2O)]?·?2H2O (2) (phen?=?1,10′-phenanthroline), have been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, infrared spectrum, and thermogravimetric analysis. Compound 1 crystallizes in the triclinic space group P 1 with a?=?11.429(4)?Å, b?=?15.760(5)?Å, c?=?15.952(5)?Å, α?=?108.825(5)°, β?=?92.194(5)°, γ?=?104.155(5)°, V?=?2615.6(15)?Å3, Z?=?1; 2 crystallizes in the triclinic space group P 1 with a?=?11.450(4)?Å, b?=?15.629(6)?Å, c?=?16.302(6)?Å, α?=?109.177(5)°, β?=?92.628(5)°, γ?=?104.251(4)°, V?=?2644.8(17)?Å3, Z?=?1. Single-crystal structural analysis shows that both 1 and 2 consist of a new type of [γ-As8V14O42(H2O)]4? cluster anion.  相似文献   

4.
This article presents a metal–organic compound [CuII(phen)(sal)]?·?0.5H2O (1) with intriguing structural motif of 3D hexagonal water channels. Furthermore, IR, element analysis, and TGA were employed to characterize it. The TG-DTA showed that this structure is stable to 300°C. Compound 1 belongs to the hexagonal system, space group R-3, a?=?33.337(5)?Å, b?=?33.337(5)?Å, c?=?9.4599(19)?Å, γ?=?120°, V?=?9105(3)?Å3, Z?=?18.  相似文献   

5.
A new Co(II) diphosphonate compound, [Co(HEDPH2)2] (4,4′-bipyH2)?·?H2O (1) has been successfully obtained by a rheological phase reaction at 80°C. Single-crystal diffraction analysis shows a 1-D chain structure and the 1-D chains are assembled via hydrogen bonds into a 3-D supramolecular structure with channels. The protonated 4,4′-bipy molecules are encapsulated in the channels. Magnetic study shows 1 to exhibit antiferromagnetic interaction in the 1D Co--O--P--O--Co chain. Crystal data for 1: monoclinic, space group Cc, a?=?15.754(6)?Å, b?=?14.457(5)?Å, c?=?10.020(4)?Å, β?=?92.024(6)°, V?=?2280.7(14)?Å3, Z?=?4.  相似文献   

6.
A ruthenium(III) complex containing ethylenediaminetetraacetate (edta), [{Ru(Hedta)}2(Pyz)]?·?8H2O (1) (Pyz?=?pyrazine), has been synthesized by the reaction between K[Ru(Hedta)Cl]?·?1.5H2O and pyrazine. The structure of the complex was determined by single X-ray diffraction. Complex 1 crystallizes in the triclinic space group P 1 with a?=?7.293(9)?Å, b?=?10.575(14)?Å, c?=?12.742(16)?Å, α?=?104.044(19)°, β?=?91.893(19)°, γ?=?93.35(2)°, Z?=?1. The product was also characterized by IR, UV-Vis, EPR spectrum and magnetic techniques.  相似文献   

7.
A new inorganic-organic hybrid, [Zn(phen)2(ppy)][{Zn(phen)2}{Zn(phen)2(H2O)}{P2W18O62}]?·?2H2O (phen?=?1,10′-phenanthroline, ppy?=?2-(5-phenylpyridin-2-yl)pyridine) (1), by using pre-prepared Wells–Dawson salt α-K6P2W18O62?·?15H2O as precursor, has been synthesized under hydrothermal conditions. Compound 1 was characterized by single-crystal X-ray diffraction, elemental analyses, IR spectrum and cyclic voltammetry. Yellow crystals crystallized in the monoclinic space group P2 (1)/c with a?=?16.2450(11)?Å, b?=?17.0918(11)?Å, c?=?43.640(3)?Å, β?=?92.0060(10)°, V?=?12109.4(14)?Å3, Z?=?4. The title compound represents a novel zero-dimensional structure based on bisupporting Wells–Dawson POM: one terminal oxygen atom located in the “belt” site and another located in the “cap” site of the same hemisphere of the polyanion are coordinated by Zn2+ cations. Compound 1 also contains the isolated secondary metal complex [Zn(phen)2(ppy)]2+ with two different organic ligands phen and ppy.  相似文献   

8.
Two new arsenic–vanadate compounds [Co(C4H13N3)2]2[As8V14O42(H2O)]?·?3.5H2O (1) and (C2N2H9)2(C2N2H10)[As8V14O42(H2O)]?·?2.33H2O (2) have been hydrothermally synthesized and characterized by X-ray single crystal diffraction, IR spectra and thermogravimetric analysis. Compound 1 crystallizes in the monoclinic space group P 2(1)/c, a?=?24.649(9)?Å, b?=?13.364(5)?Å, c?=?22.463(8)?Å, β?=?104.008(5)°, V?=?7180(5)?Å3, Z?=?4, R 1?=?0.0787, and wR 2?=?0.1859. Compound 2 crystallizes in rhombohedral system with space group R3c, a?=?b?=?c?=?22.2405(5)?Å, α?=?β?=?γ?=?110.4030(10)°, V?=?8163.4(3)?Å3, Z?=?6, R 1?=?0.0341 and wR 2?=?0.0941. The structural analyses show that both compounds have the same discrete cluster anion [As8V14O42(H2O)]4?. Moreover, in 1, the polyanions are connected through van der Waals forces to generate soft channels that are filled by [Co(C4H13N3)2]2+ cations and water. In 2, water and organic molecules link cluster anions to create the supramolecular assembly through hydrogen bonding.  相似文献   

9.
A novel europium(III) coordination polymer, [Eu2(bpdc)3(phen)2(H2O)2] n ·nH2O (1) (bpdc?= biphenyl-2,2′-dicarboxylate; phen?=?1,10-phenanthroline), has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction methods. Complex 1 is monoclinic, space group C2/c, with a?=?24.3862(6), b?=?12.0792(3), c?=?22.9120(5)?Å, α?=?90.00, β?=?115.160(1), γ?=?90.00°, V?=?6108.8(3)?Å3, Z?=?4, final R 1?=?0.0605 and wR 2?=?0.1760. Each Eu(III) ion is coordinated by six oxygen atoms from three carboxylate groups of three different bpdc anions, an oxygen atom from one coordinated water molecule and two nitrogen atoms from one phen ligand to complete a deformed monocapped square antiprism. Each pair of bpdc anions acts as a tetradentate ligand to connect two adjacent Eu(III) ions through chelating carboxylate groups, resulting in a centrosymmetric binuclear unit. Each binuclear unit links two adjacent binuclear units through two terminal bpdc anions to produce a one-directional zigzag chain. Two different kinds of hydrogen-bonding interactions link the chains and the lattice water molecules to form a hydrogen-bonding network.  相似文献   

10.
Three new coordination polymers, {[Cu(trza)(2,2′-bipy)(H2O)]?·?(ClO4)} n (1), {[Cu(trza)(2,2′-bipy)(H2O)]?·?(BF4)} n (2), and {[Cu(trza)(4,4′-bipy)]?·?(H2O)?·?(ClO4)} n (3) (Htrza?=?2-(1H-1,2,4-triazole)-1-acetic acid), have been synthesized and characterized by single-crystal X-ray diffraction analysis. Both 1 and 2 exhibit 1-D chain structure while 3 displays 2-D layer structure. The catalytic activities of 1 and 3 in the green oxidative coupling of 2,6-dimethylphenol have been investigated.  相似文献   

11.
A new organic–inorganic polyoxometalate compound [Co(2,2′-bipy)3]H[Al(OH)6 (Mo6O18)]?·?17H2O has been synthesized and characterized by elemental analysis, IR, UV spectra, thermogravimetry and differential thermal analysis (TG-DTA) and single-crystal X-ray diffraction analysis. The title compound crystallizes in a monoclinic, C2/c space group, with a?=?37.292(8), b?=?14.214(3), c?=?25.050(5)?Å, β?=?120.62(3), V?=?11426(4)?Å3, Z?=?8, F(000)?=?7200, D c?=?2.116?Mg?m?3, R?=?0.0748, wR 2?=?0.1853. Crystal structural analysis indicates that the asymmetric unit in the crystal structure of the title compound consists of one B-Anderson–Evans type heteropolyoxoanion, one octahedral [Co(2,2′-bipy)3]2+ coordination cation, seventeen water molecules of crystallization and a proton based on charge balance. The curves of TG-DTA indicate that weight loss of the title compound is divided into three stages. The third weight loss reveals that the backbone of heteropolyoxoanion decomposes at 744°C.  相似文献   

12.
The synthesis and X-ray characterization of two supramolecular isomers, [Co(oba)(2,2′-bpy)] n (1 and 2) (oba?=?4,4′-oxybis(benzoate), 2,2′-bpy?=?2,2′-bipyridine) are reported. Crystal data for 1: a?=?12.026(2), b?=?15.120(3), c?=?11.361(2)?Å, β?=?91.46(3)°, Z?=?4, R 1?=?0.0330, wR 2?=?0.0949. Crystal data for 2: a?=?16.171(3), b?=?19.162(4), c?=?22.914(5)?Å, α?=?107.66(3), β?=?91.46(3), γ?=?98.99(3)°, Z?=?2, R 1?=?0.0388, wR 2?=?0.0456. They are conformational supramolecular isomers without solvent molecules in the structures, and exhibit different one-dimensional helical structures that are further assembled into distinct two-dimensional layers via π–π stacking interactions. The results indicate that the geometry of ligand is one of the most important factors for the construction of a helical motif.  相似文献   

13.
A Cu(II) complex with mixed ligands, [Cu3(mal)3(phen)3(H2O)2]?·?11H2O (mal?=?malonate, phen?=?1,10-phenanthroline) was synthesized and characterized by elemental analysis, IR, UV, electron paramagnetic resonance (EPR) and luminescence spectra and single-crystal X-ray diffraction. The complex crystallizes in the monoclinic system, space group Cc with a?=?13.1631(10)?Å, b?=?20.1089(10)?Å, c?=?20.1267(13)?Å, β?=?103.500(3)°, V?=?5180.2(6)?Å3, Z?=?4, and R 1?=?0.0476 for 7993 observed reflections. In the complex, one Cu is coordinated by a mal dianion and a phen molecule, exhibiting N2O2 square-planar geometry, while the other two Cu atoms are coordinated, respectively, by a mal dianion, a phen and water molecules, exhibiting N2O3 square pyramidal coordination geometry.  相似文献   

14.
Four new anthraquinone-1,5-disulfonate (L)-based metal complexes with N,N-bidentate chelating coligands, {[Pb(phen)2(L)]?·?4H2O} n (1), {[Mn2(2,2′-bipy)2(H2O)6(L)]?·?L?·?6H2O} (2), [Co(phen)2(H2O)(L)] (3), and [Zn(phen)2(H2O)(L)] (4) (phen = 1,10-phenanthroline and 2,2′-bipy?=?2,2′-bipyridine), have been hydrothermally synthesized and were structurally characterized by single-crystal X-ray diffraction, elemental analyses, FT-IR spectra, thermogravimetric curves, and solid luminescence spectra. Structural analysis suggests that 1 is a polymeric 1D zigzag chain bridged by dianionic L. In contrast, the other three complexes have discrete centrosymmetric binuclear structure for 2 and isolated isomorphic mononuclear entities for 3 and 4, which are further assembled into 3D supramolecular networks by abundant hydrogen-bonding and/or π–π stacking interactions. Additionally, 2 and 4 exhibit favorable luminescent emissions, suggesting they are potential candidates for light emission materials.  相似文献   

15.
The hydrothermal reaction of 1,3-dicyanobenzene, 1,10-phenanthroline (phen) and Pb(CH3COO)2 yields a new 1D coordination polymer, {Pb[C6H4(COO)2][phen]} n . The 1,3-benzenecarboxylate anion found in the final product was generated in situ during the synthesis by hydrolysis of 1,3-dicyanobenzene. X-ray diffraction shows that complex 1 crystallizes in the triclinic system, space group P 1, a?=?7.5442(2)?Å, b?=?9.7962(3)?Å, c?=?13.1505(4)?Å, α?=?69.739(2)?Å, β?=?80.597(2)?Å, γ?=?71.377(2)?Å, v?=?862.48(4)?Å3, Z?=?2, D c?=?2.124 Mg?m?3. Complex 1 emits strong blue fluorescent light (λem(max)?=?482.4?nm) when excited by UV light in the solid state at room temperature.  相似文献   

16.
(NH4)[EuIII(pdta)(H2O)]?·?H2O has been synthesized and characterized by infrared spectrum, fluorescence spectrum, elemental analyses and single-crystal X-ray diffraction techniques. It crystallizes in the monoclinic system with space group P21/n, a?=?12.7700(15)?Å, b?=?9.3885(11)?Å, c?=?14.4070(18)?Å, α?=?90°, β?=?95.950(2)°, γ?=?90°, V?=?1718.0(4)?Å3, Z?=?4, M?=?508.28, D c?=?1.965?g?cm?3, μ?=?3.708?mm?1, F(000)?=?1108. The structure was refined to R 1?=?0.0238 for 3469 observed reflections (I?>?2σ(I)). The EuIIIN2O6 part in the [EuIII(pdta)(H2O)]? complex anion has an eight-coordinate structure with a distorted square anti-prismatic conformation, in which six coordination positions, two nitrogen atoms and four oxygen atoms are from one pdta (=propylenediaminetetraacetic acid) ligand, the seventh position is an oxygen (O(8A)) from another pdta and the eighth coordination site is occupied by a water molecule. (NH4)[EuIII(pdta)(H2O)]?·?H2O is the first eight-coordinate complex with a six-member ring in the rare earth metal complexes with aminopolycarboxylic acid ligands.  相似文献   

17.
Three complexes, Na4[DyIII(dtpa)(H2O)]2?·?16H2O, Na[DyIII(edta)(H2O)3]?·?3.25H2O and Na3[DyIII (nta)2(H2O)]?·?5.5H2O, have been synthesized in aqueous solution and characterized by FT–IR, elemental analyses, TG–DTA and single-crystal X-ray diffraction. Na4[DyIII(dtpa)(H2O)]2?·?16H2O crystallizes in the monoclinic system with P21/n space group, a?=?18.158(10)?Å, b?=?14.968(9)?Å, c?=?20.769(12)?Å, β?=?108.552(9)°, V?=?5351(5)?Å3, Z?=?4, M?=?1517.87?g?mol?1, D c?=?1.879?g?cm?3, μ?=?2.914?mm?1, F(000)?=?3032, and its structure is refined to R 1(F)?=?0.0500 for 9384 observed reflections [I?>?2σ(I)]. Na[DyIII(edta)(H2O)3]?·?3.25H2O crystallizes in the orthorhombic system with Fdd2 space group, a?=?19.338(7)?Å, b?=?35.378(13)?Å, c?=?12.137(5)?Å, β?=?90°, V?=?8303(5)?Å3, Z?=?16, M?=?586.31?g?mol?1, D c?=?1.876?g?cm?3, μ?=?3.690?mm?1, F(000)?=?4632, and its structure is refined to R 1(F)?=?0.0307 for 4027 observed reflections [I?>?2σ(I)]. Na3[DyIII(nta)2(H2O)]?·?5.5H2O crystallizes in the orthorhombic system with Pccn space group, a?=?15.964(12)?Å, b?=?19.665(15)?Å, c?=?14.552(11)?Å, β?=?90°, V?=?4568(6)?Å3, Z?=?8, M?=?724.81?g?mol?1, D c?=?2.102?g?cm?3, μ?=?3.422?mm?1, F(000)?=?2848, and its structure is refined to R 1(F)?=?0.0449 for 4033 observed reflections [I?>?2?σ(I)]. The coordination polyhedra are tricapped trigonal prism for Na4[DyIII(dtpa)(H2O)]2?·?16H2O and Na3[DyIII(nta)2(H2O)]?·?5.5H2O, but monocapped square antiprism for Na[DyIII(edta)(H2O)3]?·?3.25H2O. The crystal structures of these three complexes are completely different from one another. The three-dimensional geometries of three polymers are 3-D layer-shaped structure for Na4[DyIII(dtpa)(H2O)]2?·?16H2O, 1-D zigzag type structure for Na[DyIII(edta)(H2O)3]?·?3.25H2O and a 2-D parallelogram for Na3[DyIII(nta)2(H2O)]?·?5.5H2O. According to thermal analyses, the collapsing temperatures are 356°C for Na4[DyIII(dtpa)(H2O)]2?·?16H2O, 371°C for Na[DyIII(edta)(H2O)3]?·?3.25H2O and 387°C for Na3[DyIII(nta)2(H2O)]?·?5.5H2O, which indicates that their crystal structures are very stable.  相似文献   

18.
A new dipicolinate complex of Ru(II), cis-[Ru(phen)2dipic]?·?9.5H2O (1), where dipic is dipicolinate or pyridine-2,6-dicarboxylate and phen is 1,10-phenanthroline, has been synthesized and characterized by elemental analysis, spectroscopic (IR, UV-Vis), cyclic voltammetry, and single-crystal X-ray diffraction. ORTEP drawing of cis-[Ru(phen)2dipic]?·?9.5H2O shows that the coordination geometry around Ru(II) is a distorted octahedron. It crystallizes in the triclinic system, with space group P 1, a?=?10.4633(2)?Å, b?=?13.6332(4)?Å, c?=?13.6637(4)?Å, α?=?67.516(3)°, β?=?69.757(2)°, γ?=?77.201(2)°, V?=?1680.74(8)?Å3, Z?=?2, and R int?=?0.0311. In 1, two phen are bidentate N,N′ ligands. The Ru(II) in 1 is bonded to dipicolinate through pyridine nitrogen and one oxygen of carboxylate groups, thus pyridine-2,6-dicarboxylate is a bidentate N,O ligand. Efficient and selective oxidation of alcohols with NaIO4 as oxidant was conducted by this complex catalyst in CH3OH/H2O as solvents under air at room temperature.  相似文献   

19.
{[Pb(tsgluo)]?·?H2O} n (1), [Pb2(tsgluo)2(phen)2] (2), and [Pb2(tsgluo)2(bipy)2] (3) (H2tsgluo?=?N-p-tolylsulfonyl-L-glutamate, phen?=?1,10-phenanthroline, bipy?=?2,2′-pyridine) have been synthesized in the absence or presence of phen or 2,2′-bipy and structurally characterized by elemental analysis, IR, and X-ray crystallography. Single-crystal X-ray analyses reveal that tsgluo exhibits two coordination modes to link lead ions. Complex 1 gives a 2-D layer structure while 2 and 3 exhibit monomolecular structures; 3 is further connected into a double-chain structure by hydrogen bonds. Phen and 2,2′-bipy are very important for the crystal structure. Fluorescence of the compounds is also discussed.  相似文献   

20.
A 1?:?1 chelate complex [(C6H5)3PC(COCH3)(COC6H5)-κO,O′]UO2(NO3)2 has been synthesized by reaction of (C6H5)3PC(COCH3)(COC6H5) with UO2(NO3)2?·?6H2O in methanol at room temperature and characterized by elemental analysis, spectroscopy as well as by single-crystal X-ray diffraction. The complex crystallizes in P21/n space group with a?=?10.007(2)?Å, b?=?15.285(7)?Å, c?=?19.20(1)?Å, β?=?91.22(3)°, V?=?2936(2)?Å3, Z?=?4, D c?=?1.847?g?cm?3. In the solid state structure, the dihedral angle [88.1(4)°] between the planes defined by the two quartets of atoms O1 O8 O2 O4 and O6 O5 O3 O7 is close to 90°, as expected for a triangulated dodecahedral geometry around uranium.  相似文献   

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