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1.
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   

2.
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   

3.
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   

4.
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   

5.
A new Anderson polyoxometalate (H3O)[(3-C5H7N2)2(Cr(OH)6Mo6O18)]?·?3H2O (3-C5H6N2?=?3-aminopyridine) was hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. Crystal data: triclinic, P 1, a?=?7.8482(8)?Å, b?=?10.1800(10)?Å, c?=?10.4103(10)?Å, α?=?88.031(3)°, β?=?78.308(2)°, γ?=?88.842(3)°, V?=?813.91?Å3, Z?=?1, R(F)?=?0.0397, wR ref(F 2)?=?0.1022, and S?=?1.076. The X-ray crystallographic study showed that the structure contains Anderson-type [Cr(OH)6Mo6O18]3? polyoxoanions. The title compound has high catalytic activity for the oxidation of acetone tested in a continuous-flow fixed-bed micro-reactor. When the initial concentration is 18.3?g?m?3 in air and the flow velocity is 8.5?mL?min?1, the acetone is completely eliminated at 160°C.  相似文献   

6.
A new coordination polymer, [Ni(pydc)(H2O)2]?·?H2O (1) (H2pydc?=?pyridine-3,4-dicarboxylic acid), have been synthesized by treating Ni(II) nitrate with 3,4-pyridinedicarboxylic acid under hydrothermal conditions. The single-crystal X-ray structure reveals that 1 is a 2D bi-layered coordination polymer. Single-crystals are triclinic, space group P 1 , with a?=?7.065(3), b?=?7.812(4), c?=?9.031(4)?Å, α?=?75.568(8), β?=?68.970(8), γ?=?75.927(8)°, V?=?444.0(3)?Å3, Z?=?2. Variable temperature magnetic susceptibility measurements demonstrate a ferromagnetic interaction in 1.  相似文献   

7.
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   

8.
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   

9.
The syntheses and crystal structures of the closely related but non-isostructural Cd2(C19H21N3O3F)4(H2O)2?·?4H2O (1) and Pb2(C19H21N3O3F)4?·?4H2O (2) are described, where C19H21N3O3F? is enrofloxacinate (enro). Both compounds contain centrosymmetric, binuclear, neutral complexes incorporating a central diamond-shaped M2O2 (M?=?Cd, Pb) structural unit. The Cd2+ coordination polyhedron in 1 is a CdO6 trigonal prism, including one coordinated water. The Pb2+ coordination polyhedron in 2 can be described as a very distorted square-based PbO5 pyramid, although two additional short Pb?···?O (<3.1?Å) contacts are also present. In the crystal of the cadmium complex, O–H?···?O hydrogen bonds lead to a layered structure. In the lead compound, O–H?···?O and O–H?···?N interactions lead to chains in the crystal. Crystal data: 1: C76H96Cd2F4N12O18, M r?=?1766.45, triclinic, P 1, a?=?12.185(2)?Å, b?=?12.306(3)?Å, c?=?14.826(3)?Å, α?=?68.15(3)°, β?=?70.28(3)°, γ?=?86.11(3)°, V?=?1938.2(7)?Å3, Z?=?1, T?=?298 K, R(F)?=?0.030, wR(F 2)?=?0.079. 2: C76H88F4N12O16Pb2, M r?=?1920.00, triclinic, P 1, a?=?12.0283(4)?Å, b?=?12.7465(4)?Å, c?=?13.0585(4)?Å, α?=?83.751(1)°, β?=?74.635(1)°, γ?=?81.502(1)°, V?=?1904.3(1)?Å3, Z?=?1, T?=?298?K, R(F)?=?0.021, wR(F 2)?=?0.049.  相似文献   

10.
A lanthanide coordination complex [Eu(PAA)2(phen)(NO3)]2 (PAA?=?phenylacetic acid, phen?=?1,10-phenanthroline) has been synthesized by the hydrothermal method. Single crystal X-ray diffractions show that it forms a dimeric molecular structure. The title complex crystallizes in the triclinic system, space group P 1, with lattice parameters a?=?8.9473(8)?Å, b?=?13.3659(12)?Å, c?=?13.4745(12)?Å, α?=?60.7590(10)°, β?=?89.5100(10)°, γ?=?71.9850(10)°, V?=?1317.3(2)?Å3, D c?= 1.675?Mg?m?3, Z?=?1, F(000)?=?660, GOF?=?1.003, R 1?=?0.0206, wR 2?=?0.0575. The fluorescence excitation and emission spectra have been investigated.  相似文献   

11.
The hydrothermal reactions of Nd(ClO4)3·6H2O, Gd(ClO4)3·6H2O, Dy(ClO4)3·6H2O, Er(ClO4)3·6H2O with 1,3-dicyanobenzene, give rise to four one-dimensional rare earth-based coordination polymers: [M(3-CNC6H4COO)3(H2O)2] n (where M?=?Nd (1), Gd (2), Dy (3), Er (4), 3-CNC6H4COO?=?3-cyanobenzoato), respectively. Their solid-state structures have been characterized by X-ray single-crystal diffraction studies. The results show that 1,3-dicyanobenzene hydrolyzed to give 3-cyanobenzoato under hydrothermal condition, and the four complexes are isomorphous. Crystal data for 1: triclinic, space group P-1, a?=?9.4063(19), b?=?11.485(2), c?=?12.616(3)?Å, α?=?66.38(3), β?=?74.01(3), γ?=?86.96(3)°, V?=?1197.9(4)?Å3, Z?=?1, D c?=?1.704?Mg?m?3; for 2: triclinic, space group P-1, a?=?9.3712(19), b?=?11.446(2), c?=?12.627(3)?Å, α?=?65.86(3), β?=?73.89(3), γ?=?86.84(3)°, V?=?1184.8(4)?Å3, Z?=?1, D c?=?1.759?Mg?m?3; for 3: triclinic, space group P-1, a?=?9.3425(19), b?=?11.432(2), c?=?12.703(3)?Å, α?=?65.28(3), β?=?73.80(3), γ?=?86.86(3)°, V?=?1180.6(4)?Å3, Z?=?1, D c?=?1.780?Mg?m?3; for 4: triclinic, space group P-1, a?=?9.3425(19), b?=?11.432(2), c?=?12.703(3)?Å, α?=?65.28(3), β?=?73.80(3), γ?=?86.86(3)°, V?=?1180.6(4)?Å3, Z?=?1, D c?=?1.7794?Mg?m?3. The fluorescence emission spectra of compounds 1 to 4 are also reported.  相似文献   

12.
Two organic–inorganic compounds based on Keggin building blocks have been synthesized by hydrothermal methods, (C7N2H7)3(C7N2H6)?·?PMo12O40?·?2H2O (1) and (C7N2H7)3(C7N2H6)2?·?AsMo12O40?·?3H2O (2) (C7N2H6?=?benzimidazole). Single-crystal X-ray analysis revealed that 1 crystallized in the triclinic system, P-1 space group with a?=?9.8980(4)?Å, b?=?11.2893(4)?Å, c?=?25.8933(9)?Å, α?=?93.307(2)°, β?=?90.630(2)°, γ?=?108.330(2)°, V?=?2740.68(18)?Å3, Z?=?2, R 1(F)?=?0.0740, ωR 2(F 2)?=?0.1511, and S?=?1.037; 2 crystallized in the triclinic system, P-1 space group with a?=?12.3353(4)?Å, b?=?13.2649(4)?Å, c?=?20.2878(6)?Å, α?=?95.6630(10)°, β?=?100.1720(10)°, γ?=?99.3940(10)°, V?=?3195.72(17)?Å3, Z?=?2, R 1(F)?= 0.0329, ωR2 (F 2)?=?0.1236, and S?=?1.088. The two compounds show a layer framework constructed from Keggin-polyoxoanion clusters and benzimidazole via hydrogen bonds and π–π stacking interactions, resulting in a 3-D supramolecular network. Both have high catalytic activity for oxidation of methanol. When the initial concentration of the methanol is 5.37?g?m?3 in air and the flow velocity is 4.51?mL?min?1, methanol is completely eliminated at 150°C for 1 (160°C for 2).  相似文献   

13.
A new 1-D chain-like organic–inorganic hybrid phosphotungstate based on tetra-Ni-sandwiched polyoxoanion, [Ni(en)2]2[{Ni3(en)6(H2O)2Ni4(H2O)2(α-PW9O34)2}]?·?7H2O (en?=?ethylenediamine) (1), has been synthesized under hydrothermal conditions and characterized by IR spectrum, UV spectrum, elemental analysis, thermogravimetric analysis, and single-crystal X-ray diffraction. 1 crystallizes in the triclinic P 1 space group with cell parameters a?=?13.232(4)?Å, b?=?15.591(5)?Å, c?=?15.701(5)?Å, α?=?112.804(5)°, β?=?92.159(5)°, γ?=?109.012(5)°, Z?=?1, R 1?=?0.0588, wR 2?=?0.1387. Compound 1 displays a 1-D chain-like architecture constructed by sandwich-type polyoxoanions and [Ni(en)2]2+ linkers. Magnetic measurement reveals that intramolecular ferromagnetic interactions exist in the tetranuclear {Ni4O16} cluster.  相似文献   

14.
Two cobalt complexes [NaCoII(nta)(H2O)] n (H3nta?=?nitrilotriacetic acid) (1) and NH4[CoIII(ida)2]?·?2H2O (H2ida?=?iminodiacetic acid) (2) have been synthesized and characterized by single-crystal X-ray diffraction analysis. Compound 1 crystallizes in the orthorhombic system, space group P212121 with a?=?7.9770(12)?Å, b?=?9.7613(15)?Å, c?=?12.1945(18)?Å, V?=?949.5(2)?Å3, Z?=?4, and R 1?=?0.0705 for 1597 observed reflections. Compound 2 crystallizes in the monoclinic system, space group P2(1)/c with a?=?5.1801(3)?Å, b?=?11.2073(6)?Å, c?=?12.2891(7)?Å, V?=?707.09(7)?Å3, Z?=?2, and R 1?=?0.0349 for 1143 observed reflections. In compound 1, the Co is coordinated by a nitrogen and five oxygen atoms in a distorted octahedral geometry {CoNO5}, and the Na is coordinated by one water molecule and four carboxyl oxygen atoms in slightly distorted square pyramidal geometry. The entire structure shows a three-dimensional network. In compound 2, Co atom is equatorially coordinated by two ida ligands in a distorted octahedral geometry {CoN2O4}. The discrete [Co(ida)2]2? anions are linked by hydrogen bonding to a three-dimensional supramolecular network.  相似文献   

15.
A novel isopolyoxomolybdate complex (C10H18N)4Mo8O26·6(CH3)2SO 1 was synthesized, purified and characterized by means of elemental analysis, IR and 1H NMR spectra and single-crystal X-ray diffraction. It crystallizes in a triclinic system with a?=?11.5090(6), b?=?12.8399(3), c?=?14.774(13)?Å, α?=?105.390(16), β?=?93.09(4), γ?=?106.100(10)°, V?=?2003.1(2)?Å3, Z?=?2, R1?=?0.0789, wR2?=?0.2190. Complex 1 is constructed from [Mo8O26]4?, (C10H18N)+ and (CH3)2SO and extends to form a two-dimensional network via hydrogen bonds and weak interactions in the ab plane. Chicken embryo experiments show that Compound 1 has high antiviral activity in vitro.  相似文献   

16.
The chiral dinuclear heterometallic complexes [Cu(dach)2][Pt(CN)4]?·?2H2O (1), [Ni(dach)3][Pt(CN)4]?·?2DMF?·?H2O (2), and [Pd(dach)4][Pt(CN)4]?·?H2O (3) (dach?=?1R,2R-cyclohexanediamine) have been prepared and characterized by X-ray diffraction analysis. Crystal data: 1, monoclinic, P21, a?=?8.108(3), b?=?15.552(6), c?=?9.914(4)?Å, β?=?110.931(6)°, V?=?1167.6(8)?Å3, Z?=?2, R 1?=?0.0420, wR 2?=?0.1122; 2, monoclinic, P21, a?=?13.264(11), b?=?9.285(7), c?=?16.211(13)?Å, β?=?111.640(9)°, V?=?1856(3)?Å3, Z?=?2, R 1?=?0.0276, wR 2?=?0.0698; 3, monoclinic, P21, a?=?6.887(2), b?=?12.809(4), c?=?12.975(4)?Å, β?=?94.865(4)°, V?=?1140.6(6)?Å3, Z?=?2, R 1?=?0.057, wR 2?=?0.156. In complex 1, the Pt and Cu atoms are linked by a CN bridge that presents a very bent C=N–Cu angle [136.8(8)°].  相似文献   

17.
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   

18.
Two copper(II) triphosphonate compounds, Cu[(APTPH4)(phen)(H2O)]?·?2.16H2O (1) and [Cu(APTPH4)(2,2′-bipy)(H2O)]?·?2.63H2O (2), have been prepared by a low temperature hydrothermal reaction from 1-aminopropane-1,1,3-triphosphonic acid (APTPH6), CuO and a second ligand, phen?=?1,10-phenanthroline, or 2,2′-bipy?=?2,2′-bipyridyl. These two compounds were characterized by single crystal X-ray diffraction, elemental analysis, IR and TG. Crystal data for 1: Monoclinic, space group P21 /c, a?=?14.4830(7)?Å, b?=?9.1721(5)?Å, c?=?16.7403(8)?Å, β?=?90.101(2)°. For compound 2: Triclinic, space group P 1, a?=?7.1215(7)?Å, b?=?10.460(2)?Å, c?=?14.671(2)?Å, α?=?82.983(2)°, β?=?83.882(2)°, γ?=?80.617(2)°. In both compounds, each Cu2+ ion is five-coordinate with two oxygen atoms from the triphosphonate, two nitrogen atoms from the second ligand and one water molecule, to form a distorted square-pyramidal geometry. Both complexes have 3D supramolecular structures constructed by hydrogen bonds and π–π stacking interactions.  相似文献   

19.
Two zinc complexes of enoxacin were synthesized and their crystal structures were determined. Compound 1, [Zn(H-Eno) · Cl2] · 3H2O (H-Eno = Enoxacin), crystallizes in the triclinic system, space group P 1, with lattice parameters a = 8.7731(12), b = 9.4976(14), and c = 13.2033(19) Å, α = 86.319(7)°, β = 71.912(7)°, and γ = 80.604(7)°, V = 1031.6(3) Å3, Z = 2, D Calcd = 1.631 Mg m?3; compound 2, [Zn(H-Eno) · (H2O)2] · 2NO3, also crystallizes in the triclinic system, space group P 1, with lattice parameters a = 8.751(2), b = 9.014(2), and c = 12.594(3) Å, α = 92.277(14)°, β = 109.867(12)°, and γ = 111.469(12)°, V = 854.1(3) Å3, Z = 1, D Calcd = 1.684 Mg m?3.  相似文献   

20.
A cyanide-containing cobalt(III) complex, [Co(phen)2(CN)2][Co(phen)(CN)4]?·?4.5H2O (1: phen?=?1,10-phenanthroline) has been synthesized by hydrothermal techniques and characterized by elemental analyses, IR spectroscopy, UV–vis spectroscopy and single-crystal X-ray diffraction methods. The complex is triclinic, space group P 1 , with a?=?11.0047(16), b?=?12.9587(19), c?=?15.076(2)?Å, α?=?100.060(2), β?=?102.061(2), γ?=?91.803(2)°, V?=?2065.0(5)?Å3, Z?=?2, and R 1 [I?>?2σ(I)]?=?0.0481. The molecular unit of 1 consists of a cation/anion pair with interstitial water molecules in the crystal lattice. The combination of coordinative, hydrogen bonding and π–π stacking interactions results in the stabilization of a supramolecular solid-state architecture.  相似文献   

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