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1.
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   

2.
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   

3.
A novel cadmium complex Cd(IPA)2(phen)2 (IPAH?=?isophthanic acid, phen?=?1,10-phenanthroline) was synthesized by hydrothermal methods and characterized structurally by X-ray diffraction. The complex possesses a monomeric molecular structure. Cd(IPA)2(phen)2 is orthorhombic, space group Aba2, with a?=?14.670(7), b?=?22.876(8), c?=?9.473(6)?Å, V?=?3179(3)?Å3, D c?=?1.573?Mg?m?3, Z?=?4, F(000)?=?1520, GOF?=?1.027, R1?=?0.0299, wR2?=?0.0617. Photophysical properties (fluorescence excitation and emission spectra) are reported.  相似文献   

4.
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   

5.
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   

6.
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   

7.
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   

8.
Two new binuclear complexes, [Mn2(μ-dmpo)2(SCN)4(H2O)2] (1) (where dmpo?=?3,5-dimethylpyridine N-oxide), [Mn2(μ-po)2(H2O)6I2]I2 (2) (where po?=?pyridine N-oxide), have been synthesized and their crystal structures determined by X-ray crystallography. Complexes 1 and 2 crystallize in monoclinic, space group P21/c, with unit cell dimensions a?=?8.8836(18)?Å, b?=?15.450(3)?Å, c?=?15.484(3)?Å, β?=?91.020(3)° for 1, and a?=?8.8352(13)?Å, b?=?17.927(3)?Å, c?=?8.3338(12)?Å, β?=?103.765(2)° for 2. In each binuclear complex two Mn(II) were bridged by two 3,5-dimethylpyridine N-oxides or by two pyridine N-oxides and the distances between the bridged Mn(II) ions are 3.599?Å for 1 and 3.552?Å for 2. Variable temperature (4–300?K) magnetic measurements were performed for 1 and the susceptibility data were fitted by using a binuclear Mn(II) magnetic coupling formula producing the 2J?=??2.17?cm?1.  相似文献   

9.
Two metal complexes, [NiII(mscinn)2(pda)2] (1) and [CdII(mscinn)2(dmeda)2·2H2O] (2) (mscinn?=?4-methylsulfonyl cinnamate, pda?=?propane-1,3-diamine, dmeda?=?N′,N′-dimethylethane-1,2-diamine), were synthesized by reacting 4-methylsulfonyl cinnamate with the diamines and metal salts. Their structures were determined by single-crystal X-ray diffraction analysis. Crystal parameters of 1: C26H38N4NiO8S2, M?=?657.43, monoclinic, P21/c, a?=?16.6123(8)?Å, b?=?8.5956(4)?Å, c?=?11.2047(5)?Å, β?=?107.423(1)°, V?=?1526.54(12)?Å3, Z?=?2, D calcd?=?1.430?g?cm?3, F(000)?=?692, μ?=?0.825?mm?1, R 1?=?0.0257, wR 2?=?0.0669. Crystal data of 2: C28H42CdN4O8S2?·?2(H2O), M?=?775.24, monoclinic, P21/c, a?=?9.8278(4)?Å, b?=?11.6611(5)?Å, c?=?15.3972(7)?Å, β?=?96.195(1)°, V?=?1754.26(13)?Å3, Z?=?2, D calcd?=?1.468?g?cm?3, F(000)?=?804, μ?=?0.798?mm?1, R 1?=?0.0299, wR 2?=?0.0770. Antimicrobial activities for 1 and 2 against Escherichia coli, Pseudomonas putida, Bacillus subtilis, and Bacillus cereus had better antibacterial activity than their parent carboxylic acid against Gram-positive bacteria (B. subtilis and B. cereus). The cadmium complex of the cinnamate displayed high inhibitory activity with an MIC value of 5?µg?mL?1 against P. putida, while the nickel complex also exhibited good inhibitory potency with an MIC value of 5?µg?mL?1 against B. subtilis.  相似文献   

10.
11.
A linear-chain one-dimension polymeric complex of Co(II), [[Co(TMA)2(4,4′-bipyridine)2]?·?H2O] n has been synthesized and characterized. The complex crystallizes in the monoclinic system, space group P2(1)/c with a?=?11.344(3)?Å, b?=?15.880(4)?Å, c?=?23.436(5)?Å, β?=?117.831(10)°, V?=?3733.5(16)?Å3 and D c?=?1.437?g?cm?3. The effective magnetic moment for this complex indicates that there is almost no ferromagnetic coupling between the Co(II) ions and the magnetic behavior is due to the isolated Co(II).  相似文献   

12.
Two dysprosium coordination compounds, (mnH)2[DyIII(Httha)]·3H2O (1) (H6ttha?=?triethylenetetramine-N,N,N′,N″,N′′′,N′′′-hexaacetic acid and mn?=?methylamine) and (enH2)3[DyIII(ttha)]2·9H2O (2) (en?=?ethylenediamine), were synthesized through direct heating and characterized by elemental analysis, FT-IR, thermal analysis, and single-crystal X-ray diffraction. X-ray diffraction analysis displays that 1 is a mononuclear nine-coordinate complex with a pseudo-monocapped square antiprismatic conformation (MCSAP) crystallizing in the monoclinic crystal system with P2(1)/c space group. The crystal data are as follows: a?=?16.1363(19)?Å, b?=?13.9336(11)?Å, c?=?13.6619(14)?Å, β?=?102.2490(10)°, and V?=?3001.8(5)?Å3. There are two kinds of methylamine cation in 1. They connect [DyIII(Httha)]2?and crystal waters through hydrogen bonds, leading to formation of a 2-D ladder-like layer structure. The polymeric 2 also is a nine-coordinate structure with a pseudo-MCSAP crystallizing in the monoclinic crystal system with P2/c space group. The cell dimensions are: a?=?17.7801(16)?Å, b?=?9.7035(10)?Å, c?=?22.096(2)?Å, β?=?118.874(2)°, and V?=?3338.3(6)?Å3. In 2 there are also two types of ethylenediamine cations. One connects three adjacent [DyIII(ttha)]3? complex anions through hydrogen bonds and the other is symmetrical forming hydrogen bonds with two neighboring [DyIII(ttha)]3? complex anions. These hydrogen bonds result in formation of a 2-D ladder-like layer structure as well.  相似文献   

13.
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   

14.
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   

15.
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   

16.
A novel supramolecular complex, [Na2(2,3-naphtho-15-crown-5)2(NO3)][Cu(NO3)3(H2O)] (1), has been prepared and characterized by X-ray single crystal diffraction. The complex crystallizes in the triclinic system, space group Pī, with a?=?11.233(6), b?=?13.342(7), c?=?16.601(8)?Å, α?=?89.836(7), β?=?79.132(8), γ?=?66.545(7)°, V?=?2234(2)?Å3, Z?=?2 and final R 1(wR 2)?=?0.0467(0.1164). Novel coordination features and supramolecular architectures are found in the solid state of 1. Two [Na(2,3-naphtho-15-crown-5)]+ cations containing two different sodium coordination numbers (six and seven) are bridged by a tridentate nitrate group, to form a larger complex cation, [Na2(2,3-naphtho-15-crown-5)2(NO3)], which is assembled into a novel 1D zigzag chain-like structure through aromatic C–H?···?π interactions.  相似文献   

17.
A novel one-dimensional chain coordination polymer [[CuCl2]2(phen)2] (1) and a three-dimensional coordination polymer [[CuCl] (phen)2](CuCl2) (2) were synthesized from simple hydrothermal reactions and the structures were characterized with elemental analysis, FT-IR spectrum and X-ray diffraction. Compound 1 crystallized in the monoclinic space group Cc with a?=?9.874(2), b?=?17.871(4), and c?=?13.440(3)?Å, α?=?90.00°, β?=?106.59(3)°, γ?=?90.00°, R 1?=?0.0463, wR 2?=?0.0819. Compound 2 crystallized in the monoclinic space group P2/c with a?=?14.4084(13), b?=?12.6280(11) and c?=?13.3560(12)?Å, α?=?90.00°, β?=?111.490(2)°, γ?=?90.00°, R 1?=?0.0771, wR 2?=?0.1439. In the packing structure, π–π stacking interactions are the most significant factors controlling the novel supramolecular sheets for the title compound. Moreover, the third-order non-linear optical property of the two compounds were also investigated and they show reverse saturable absorption and self-focusing performance.  相似文献   

18.
The title compound Cd8(OH)8(SO4)4 (1) obtained under hydrothermal conditions by reacting Cd(OH)2 with 4-aminobenzenesulfonic acid in an aqueous ethanol solution was confirmed by single-crystal X-ray diffraction. Crystal data: P21/c with a?=?6.8984(4), b?=?7.5640(4), c?=?11.3919(5)?Å, β?=?119.763(2)°, V?=?516.01(5)?Å3, H8Cd8O24S4, M r ?=?1419.50, Z?=?1, D c ?=?4.568?Mg?m?3, μ?=?8.595?mm?1, F(000)?=?648, R?=?0.023, wR?=?0.060 for 1208 observed reflections [I?>?2σ(I?)]. The crystal structure of complex 1 forms a three-dimensional (3-D) framework.  相似文献   

19.
Two Cd(II) coordination polymers have been synthesized with derivatives of pyrazine-1,4-dioxide and thiocyanate anion as bridging ligands and structurally determined by X-ray crystallography. Complex 1, [Cd(μ1,3-SCN?)21,6-L1)] n (L1?=?2,5-dimethylpyrazine-1,4-dioxide), belongs to the triclinic, space group P 1 with a?=?5.7627(18)?Å, b?=?7.182(2)?Å, c?=?7.509(2)?Å, α?=?74.042(3)°, β?=?84.766(4)°, γ?=?88.162(4)°; complex 2, [Cd21,3-SCN?)44-L2)] n (L2?=?2,3,5,6-tetramethylpyrazine-1,4-dioxide), crystallizes in a monoclinic system with space group C2/m with a?=?10.194(4)?Å, b?=?13.491(6)?Å, c?=?8.140(3)?Å, β?=?120.372(4)°. Complex 1 shows a two-dimensional sheet structure, and in a direction the Cd(II) ions were coordinated by μ1,3-SCN? forming the one-dimensional chain and the L1 bridging ligand made the chains connect in the c direction leading to formation of a two-dimensional sheet on the ac plane. For 2 the one-dimensional chains in the a axis were constructed by coordination of μ1,3-SCN? bridging ligands with the Cd(II) ions, and in b and c directions the chains were joined by L2 bridging ligands leading to a three-dimensional structure. In 2 L2 displays a μ4-bridging coordination mode. Both complexes exhibit strong fluorescence emission.  相似文献   

20.
An organic-inorganic hybrid polyoxometalate [Ni(phen)(H2O)3]2[Ni(H2O)5][H2W12O40]?·?6H2O (phen?=?1,10-phenanthroline) has been isolated and characterized by IR, UV, electrochemistry and single-crystal X-ray diffraction. X-ray crystallographic study indicates that the title compound is monoclinic, space group C2/c, with lattice constants a?=?21.7672(17), b?=?16.1189(12), c?=?20.7949(16)?Å, β?=?107.8440(10)°, V?=?6945.2(9)?Å3, D c?=?3.528?Mg?m?3, F(000)?=?6600, Z?=?4, R 1?=?0.0372, wR 2?=?0.0845. The molecular fragment of the title compound consists of two supporting [Ni(phen)(H2O)3]2+ coordination cations, one supporting [Ni(H2O)5]2+ unit, one metatungstate polyoxoanion [H2W12O40]6? and six H2O molecules of crystallization.  相似文献   

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