首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到20条相似文献,搜索用时 940 毫秒
1.
Two malonato-bridged hexamethylenetetramine coordination polymers, M2(hmt)(H2O)2(mal)2 [hmt?=?hexamethylenetetramine, mal?=?malonate(2-), M?=?Mn (1), Cu (2)] were prepared and structurally characterized. The isostructural complexes are orthorhombic, space group Imm2, with a?=?7.104(1), b?=?15.982(3), c?=?7.702(1)?Å, Z?=?2, D calc?=?1.862?g?cm?3(1) and a?=?6.962(3), b?=?15.500(7), c?=?7.627(3)?Å, Z?=?2, D calc?=?2.047?g?cm?3for 2. The transition metals are octahedrally coordinated by one nitrogen atom of an hmt ligand and five oxygen atoms of a water molecule and three malonate anions. The latter coordinate in chelating/bis-monodentate mode to give 2D layers with a (4,?4) topology, and which are pillared by bridging bidentate hmt ligands to generate an open 3D framework with channels extending in the [001] direction. Over the temperature range 5–300?K, 2 behaves paramagnetically, following the Curie–Weiss law χm(T???θ)?=?4.521(6)?cm3mol?1K with a Weiss constant θ?=??4.8(2)?K.  相似文献   

2.
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   

3.
4.
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   

5.
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   

6.
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   

7.
Two complexes [CuL2(H2O)2] (1) and [ZnL2(H2O)2] (2) (L?=?3-carboxyl-1,2,4-triazole (L)) have been synthesized and characterized by single-crystal X-ray diffraction analysis. Compound 1 crystallizes in the monoclinic space group P 2(1)/n, a?=?8.632(8)?Å, b?=?9.153(8)?Å, c?=?6.991(7)?Å, β?=?94.279(12)°, Z?=?2, R 1?=?0.0296, wR 2?=?0.0918. Compound 2 also crystallizes in the monoclinic space group P 2(1)/n, a?=?4.937(3)?Å, b?=?18.107(10)?Å, c?=?6.344(4)?Å, β?=?106.839(7)°, Z?=?2, R 1?=?0.0230, wR 2?=?0.0556. Extensive intermolecular hydrogen bonds assemble 1 and 2 into three-dimensional (3D) supramolecular architectures, with eight-member H-bonded synthons. Compounds 1 and 2 were also characterized by element analysis, FT–IR, luminescence and EPR studies.  相似文献   

8.
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   

9.
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   

10.
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   

11.
A manganese(II) coordination polymer [Mn(TMB)2?·?H2O] n (1) (HTMB?=?3,4,5-trimethoxybenzoic acid) has been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction, elemental analysis, powder X-ray diffraction analysis, spectroscopic (IR, solid state UV-Vis), and thermal methods. The crystal belongs to orthorhombic system, space group P212121, with cell parameters a?=?7.3001(8), b?=?11.4146(13), c?=?27.053(3)?Å, α?=?β?=?γ?=?90°, V?=?2254.3(4)?Å3, Z?=?4. In 1, TMB in two different coordination modes bridges six-coordinate manganese(II) centers forming a 1-D infinite chain coordination framework. The spectral and thermal properties of the complexes have also been studied.  相似文献   

12.
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   

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.
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   

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.
This article reports the hydrothermal synthesis and characterization of two new phosphonate compounds NaCo[O3PCH(OH)CO2] (1) and NaMn[O3PCH(OH)CO2] (2) based on 2-hydroxyphosphonoacetic acid (H3L). Their structures have been characterized by single-crystal X-ray diffraction as well as with elemental analysis, infrared spectroscopy and thermogravimetric analysis. The two isomorphous compounds crystalline in the orthorhombic, space group Pbca: Crystal data for 1: a?=?10.1827(8)?Å, b?=?9.6673(8)?Å, c?=?10.7853(9)?Å, V?=?1061.70(15)?Å3, Z?=?8, R 1?=?0.0252, wR 2?=?0.0577; Crystal data for 2: a?=?10.4309(18)?Å, b?=?9.7913(17)?Å, c?=?10.9012(19)?Å, V?=?1113.4(3)?Å3, Z?=?8, R 1?=?0.0194, wR 2?=?0.0536. In the two compounds, the metal atoms are octahedrally coordinated; all oxygen atoms from the H3L ligand are involved in coordination. The overall structures can be described as a 3D open framework with channels running along the a axis and the charge-compensating Na+ cations being located at the intersections of these channels.  相似文献   

17.
A new dinuclear manganese complex, [Mn2L2(N3)2], was prepared by reaction of bis-Schiff base N,N'-bis(5-fluoro-2-hydroxybenzylidene)ethane-1,2-diamine (H2L) with manganese acetate and sodium azide in methanol. Both the Schiff base and the complex were characterized by physico-chemical methods and single crystal X-ray determination. The Schiff base crystallized in the orthorhombic space group Pbca with unit cell dimensions a?=?7.3191(7)?Å, b?=?6.0948(6)?Å, c?=?35.382(3)?Å, V?=?1578.3(3)?Å3, Z?=?4, R1?=?0.0481, wR2?=?0.1488. The manganese complex crystallized in the monoclinic space group P21/c with unit cell dimensions a?=?8.802(1)?Å, b?=?14.928(2)?Å, c?=?14.478(2)?Å, β?=?105.517(2)°, V?=?1833.0(4)?Å3, Z?=?2, R1?=?0.0768, wR2?=?0.1640. There are crystallographic inversion centers in both the ligand and the complex. The ligand coordinates to Mn through all the phenolate oxygens and imino nitrogens. The two Mn in the complex are bridged by two phenolate oxygens with separation of 3.549(1)?Å. Each Mn is octahedral with four donors of the Schiff base ligand defining the equatorial plane, and with one azido nitrogen and one phenolate oxygen of an adjacent Schiff base ligand occupying the axial positions. The Schiff base and the complex were tested in vitro for their antibacterial activities.  相似文献   

18.
Polymeric dioxomolybdenum(VI) complexes, [MoO2L]n (L?=?L1?=?N′-(2-hydroxybenzylidene)nicotinohydrazide for 1, L?=?L2?=?N′-(2-hydroxy-5-methoxybenzylidene)isonicotinohydrazide for 2), were prepared and characterized by physico-chemical, spectroscopic methods, and single-crystal X-ray determination. Complex 1 crystallizes in the orthorhombic space group P212121 with a?=?7.6568(4), b?=?11.6315(7), c?=?15.2211(9)?Å, V?=?1355.59(13)?Å3, Z?=?4, R 1?=?0.0181, wR 2?=?0.0464, and S?=?1.097. Complex 2 crystallizes in the monoclinic space group P2 1 /n with a?=?11.2516(6), b?=?11.8134(7), c?=?12.4371(6)?Å, β?=?116.2210(10)°, V?=?1483.02(14)?Å3, Z?=?4, R 1?=?0.0399, wR 2?=?0.0874, and S?=?1.096. X-ray analysis indicates that Mo in each complex is octahedral with two oxo groups and N2O2 donor set of the nicotinohydrazone or isonicotinohydrazone. The complexes are efficient catalysts for oxidation of olefins.  相似文献   

19.
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   

20.
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   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号