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1.
The title compound 6H,7H,13H,14H-5a,6a,7a,12a,13a,14a-hxaazbenz[f]indeno[2,1,8- ija]naphth[2,3-f]azulene- 14b, 14c-dicarboxylic-5,8,12,15-tetrahydro-6,8,14-trioxo-diethyl ester (C27H26N6OT, Mr = 546.54) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P211c with a = 8.8129(6), b = 17.9883(13), c = 16.2623(11)A, β = 98.770(2)°, V = 2547.9(3)A3, Z = 4, De= 1.425 g/cm3, p(MoKa) = 0.105 mm-1, F(000) = 1144, the final R = 0.0672 and wR = 0.1162 for 2275 observed reflections with I 〉 2σ(I). The crystal structural analysis shows that intermolecular C-H...O hydrogen bonds and π-π stacking interactions result in a three-dimensional framework. The binding study by fluorescence spectroscopy titration showed that he title compound can selectively recognize Fe3+ with fluorescence quenching.  相似文献   

2.
A new Cd(II) coordination polymer, namely, [Cd3(1,2,3-BTC)2(L)2]·2.25H2O (1, L = 2-(2-chloro-6-fluorophenyl)-1H-imidazo[4,5-A][1,10]phenanthroline and 1,2,3-BTC = 1,2,3-ben- zenetricarboxylate), has been synthesized under hydrothermal conditions. The compound was characterized by single-crystal X-ray diffraction. It crystallizes in triclinic, space group Pī with α = 11.650(2), b = 12.240(2), c = 19.760(4) A, α = 72.01(3), β = 77.11(3), γ = 83.48(3)°, V = 2609.4(9) A3, Z = 2, C56H31Cd3Cl2F2N8O14.25, Mr = 1489.99, Dc = 1.896 g/cm3, F(000) = 1466, μ(MoKa) = 1.401 mm^-1, R = 0.0401 and wR = 0.1104. Compound 1 shows a 1D chain structure, and the neigh- boring 1D chains of 1 are joined together by π···π interactions to result in a 2D supramolecular layer. In addition, the luminescent property of 1 has been studied in the solid state at room temperature.  相似文献   

3.
Two new complexes, [Cu(DMB)2(NAA)2](1) and [Co(DMB)2(NAA)2](2)(DMB = 5,6-dimethylbenzimidazole, HNNA = 1-naphthylacetic acid), were hydrothermally synthesized and characterized by elemental analysis, IR spectroscopy, TGA, PXRD and single-crystal X-ray diffraction analysis. The coordination geometry of the metal centers is a perfect square plane for 1 and a distorted tetrahedron for 2. In compound 1, the mononuclear units are linked by N–H···O hydrogen bonds to form a 1D chain structure, while mononuclear motifs of 2 are extended via N–H···O hydrogen bonding and π-π stacking interactions into a 2D supramolecular layer. The remarkable catalytic properties of the two complexes for the degradation of Congo red dye have been found.  相似文献   

4.
Two unusual complexes [Cda(Do)4(H2O)2CI](PW12O4O)'2H2O (1) and [Aga(Do)6(PW12O40)][Ag(Do)2]2(PW12O4O)'2H2O (2) were hydrothermally synthesized by the combination of two different metallic salts, Keggin-type polyoxometalate and 1,10-phen-5,6-dione (Do), and characterized by elemental analyses, inductively coupled plasma analyses, infrared spectra, X-ray photoelectron spectroscopy, thermal gravimetry, photoluminescent spectra and single-crystal X-ray diffraction analyses. Crystal 1 is of monoclinic, space group P21/n with a = 12.383(3), b = 18.326(4), c = 16.437(3) A, β = 90.29(3)°, V = 3730.1(13) A3, Z = 2, CdzCasH32NsC1052PW12, Mr. = 4050.24, Dc = 3.604 g'cm-3,μ(MoKa) = 19.145 mm1, F(000) = 3608, GOOF = 1.168, the final R = 0.0569 and wR = 0.0745 for 5715 observed reflections (1 〉 2σ(I)). Crystal 2 is of triclinic, space group Pi with a = 13.959(5), b = 16.972(5), c = 17.647(5)A, α = 85.970(5), β = 81.353(5), γ = 86.316(5)°, V = 4117(2) A3 Z = 1, Ag6C120H64N200102P2W24, Mr. = 8539.47, Dc = 3.444 g-cm-3,μ(MoKa) = 17.511 mm-1, F(000) = 3828, GOOF = 1.033, the final R = 0.0981 and wR = 0.1658 for 9906 observed reflections (I 〉 2σ(I)). Structural analyses show that complex 1 has a zero dimensional structure, which is further assembled into a one-dimensional ladder-like structure through hydrogen bonds. Complex 2 possesses a one-dimensional chain structure. Furthermore, solid-state luminescent spectra of complexes 1 and 2 indicate red and green fluorescent emission, respectively.  相似文献   

5.
The coordination polymer, [Mn3(bpta)2(bip)2], (H3bpta = biphenyl-3,3',5-tricar- boxylic acid, bip = 2,6-bis(imidazole-1-yl)pyridine), has been synthesized under hydrothermal con- ditions and characterized by elemental analysis, FT-IR, XRD, TGA and single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21/c with a = 14.919(3), b = 9.780(2), c = 20.352(7) A, V = 2344.4(10) A3, Z= 2, C52H32Mn3N10012, Mr = 1153.70, Dc = 1.634 g/cm3, p(MoKa) = 0.876 mm-1, F(000) = 1170, the finalR = 0.0605 and wR = 0.1177. The complex forms a 2D layer with trinuclear Mn(II) units and further assembles into a 3D supramolecular network structure through C-H..'O hydrogen bonding and C-H...π interactions. Moreover, the negative J value indicates the presence of antiferromagnetic coupling between the Mn(II) ions within a trinuclear unit.  相似文献   

6.
The complex [Cu2(H2dhbd)2(tpy)2]·CH3OH·4H2O 1 (H4dhbd =2,3-dihydroxybutanedioic acid, tpy = 2,2':6',2''-terpyridine) has been hydrothermally synthesized and characterized by single-crystal X-ray diffraction analysis. The crystal is of triclinic, space groups Pi with a= 8.6859(17), b = 11.223(2), c = 12.275(2)A, α = 112.454(3), β= 98.435(3), γ = 105.593(3)°, V= 1022.5(3) A^3, Z = 1, C38H42Cu2N6O18, Mr = 997.86, Dc = 1.621 g/cm^3, μ= 1.127 mm^-1, F(000) = 514, T = 293(2) K, the final R = 0.0539 and wR = 0.1394 for 3550 observed reflections with I 〉 2σ(I). In the dinuclear unit, two Cun atoms are bridged by two H2dhbd chelate anions, forming a 14-membered ring, in which the distance of Cu…Cu atoms is 7.0526(12)A. Adjacent dinuclear units are constituted through π-π interactions and C-H…O hydrogen-bonding interactions, fashioning the final 3-D supramolecular framework with 1-D open channels. Variable-temperature magnetic susceptibility measurement indicates the presence of weak antiferromagnetic exchange interactions between Cu^II ions.  相似文献   

7.
1 INTRODUCTION With the increasing interest in diode-pumped solid state lasers, researches on more efficient new materials for diode pumping become more important. The double borates are a type of excellent laser gain media, for example, Nd3 -doped RAl…  相似文献   

8.
A manganese(Ⅱ) complex (tataH)2[Mn(pydc)2]·4H2O (C20H28MBN14O12, Mr = 711.50, tata = 2,4,6-triamino-1,3,5-triazine, pydcH2 = pyridine-2,6-dicarboxylic acid) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1^-, with a = 9.9847(3), b = 10.9813(3), c = 15.2616(5)A, a = 101.5310(10), β = 90.2610(10), γ = 116.4600( 10)% V = 1459.44(8)A^3, Z = 2, Dc = 1.619 g/cm^3,μ = 0.539 mm^-1, F(000) = 734, the final R = 0.0292 and wR = 0.0745. In the crystal the Mnn atom is six-coordinated by four carbonyl oxygen atoms and two pyridine nitrogen atoms from two tridentate pydc ligands to furnish a distorted octahedral geometry. The complex shows the A…D…D'…A' H-bonded tetramer. The molecules are packed in a three-dimensional framework structure by the combination of O-H…O, N-H…O and N-H…N hydrogen bonds between (tataH)^+, [Mn(pydc)2]^2- and crystal water.  相似文献   

9.
Six ternary lanthanide complexes formulated as [Ln(2, 4, 6-TMBA)3(5, 5'-DM-2, 2'-bipy)]2 (Ln = Pr 1, Nd 2, Sm 3, Eu 4, Gd 5, Dy 6; 2, 4, 6-TMBA = 2, 4, 6-trimethylbenzoate; 5, 5'-DM-2, 2'-bipy = 5, 5'-dimethyl-2, 2'-bipyridine) have been synthesized under solvothermal conditions and characterized by single-crystal X-ray diffraction, elemental analysis, thermogravimetric analysis, etc. The results of crystal diffraction analysis show that complexes 1–6 are binuclear units, crystallizing in the triclinic space group. Complexes 1–5 are isostructural, and each of the central metal ions has a coordination number of 9. The asymmetric unit of complexes 1–5 consists of one Ln3+, one 5, 5'-DM-2, 2'-bipy ligand, and three 2, 4, 6-TMBA- moieties with three coordination modes: chelation bidentate, bridging bidentate, and bridging tridentate. The coordination geometry of Ln3+ is distorted monocapped square antiprismatic. The binuclear units of complexes 1–5 form a one-dimensional (1D) supramolecular chain along the c-axis via ππ stacking interactions between the 2, 4, 6-trimethylbenzoic acid rings. The 1D chains are linked to form a supramolecular two-dimensional (2D) sheet in the bc plane via ππ stacking interactions between the pyridine rings. Although the molecular formulae of complex 6 and complexes 1–5 are similar, the coordination environment of the lanthanide ions is different in the two cases. The asymmetric unit of complex 6 contains a Dy3+ ion coordinated by a bidentate 5, 5'-DM-2, 2'-bipy and three 2, 4, 6-TMBA- ligands adopting bidentate and bridging bidentate coordination modes. The Dy3+ metal center has a coordination number of 8, with distorted square antiprismatic molecular geometry. The binuclear molecule of 6 is assembled into a six-nuclear unit by ππ weak staking interactions between two 5, 5'-DM-2, 2'-bipy ligands; then, adjacent six-nuclear units form a 1D chain via offset ππ interactions between 5, 5'-DM-2, 2'-bipy ligands on different adjacent units. The adjacent 1D chains are linked by C―H···O hydrogen bonding interactions to form a 2D supramolecular structure. The thermal stability and thermal decomposition mechanism of all the complexes are investigated by the combination of thermogravimetry and infrared spectroscopy (TG/FTIR) techniques under a simulated air atmosphere in the temperature range of 298–973 K at a heating rate of 10 K·min-1. Thermogravimetric studies show that this series of complexes have excellent thermal stability. During the thermal decomposition of the complex, the neutral ligand is lost first, followed by the acid ligand, and finally, the complex is decomposed into rare earth oxides. The three-dimensional infrared results are consistent with the thermogravimetric results. The photoluminescence spectra of complex 4 show the strong characteristic luminescence of Eu3+. The five typical emission peaks at 581, 591, 621, 651, and 701 nm correspond to the 5D07F0, 5D07F1, 5D07F2, 5D07F3, and 5D07F4 electronic transitions of Eu3+, respectively. The emission at 621 nm is due to the electric dipole transition 5D07F2, while that at 591 nm is assigned to the 5D07F1 the magnetic dipole transition. The lifetime (τ) of complex 4 is calculated as 1.15 ms based on the equation τ = (B1τ12 + B2τ22))/(B1τ1 + B2τ2), and the intrinsic quantum yield is calculated to be 45.1%. Further, the magnetic properties of complex 6 in the temperature range of 2–300 K are studied under an applied magnetic field of 1000 Oe.  相似文献   

10.
A new cadmium-organic framework, [Cd2(TBDC)2(DMF)2(H2O)]n (1), was synthesized by solvothermal reaction of rigid carboxylate ligand 2,3,5,6-tetramethyl-l,4-ben- zenedicarboxylate (H2TBDC) and cadmium nitrate and characterized by elemental analysis, infrared spectrum, thermal analysis, PXRD, single-crystal X-ray diffraction and photoluminescence in the solid state. Compound 1 crystallizes in orthorhombic, space group Pca21 with a = 21.487(6), b = 7.790(2), c = 20.666(6) A, C30H40Cd2N2O11, Mr = 829.44, V= 3459.3(16) A3, Z = 4, Dc = 1.593 g.cm-3,μ = 1.29 mm-1, F(000) = 1672, 2.7〈θ〈27.2°, λ(MoKa) = 0.71073 A, T= 293(2) K, the final R = 0.026, wR = 0.0548 and S = 1.027. X-ray diffraction analysis reveals that complex 1 possesses a 3D framework and exhibits rnsw net. Thus, the solid-state luminescent spectrum of 1 displays that the emission of cadmium(lI) complex shows a peak at 317 nm upon 250 nm excitation at room temperature.  相似文献   

11.
利用三苯基氯化锡和2,6-吡啶二甲酸在三乙胺存在下以1:1摩尔比反应,合成了离子型有机锡化合物{[Ph~2Sn]~2[2,6-Py(CO~2)]~3H~2O}^2^-[HNEt~3]^+~2。通过元素分析、红外光谱和核磁共振氢谱对其结构进行了表征。用X射线单晶衍射测定了该化合物的晶体结构。化合物为单斜晶系,空间群P2~1/n,a=1.7073(7)nm,b=1.7447(7)nm,c=2.5333(10)nm,β=109.694(7)°,Z=4,V=6.824(5)nm^3,D~c=1.282g/cm^3,μ=0.793mm^-^1,F(000)=2696,R~1=0.0563,WR~2=0.1539。化合物中两个锡原子呈七配位畸变五角双锥构型。生物活性测试结果表明,该化合物具有较强的体外抗肿瘤活性。  相似文献   

12.
Indolocarbazole derivatives have been reported to be promising organic semicon- ductor candidates and electroluminescent (EL) materials. One novel indolocarbazole derivative, 2,8-acetyl-5,11-dihexyl-6,12-(di-p-tolyl)-5,11-indolo[3,2-b]carbazole (YK4), has been synthesized, and its crystal structure has also been carefully studied. YK4 is triclinic, space groups Pi with a = 9.409(5), b = 13.974(5), c = 15.488(5) A, α = 90.281(5), β = 105.456(5), Z= 93.728(5)°, M,. = 688.94, V= 1958.1(14) A3, Z = 2, Dc.= 1.168 g/cm-3,μ = 0.070 mm-1, F(000) = 740, Rint = 0.0475, R (I〉 20(/)) = 0.1146, wR (I〉 20(/)) = 0.2186, R(all data) = 0.2192 and wR (all data) = 0.2701. Like other indolo[3, 2-b]carbazole derivatives which were introduced in the 5- and 11-positions, the intermolecular short contacts are localized between the pendant groups and acetyl groups of the neighboring indolocarbazole molecules. The molecule of YK4 possesses poor face-to-face π-π stacking between two adjacent molecules in the crystal. The calculated bond lengths and bond angles of YK4 also proved the result of crystallography.  相似文献   

13.
合成了苯并15-冠-5、二苯并18-冠-6与Na_2[Pt(SCN)_6]的配合物:[Na(B15- C-5)]_2[Pt(SCN)_6] (1),[Na(DB18-C-6)]_2[Pt(SCN)_6] (2),并通过元素分析 、红外光谱、单晶X射线衍射进行了表征。1为单斜晶系,空间群P2_1/c,a = 1. 0974(5) nm,b = 1.5187(7) nm,c = 1.3632(6) nm,β = 96.407(7)°,V = 2. 2568(18) nm~3,Z = 2,D_(calcd) = 1.746 g/cm~3,F(000) = 1184,R_1 = 0. 0357,wR_2 = 0.0868。 2为三斜晶系,空间群 P1-bar,a = 1.2500(3) nm,b = 1.2825(3) nm,c = 1.9342(4) nm,α = 106.82(3)°,β = 102.51(3)°,γ = 103.04(3)°,V = 2.7562 nm~3,Z = 2,D_(calcd) = 1.579 g/cm~3,F(000) = 1316,R_1 = 0.0364,wR_2 = 0.0771。配合物分别由两个[Na(B15-C-5)]~+, [Na(DB18-C-6)]~+配阳离子和一个[Pt(SCN)_6]~(2-)配阴离子组成。配阳离子和配 阴离子通过Na-N键形成二维网状结构。  相似文献   

14.
A novel coordination polymer [Na2Pd(2,6-pydc)2(H2O)6]n (2,6-H2pydc = 2,6-pyridinedicarboxylic acid) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclirtic system, space group P21/c, with a = 11.962(2), b = 6.5552(13), c = 12.673(3) A, β = 91.72(3)^o, V = 993.3(3) A^3, Z = 2, Mr = 590.68, Dc = 1.975 g/cm^3,μ = 1.059 mm^-1, F(000) = 592, the final R = 0.0211 and wR = 0.0454. In the crystal the Pd(II) ion adopts a distorted four-coordinated square-planar geometry and bonds to two bidentate 2,6-pyridinedicarboxylate molecules through caronyl oxygen and pyridine nitrogen atoms. The title complex exhibits a novel three-dimensional network structure.  相似文献   

15.
胡胜利  王治国  殷国栋  陶清  郑静 《结构化学》2012,31(11):1569-1574
A new molecular clip based on diethoxycarbonyl glycoluril 5: C42H36N6O6 , has been synthesized and characterized by single-crystal X-ray diffraction. The crystal belongs to orthorhombic, space group Pbca with a=12.7639(5), b=16.9727(7),c=34.2069(14) , V=7410.5(5)3 , Z=8, Dc=1.292 g/cm3 , μ(MoKα)=0.088 mm-1 , F(000)=3024, the final R=0.0655 and wR=0.1566 for 5123 observed reflections with I>2σ(I). The crystal structural analysis shows that intermolecular c-H…O and C-H…N hydrogen bonds stabilized the whole crystal structure. The binding study by fluorescence spectroscope titration showed that the title molecule can selectively recognize Fe3+ with fluorescence quenching.  相似文献   

16.
通过2,4-二苯基-2,3-二氢-1H-1,5-苯并二氮杂与苯甲酰氯苯腙的[2+3]环加成反应制备了标题化合物,用X射线单晶衍射仪测定了其晶体结构。晶体属正交晶系,空间群为Fdd2.晶胞参数:a=1.7628(4)nm,b=5.7512(12)nm,c=1.0227nm,V=10.368(5)nm3,Z=16,Dc=1.262g·cm-3,μ=0.075mm-1,F(000)=4160,1139个可观测衍射点,R=0.0461,Rw=0.0560.  相似文献   

17.
合成了含异硫氰酸根和喹啉(q1)混合配体的钴配合物[Co(NCS)2(q1)2];利用红外光谱、紫外光谱和X射线单晶衍射等手段对其结构进行了表征;研究了配合物在室温下的荧光发射光谱特性.单晶结构解析结果表明,标题化合物属于单斜晶系,P21/c空间群,晶胞参数为:a=1.48633(5)nm,6=0.84444(3)nm,c=1.54116(5)nm,β=92.093(2),V=1.9330(2)nm^3,Z=4,Dc=1.489g/cm^3,μ=1.116mm^-1,F(000)=884,R1=0.0322,wR2=0.0786.配合物中钴离子采用四配位的四面体配位构型,晶体堆积中通过π-π作用形成一维超分子结构.  相似文献   

18.
GU Wen  HAO Yun  CHEN  Hong-Tu WANG  Shi-Fa 《结构化学》2013,(12):1904-1910
The title compound (C29H33NO2, 3) was synthesized and structurally characterized by elemental analysis, IR, MS, 1H- and 13C-NMR and single-crystal X-ray diffraction. The crystal is of monoclinic system, space group P21 with a = 14.428(3), b = 7.3440(15), c = 22.768(5) A, β = 95.17(3)°, V = 2402.7(8) A3, Z = 4, Mr = 427.56, Dc = 1.182 g/cm3, F (000) = 920, 2(MoKa) = 0.71073 A,μ = 0.073 mm-1, the final R= 0.0670 and wR= 0.1002 for 2437 reflections with I〉 2σ(I) Two crystallographically independent molecules with different conformations co-exist in the structure. The crystal structure is stabilized by intermolecular C-H…π interactions which make the molecules stack along the b axis. In addition, the preliminary cytotoxic assay showed that the title compound exhibited moderate inhibitory activity against KB and SW1116 cells.  相似文献   

19.
Pseudostate decomposition of static dipole polarizabilities for ground state H2+ from a Givens-Householder diagonalization of the excitation operator (H" height="17" width="20">0E0) over an N-term basis of appropriate symmetry allows for a rapidly convergent evaluation of C6 dispersion coefficients for H2+–H2+. 27-term pseudospectra of hypergeneralized James functions with a 30-term GGJ+ unperturbed wavefunction with an optimized scale factor δ=0.918 at R=20 give C6 and γ6 values that are accurate to no less than nine significant figures.  相似文献   

20.
The Schiff base organotin(IV) complex {[4-Et2NC6H3(O)C=NC6H3(O)-5-NO2](nBu2Sn)}2 has been synthesized via the reaction between 4-(diethylamino) salicylaldehyde-2-amino-4-nitrophenol Schiff base(H2L) and dibutyltin oxide. Complex C1 has been characterized by IR, 1H NMR, 13 C NMR spectra, and elemental analysis, and its crystal structure was determined by X-ray diffraction. It crystallizes in the monoclinic system, space group P21/n with a = 15.6559(8), b = 9.1657(5), c = 18.8351(10) , β = 107.3440(10)°, Z = 4, V = 2579.9(2) 3, Dc = 1.442 Mg·m-3, μ(MoKα) = 1.025 mm-1, F(000) = 1152, R = 0.0250 and wR = 0.0633. The central Sn atom is coordinated in a hexadentate manner to assume a distorted octahedral configuration. Complex C1 was studied by TGA analysis in air atmosphere. The interaction between complex C1 and the herring sperm DNA was realized through the intercalation of the complex based on the studies by EB fluorescent probe.  相似文献   

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