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1.
Compounds [Zn(2,2'-bipy)(L)Cl]2 1 and [Zn(phen)(L2)]2 2 (2,2'-bipy = 2,2'-bipyridine, HL = 3-methylbenzoic acid, phen = 1,10-phenanthroline) have been synthesized under hydrothermal conditions. 1: monoclinic, space group C2/c, a = 20.240(4), b = 9.2960(19), c = 17.904(4)A, β = 92.63(3)°, V = 3365.1(12) A^3, C36H30Cl2N4O4Zn2, Mr = 784.32, Z = 4, Dc = 1.548 g/cm^3, μ = 1.631 mm^-1, F(000) = 1600, the final R = 0.0367 and wR = 0.1289 for 3867 observed reflections (I 〉 2σ(I)). 2: monoclinic, space group C2/c, a = 23.035(5), b = 9.0395(18), c = 23.799(5) A, β = 98.55(3)°, V = 4900.6(17)A^3, C56H44N4O8Zn2, Mr = 1031.73, Z = 4, Dc = 1.398 g/cm^3, μ = 1.039 mm^-1, F(000) = 2128, the final R = 0.0540 and wR = 0.1287 for 5002 observed reflections (I 〉 2σ(I)). The two compounds have the same space group and similar isolated dinuclear structure, but different space packing structures are formed by different weak intermolecular interactions. Mo- reover, IR and luminescence spectra are also employed to study the crystal structures and pro- perties of these two compounds.  相似文献   

2.
The title compounds 3-(3,5-bis(trifluoromethyl)phenyl)quinoline (1) and 3-(4- fluoro-3-methylphenyl)quinoline (2) were synthesized through Suzuki-Miyaura Cross coupling reaction of 3-bromoquinoloine with aryl boronic acids. The title compounds were characterized by single-crystal X-ray diffraction, 1H NMR, 13C NMR, El-MS, elemental analysis and IR. The crystals of 3-(3,5-bis(trifluoromethyl)phenyl)quinoline (C17H9F6N, Mr = 341.25) belongs to the monoclinic system, space group P21n, a = 12.3072(13), b = 4.9378(6), c = 24.493(2) A, V= 1473.1(3) A3, Z = 4, Dc = 1.539 Mg m-3, 2 - 0.71073A, μ = 0.144 mm^-1, F(000) = 688, the final R = 0.0715 and wR = 0.1873 for 1875 obserwed reflections with I 〉 2σ(I) and the crystal of 3-(4-fluoro-3- methylphenyl)quinoline (C16H12FN, Mr= 237.27) belongs to the orthorhombic system, space group Pca21, a = 23.794(2), b = 3.9094(3), c = 25.669(2) A, V = 2387.7(4) A3, Z = 8, D, = 1.320 Mg m-3, 2 = 0.71073 A, μ = 0.088 mm-1, F(000) = 992, the final R = 0.0534 and wR = 0.1188 for 2270 observed reflections with I 〉 2σ(I).  相似文献   

3.
Two new 1,3-oxazin derivatives, C22H24N2O5(3I) and C19H16N2O5(3II), have been synthesized via an unusual cascade reaction. The attractive aspect of this cascade reaction is that the novel construction of 1,3-oxazine and the direct C-N bond formation from C-C bond can be easily achieved via pyridine-mediated acylation in a one-pot operation. Both compounds have been synthesized and characterized by elemental analysis, IR, NMR spectra and X-ray single-crystal diffraction. Compound 3I crystallizes in monoclinic, space group P21/n with a = 16.282(4), b = 7.4117(18), c = 17.256(5) , β = 103.193(9)°, V = 2027.4(9) 3, Mr = 396.43, Z = 4, Dc = 1.299 g/cm3, F(000) = 840, MoKa radiation(λ = 0.71073 ), the final R = 0.0771 and wR = 0.1582 for 3662 were observed reflections with I 2σ(I). Compound 3II crystallizes in triclinic, space group P1 with a = 7.1265(9), b = 10.1071(13), c = 23.529(3), α = 97.463(9), β = 96.981(9), γ = 94.345(9)°, V = 1600.5(4) 3, Z = 4, Dc = 1.409 g/cm3, F(000) = 736, CuKa radiation(λ = 1.54186 ), the final R = 0.0515 and wR = 0.1241 for 4920 observed reflections with I 2σ(I). The preliminary antibacterial activities of 2 and 3 against E. coli and S. aureus were investigated. The results showed that the inhibiting effect of 3 was higher than that of 2.  相似文献   

4.
YU Peng  ;LI Xi  ;HU Jun  ;XU Yan-Hua 《结构化学》2014,(9):1375-1382
A novel benzisothiazolin-3-one derivative, 2-(benzo[d]isothiazol-3-yloxy)-N-(3- cyano-l-(4-fluorophenyl)-lH-pyrazol-5-yl) acetamide (8), was synthesized from the initial compound benzo[d]isothiazol-3(2H)-one (BIT) 1 and 4-fluoroaniline 3. The structure of the target compound 8 was determined by elemental analyses, IR and 1H NMR. The single crystals of intermediate compound 6 and the target compound 8 were obtained and determined by X-ray diffraction analysis. The preliminary biological activity was also evaluated and the results showed tile target compound exhibited a good anti-microbial activity.  相似文献   

5.
The title compound (C50H.44010) was synthesized and structurally determined by single-crystal X-ray diffraction method. It crystallizes in monoclinic, space group P21/c with a = 16.713(4), b --- 13.189(3), c = 19.434(5) A, β = 104.411(4)°, Mr = 804.85, Dc = 1.288 g/cm3, V = 4149.2(17) A3, Z = 4, F(000) = 1696, #(MoKa) = 0.089 mm-1T = 296(2) K, 7279 independent reflections with 3172 observed ones (I 〉 2δ(/)), R = 0.0520 and wR = 0.1203 with GOF = 0.928 (R = 0.1464 and wR = 0.1657 for all data). The calixarene moiety maintains the symmetric cone conformation through intramolecular O-H…O hydrogen bonds. Preliminary bioassays indicated that the title compound has a potent inhibitory activity against the strand transfer process of HIV-1 integrase.  相似文献   

6.
Two novel cobalt(Ⅱ) compounds were obtained and characterized by X-ray sing- le-crystal diffraction, IR, 1H NMR and elemental analysis. Compound 1 crystallizes in monoclinic, space group P21/n, with a = 18.046(4), b = 11.335(3), c = 19.157(5)A, β = 92.707(3)°, Z = 4, V = 3914.4(16) A3, Mr = 968.56, Dc = 1.644 g/cm3, μ = 1.378 mm^-1, F(000) = 1960, the final R = 0.0367 and wR = 0.0895. The crystal of compound 2 is of monoclinic, space group P211c with a = 8.7253(10), b = 10.9031(13), c = 18.235(2)A,β = 93.2210(10)°, Z = 4, V = 1732.0(3)A3, Mr = 464.21, Dc = 1.780 g/cm3,μ = 1.560 mm-1, F(000) = 932, the final R = 0.0322 and wR = 0.0743.  相似文献   

7.
A new borophosphate compound Cd3 BPO7(Mr = 490.98) has been successfully synthesized by conventional high temperature solid state reaction for the first time and its structure was determined by single-crystal X-ray diffraction. It crystallizes in orthorhombic, space group Pna21, with a = 13.247(3), b = 8.8217(18), c = 5.0792(10), V = 593.56(20)3, Z = 4, Dc = 5.494 g/cm3, λ(CuKα) = 1.5406, F(000) = 880, the final R = 0.0212 and wR = 0.0513 for 1287 observed reflections(I 2σ(I)). In the crystal structure of Cd3 BPO7, the Cd(II) forms a slightly distorted octahedral geometry, BO3 3- and PO4 3- ions linking adjacent Cd(II) ions to form a 3D network. The second harmonic generation(SHG) on powder samples was measured using Kurtz and Perry technique. The result indicates that Cd3 BPO7 exhibits a SHG response 2.2 times larger than that of potassium dihydrogen phosphate(KDP) and is phase-matchable.  相似文献   

8.
The title compound diethyl 1,4-dihydro-2,6-dimethyl-4-(4-methyl-1,2,3-thiadiazol-5-yl) pyridine-3,5-dicarboxylate(C16H21N3O4S, Mr = 351.42) was prepared by the Hantszch reaction with 4-methyl-1,2,3-thiadiazole-5-formaldehyde, ethyl acetoacetate and ammonium acetate in the presence of aluminum chloride in alcohol, and its structure was characterized by IR spectra, 1H-NMR, EA, and single-crystal X-ray diffraction. The crystal of the title compound belongs to monoclinic system, space group P21/n with a = 11.300(2), b = 12.771(3), c = 12.826(3) ?, β = 96.55(3)o, V = 1839.0(6) ?3, Z = 4, Dc = 1.296 g/cm3, μ(MoKa) = 0.71073 mm-1, F(000) = 744, R = 0.0981 and wR = 0.1994. X-ray diffraction result shows that the torsion angles of N(1)–C(2)– C(3)–C(4) and C(2)–C(3)–C(4)–C(8) are 178.9(3)° and –130.3(3)°, respectively. All rings in the title compound are non-planar. The bioassay results indicate that the title compound has good fungicidal activity, good antivirus activity against tobacco mosaic virus and certain extent of insecticidal activity against Mythimna separata.  相似文献   

9.
The title compound trans-4-[(5-(2,4-dichlorophenoxy)-3-methyl- 1-phenyl-1H-pyrazol-4-yl)methyleneamino]- 1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 (C28H23Cl2N5O2, Mr = 532.41) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1- with a = 8.9438(4), b = 11.6065(5), c = 14.2215(6)A, α = 112.566(1), β = 92.324(2), γ = 102.91(1)°, V= 1315.65(10) A^3, Z = 2, Dc = 1.344 g/cm^3,μ(MoKa) = 0.282 mm^-1, λ = 0.71073 A, F(000) = 552, the final R = 0.0587 and wR = 0.1578 for 5071 observed reflections (I 〉 2σ(I)). X-ray analysis reveals that the product is a thermodynamically stable trans isomer. Intra- and intermolecular C( 12)-H(12)…O(1) and C(28)-H(28)...O(1)# 1 hydrogen bonds were observed in the title compound.  相似文献   

10.
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   

11.
A novel manganese(H) coordination polymer [Mn(pdc)]n (pdc = pyridine-2,4- dicarboxylate) has been synthesized under hydrothermal conditions. The crystal is of monoclinic, space group P211n with a = 6.506(4), b = 9.392(6), c = 11.217(7) A, β = 105.650(12)°, V= 660.0(7)A3, Z = 4, Mr = 220.04, Dc = 2.215 g/cm3,μ = 1.971 mm-1, F(000) = 436, Rint = 0.0345, R = 0.0360 and wR = 0.0778 for 1259 observed reflections with I 〉 2σ(I). In the structure, the Mn(Ⅱ) atom is coordinated in a distorted octahedral arrangement by one pyridine N and five carboxylate O atoms from five pdc ligands, each of which coordinates to five Mn atoms to propagate a three-dimensional layered framework.  相似文献   

12.
李欢欢  刘利  明春伦  崔广华 《结构化学》2014,33(7):1050-1056
A new Cd(Ⅱ) coordination polymer, {[Cd(Hnbta)(L)]·H2O}n(L = 1,4-bis(5,6-dimethylbenzimidazol-1-yl)butane), H3nbta= 5-nitrobenzene-1,2,3-tricarboxylic acid), has been hydro-thermally synthesized and characterized by elemental analyses, IR, XRPD, and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/n with a = 17.3056(13), b = 11.0114(9), c = 17.7484(14) A, β = 117.3640(10)o, V = 3003.7(4) A3, Z = 4, C31H31CdN5O9, Mr = 730.01, Dc = 1.614 g/cm3, μ = 0.792 mm-1 and F(000) = 1488. The cadmium(Ⅱ) ions are bridged by Hnbta2- to generate a two-dimensional metal organic framework with fes topology. In addition, the thermal stability and fluorescence properties of the complex were also studied.  相似文献   

13.
The title compound, N,N'-bis-[3-chloro-5-S-(l-menthyloxy)-2(5H)-4-furanon-yl]- propane-l,3-diamine (C31H48Cl2N2O6, Mr = 615.61), has been synthesized and characterized by IR, 1H NMR, MS, elemental analysis and single-crystal X-ray diffraction. The crystal crystallizes in the monoclinic system, space group C2 with a = 16.1091(4), b = 11.1880(3), c = 19.2854(5) A, β = 106.297(2)°, V = 3336.12(15) A3, Z = 4, Dc = 1.226 mg/m3,μ = 0.237 mm^-1, F(000) = 1320, the final R = 0.0531 and wR = 0.0700 for 2760 observed reflections (I 〉 2σ(I)). X-ray analysis reveals that the title compound possesses four rings: two chiral five-membered furanone rings and two six-membered cyclohexane rings with chair conformation, containing eight chiral centers: C2(S), C3(R), C5(R), C10(S), C18(S), C21(R), C22(S) and C25(R). The structure is stabilized by N-H…O hydrogen bonding interaction.  相似文献   

14.
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   

15.
A new Co(ll) polymer [Co(tdc)(l,4-bimb)]n 1 (H2tdc = thiophene-2,3-dicarboxy- lic acid, 1,4-bimb -- 1,4-bis(imidazol-1 '-yl)butane) was synthesized under hydrothermal conditions The compound crystallizes in the monoclinic system, space group C2/c with a = 15.643(9), b = 8.839(5), c=12.952(7) A, β = 105.964(6)°, V= 1721.8(16) A3, Z = 4, Mr = 419.32, Dc= 1.618 Mg/m3,μ = 1.149 mm-1, F(000) = 860, the final R = 0.0243 and wR =0.0613 for 1460 observed reflections with I 〉 2σ(I). The compound presents a three-dimensional (3D) network extended by both tdc2- anions and 1,4-bimb ligands in which the tdc2- anions employ a chelating coordination mode. From the topology point of view, the structure could be described as a 3D 4-connected 65.8 CdSO4-type net. Infrared spectroscopy, elemental analyses, thermogravimetric analysis and powder X-ray diffraction properties of 1 are also investigated.  相似文献   

16.
A new copper(II) complex 3, Cu(C17H13F3O3)2·C5H5N, has been synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group C2/c with a = 17.8511(7), b = 17.4136(7), c = 13.9425(7) A, β = 124.4830(10)°, V = 3572.5(3) A^3, Z = 4, C39H29CuF6NO6, Mr = 785.17,/7(000) = 1604, T = 292(2) K, Dc = 1.460 g/cm^3 and p = 0.691 mm^-1. The structure was refined to R = 0.0477 and wR = 0.1110 for 2935 observed reflections with I 〉 2σ(I). For the title compound, X-ray analysis reveals that the copper(II) is penta-coordinated by four oxygen atoms from the corresponding 1-(4-(benzyloxy)phenyl)-4,4,4-trifluorobutane-1,3-dione ligands and one nitrogen atom of pyridine, forming a distorted square pyramidal geometry. It is found that the trifluoromethyl group, F(1)/F(1'), F(2)/F(2') and F(3)/F(3')), is disordered over two orientations in an approximate 3:1 ratio.  相似文献   

17.
In this paper, 5'-O-tosyl-2,3'-anhydrothymidine has been synthesized and its crystal structure was analyzed. The crystal belongs to the triclinic system, space group P1, with a = 5.397(2), b = 6.1886(18), c = 3.507(5)A, α = 87.74(2),β = 89.84(4),γ = 73.79(2)°, C17H18N2O6S, Mr = 378,39, Z = 1, V = 432.8(3)A^3, Dc = 1.452 g/cm^3, F(000) = 198 and Flack = -0.11(14). No intermolecular hydrogen bonds exist in the crystal, and the angle between benzene ring and pyrimidine planes is 32.23°.  相似文献   

18.
The title compound ethyl 2-(6-(1,3-dioxo-4,5,6,7-tetrahydro-lH-isoindol-2(3H)- yl)-7-fluoro-3-oxo-2H-benzo[b][1,4]oxazin-4(3H)-yl) butanoate 3 was synthesized by the reaction of ethyl 2-(6-amino-7-fluoro-3-oxo-2H-benzo[b][1,4]oxazin-4(3H)-yl) butanoate with 4,5,6,7- tetraydrophthalic anhydride, and its structure was determined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P2 1/n with a = 9.3469(2), b = 16.7715(5), c = 13.7153(4) A, β= 104.9680(10)°, μ = 0.107 mm^-1, Mr = 430.42, V= 2077.08(10) ,A3, Z= 4, Dc = 1.376 g/cm3, F(000) = 904, T= 296(2) K, R = 0.0508 and wR = 0.1478.  相似文献   

19.
Two lead(ll) compounds, [Pb(qlc)(phen)2(NO3)]e-H20 (1) and [Pb(qlc)z(phen)]-3H20 (2) (Hqlc = quinoline-3-carboxylic acid, phen = 1,10-phenanthroline), were synthesized and charac- terized by elemental analysis, single-crystal X-ray diffraction, IR and thermogravimetric analysis. Crystal 1 is of monoclinic, space group C2/c with a = 25.246(5), b = 12.543(3), c = 18.917(4) A, β = 105.77(3)°, V= 5765(2) A3, Z = 4, C68H46N12OllPb2, Mr = 1621.53, Dc = 1.886 g.cm-3,/.t(MoKa) = 5.912 mm-1, F(000) = 3152, GOOF = 1.080, the final R = 0.022 and wR = 0.0571 for 4822 observed reflections (1 〉 2a(/)). Crystal 2 is oftriclinic, space group Pi with a = 8.7883(10), b = 11.7031 (13), c = 15.9320(17) A, a = 69.9400(10), fl = 78.9780(10), 7 = 79.1650(10)°, V = 1497.4(3) A3, Z = 2, C32H26NaO7Pb, Mr. = 785.71, Dc = 1.729 g.cm-s, p(MoKa) = 5.688 mm-1, F(000) = 756, GOOF = 1.106, the final R = 0.0313 and wR = 0.088 for 59i5 observed reflections (1 〉 2σ(I)). Single-crystal X-ray diffraction analysis reveals that 1 exhibits a two-dimensional (2D) layer based on π-π stacking interactions between phen. Simultaneously, the adjacent 2D layers are assembled via π-π stacking interactions between phen and quinoline tings into a 3D supramolecular structure. The zero- dimensional structure of 2 is also further extended by π-π interactions to form a 2D supramolecular layer. Furthermore, these two compounds exhibit photoluminescence at room temperature in the solid state and their photocatalytic activities have been studied by degradation methylene blue.  相似文献   

20.
The title compound (C21H24N4O4, Mr = 396.44) has been synthesized by the func- tionalized ethyl 4-chloro-6-methyl-2-arylamino-furo[2,3-d]pyrimidine-5-carboxylates and mor- pholine. Its structure was confirmed by means of 1H NMR IR, MS and elemental analysis. The crystal structure of the title compound was determined by X-ray single-crystal diffraction. The compound crystallizes in triclinic system, space group P1, a = 7.9919(8), b = 9.9312(1), c = 12.9380(13) A, aα = 86.987(2), β = 83.604(2), γ = 89.641(2)°, V = 1019.08(18) A3, Z = 2, F(000) = 420, Dc = 1.292 g/cm3,μ = 0.091 mm-1, R = 0.0602 and wR = 0.1548 for 3943 independent (Rint = 0.0639) and 3414 observed (I 〉 2σ(I)) reflections, lntermolecular N-H…O and π-π stacking interactions contributed to the stability of the structure. The preliminary biological test indicated the title compound exhibited cytotoxicity against human lung cancer cell lines.  相似文献   

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