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1.
Abstract The two 1-aryl-5-methyl-1,2,3-triazole derivatives were prepared by the 1-aryl-5-methyl-1,2,3-triazol-4-carboxylic acids 3. The yielded products 4a–b were confirmed by NMR, MS, IR spectra. We investigated the crystalline structure of compounds 4a and 4b. Compound 4a, C9H8BrN3, Mr = 238.09, crystallizes in the monoclinic space group P2(1)/n with unit cell parameters a = 11.660(2), b = 7.668(2), c = 11.818(2) ?, α = 90.00, β = 116.01(3), γ = 90.00o. V = 949.6(3) ?3, Z = 4, Dx = 1.665 Mg m−3. The final R was 0.0477. Compound 4b, C13H11N3, Mr = 209.25, crystallized in the orthorhombic space group Pbca with unit cell parameters a = 10.373(2) ?, b = 11.691(2) ?, c = 17.579(4) ?, α = 90.00o, β = 90.00o, γ = 90.00o, V = 2131.8(7) ?3, Z = 8, D
m = 1.304 Mg m−3. The final R was 0.0565.
Index Abstract The two 1-aryl-5-methyl-1,2,3-triazole derivatives were prepared by the 1-aryl-5-methyl-1,2,3-triazol-4-carboxylic acids 3. The yielded products 4a–b were confirmed by NMR, MS, IR spectra. We investigated the crystalline structure of compounds 4a and 4b. Compound 4a, C9H8BrN3, Mr = 238.09, crystallizes in the monoclinic space group P2(1)/n with unit cell parameters a = 11.660(2), b = 7.668(2), c = 11.818(2) ?, α = 90.00, β = 116.01(3), γ =90.00o. V = 949.6(3) ?3, Z = 4, Dx = 1.665 Mg m−3. The final R was 0.0477. Compound 4b, C13H11N3, Mr = 209.25, crystallized in the orthorhombic space group Pbca with unit cell parameters a = 10.373(2) ?, b = 11.691(2) ?, c = 17.579(4) ?, α = 90.00o, β = 90.00o, γ = 90.00o, V = 2131.8(7) ?3, Z = 8, D
m = 1.304 Mg m−3. The final R was 0.0565.
相似文献
2.
Sheng-Li Cao Jie Zhao Nan Zhang Yue Wang Yu-Yang Jiang Yu-Ping Feng 《Journal of chemical crystallography》2011,41(10):1456-1460
Abstract
The title compounds, 4-(3-nitropyridin-2-ylamino)phenol (I) and 4-(3-aminopyridin-2-ylamino)phenol (II), are two intermediates for the synthesis of a potential antitumor agent ABT-751. The reaction of 4-aminophenol with 2-chloro-3-nitropyridine yielded I which was converted into II by reduction. Instead of the Pd/C catalytic hydrogenation described in many literature, reduction with cheap sodium sulfide in aqueous media was utilized for shorting the reaction time and simplifying the operation. The crystal structures of the resultant compounds were determined by single-crystal X-ray diffraction. The compound I is crystallized in P21/c space group of monoclinic system, with a = 11.5236(19) ?, b = 8.7389(17) ?, c = 10.684(3) ? and α = 90.00°, β = 107.76(3)°, γ = 90.00°. The compound II is crystallized in Cc space group of monoclinic system, with a = 10.688(2) ?, b = 14.2181(18) ?, c = 7.9836(15) ? and α = 90.00°, β = 125.801(7)°, γ = 90.00°. In both crystal structures, the intermolecular N–H–O and O–H–N hydrogen bonds link the molecules, which effectively stabilize the structures. 相似文献3.
Joanna Kobylecka Rafal Kruszynski Slawomir Beniak Ewelina Czubacka 《Journal of chemical crystallography》2012,42(4):405-415
Abstract
The zinc(II) and cadmium(II) 2,4-dichlorophenoxyacetate salts were synthesized in mixed water–methanol environment and characterized by elemental analysis, IR spectrometry and thermal analysis coupled with mass spectrometry. The crystal structures were determined by X-ray crystallography (compound 1, [C18H18Cl4O8Zn] n : monoclinic, P21/c, a = 19.094, b = 7.378, c = 8.008, α = 90.00, β = 101.134, γ = 90.00, V = 1106.95; compound 2, [C16H14Cl4O8Cd] n : monoclinic, P21/c, a = 17.730, b = 7.293, c = 8.060, α = 90.00, β = 95.18, γ = 90.00, V = 1037.9). The structural and some thermal data about the presented cadmium salt were previously reported (Song et al. Acta Crystallogr E 62:m2397, 2006; Kobylecka et al. Thermochim Acta 482:49, 2009). 相似文献4.
Abstract
2-(p-Tolylimino-methyl)-phenol-copper (II) has been synthesized and its structure determined by X-ray diffraction. It crystallizes in the monoclinic system, space group P2(1)/c, with the cell parameters a = 12.0266 (15) ?, b = 27.714 (2) ?, c = 11.0043 (11) ?, α = γ = 90.00°, β = 107.7510 (10)°, V = 3493.1 (6) ?3 and Z = 6. The Cu atom is surrounded by two O atoms and two N atoms from two 2-(p-Tolylimino-methyl)-phenol molecules to form a tetrahedron coordination environment. The complex is linked into a column by weak intermolecular interactions. 相似文献5.
《Journal of chemical crystallography》1994,27(11):641-644
The heliangolide-class sesquiterpene lactone 8β-angeloyloxy-9α-acetoxycalyculatolide, C22H26O8,1, crystallizes in orthorhombic space groupP212121 witha=12.455(3),b=12.601(3),c=14.023(5) ?,V=2200(1)?,3
Z=4.R=0.059 for 1735 observed data. The 11,13-dihydro-11α, 13-epoxyatripliciolide-8β-angelate, C20H22O7. 1/2 H2O,2, crystallizes as the hemihydrate with two molecules in the asymmetric unit in triclinic space groupP1 witha=9.422(1),b=9.559(1),c=12.358(3) ?, α=101.62(2)°, β=91.30(2)°, γ=117.80(1)°,V=955.6(7)?3,Z=2.R=0.046 for 3607 observed data. In both, the 10-membered rings adopt approximate chair-boat conformations. Their conformations
are typical for heliangolides. The methyl group C14 is α, while the C-15 has a β-orientation. The α-methylene-γ-lactone istrans-fused at C6 and C7 with H6 β and H7 α. In compound2, the epoxide at C11–C13 has an α orientation. 相似文献
6.
Gang Chen Ying Tang Qun-Zheng Zhang Mei Meng Xiao-Jiang Hao 《Journal of chemical crystallography》2011,41(2):251-254
Abstract
(S)-N-(2-Hydroxyphenyl)pyrrolidine-2-carboxamide was synthesized from Cbz-l-proline through two steps and characterized by NMR and MS. The crystal structure was determined from single-crystal X-ray diffraction data. It crystallizes in the monoclinic space group, P21, with unit cell dimensions a = 7.284(6) ?, b = 10.262(9) ?, and c = 7.975(7) ?, α = 90.00°, β = 114.451(14)°, γ = 90.00° and Z = 2. The absolute configuration of the chiral center is determined as S. In the crystal structure, intermolecular and intramolecular hydrogen bonds are responsible for the formation of a 1-dimensional network. 相似文献7.
Mohd Abdul Fatah Abdul Manan M. Ibrahim M. Tahir Karen A. Crouse David J. Watkin 《Journal of chemical crystallography》2011,41(2):230-235
Abstract
S-methyl 2-(5-chloro-2-oxoindolin-3-ylidene)hydrazinecarbodithioate (SM5ClISA) has been prepared from S-methyldithiocarbazate and 5-chloroisatin. The compound crystallized in monoclinic crystal system with space group P 21/n, Z = 4, V = 1201.85(7) ?3 and unit cell parameters a = 6.5466(2) ?, b = 7.5056(3) ?, c = 24.6509(8) ?, α = γ = 90° and β = 97.1434(18)°. The crystal structure reveals that the compound exists in the thione form with the chlorine occupies the fifth position in the isatin ring with the bond length of 1.739(2) ?. The 5-chloroisatin moiety is trans with respect to the C3–N2 and C3–S4 bonds whereas the methyl group of the dithiocarbazate moiety is cis with respect to the C3–N2 and C3–S5 bonds. 相似文献8.
《Journal of chemical crystallography》1994,27(11):635-639
The germacrolide-class sesquiterpene lactone, 1,10-epoxyparthenolide, C15H20O4,1, crystallizes with two independent molecules in monoclinic space groupP21 witha=10.6845(5),b=9.0763(4),c=15.4326(7) ?, β=105.887(4)°,V=1439.4(3) ?3,Z=4.R=0.037 for 2425 observed data. Its 11βH, 13-dihydro-derivative 1,10-epoxydihydroparthenolide, C15H22O4,2, crystallizes in orthorhombic space groupP212121 witha=7.6414(10),b=12.559(2),c=14.6821(14) ?,V=1409.0(3) ?3
Z=4.R=0.031 for 1555 observed data. The corresponding unexposidized compound, 11βH,13-dihydrocostunolide, C15H22O2,3, crystallizes with three independent molecules in orthorhombic space groupP212121 witha=7.3576(5),b=23.505(3),c=24.185(2) ?,V=4182(1) ?3,Z=12.R=0.070 for 2767 observed data. In all, the 10-membered rings adopt approximate chair-chair conformations. In all, the double
bonds or epoxidized double bonds are E, both methyl groups on the 10-ring are β, and the α-methylene-γ-lactone (or α-methyl-γ-lactone)
istrans-fused at C6 and C7 with H6 β and H7 α. In the dihydro compounds, the H at C11 is β. 相似文献
9.
Ezhumalai Yamuna Makuteswaran Sridharan Karnam Jayarampillai Rajendra Prasad Matthias Zeller 《Journal of chemical crystallography》2010,40(5):402-411
Abstract
Several 4-chloro-6-phenyl-7,8,9,14-tetrahydroquinolino[2′,3′:7,6]cyclohept[b]indole derivatives were obtained in one pot synthesis reactions via acid catalyzed condensation and cyclization of 1-oxo-1,2,3,4,5,10-hexahydrocyclohept[b]indoles with 2-amino-5-chlorobenzophenone in glacial acetic acid. Parent 4-chloro-6-phenyl-7,8,9,14-tetrahydroquinolino[2′,3′:7,6]cyclohept[b]indole and the 10, 11, 12 and 13-methyl derivatives all crystallize in the triclinic space group P[`1] overline{1} . The 11-methyl derivative crystallizes with Z′ = 2, the 10 and 12-methyl isomers cocrystallize as a solid solution of the two molecules, and the 13-methyl derivative and the parent compound each with Z′ = 1. The unit cell parameters for the four structures are a = 10.1826(8), b = 12.3918(7), c = 16.3825(8)?, α = 91.626(1), β = 95.718(1), γ = 94.966(1)° and V = 2,047.7(2) ?3 for the 11 methyl derivative; a = 10.168(2), b = 10.304(2), c = 10.610(2)?, α = 89.169(3), β = 87.774(3), γ = 63.726(2)° and V = 996.0(3) ?3 for the solid solution of the 10 and 12-methyl derivative, a = 9.0412(5), b = 10.4926(6), c = 10.9093(6)?, α = 94.482(1), β = 102.181(1), γ = 95.812(1)° and V = 1,001.13(10) ?3 for the 13-methyl compound, and a = 9.6463(6), b = 10.2395(6), c = 10.6062(6)?, α = 91.7263(8), β = 94.7200(8), γ = 114.0812(7)° and 950.85(10) ?3 for the unsubstituted parent compound. The molecular shape of the molecules is not affected by the substitution pattern and all molecules exhibit the same conformation with very similar geometries. Intermolecular interactions are limited to weak C–H···Cl hydrogen bonds, a small number of π···π stacking interactions and several C–H···π interactions, which, in combination with shape recognition, dominate the packing of the quinolinocyclohept[b]indoles. 相似文献10.
Naijue Zhu Danielle Lightsey Maryam Foroozesh William Alworth Amit Chaudhary Kristine L. Willett Cheryl L. Klein Stevens 《Journal of chemical crystallography》2006,36(5):289-296
Cytochrome P450 enzymes protect the body from foreign substances through a mechanism that involves oxidation of those substances into more readily excretable polar compounds. It has been shown that some naphthoflavones function as substrates of certain P450 enzymes (CYP1A1 and CYP1B1) and with appropriate structural changes may become inhibitors. Moreover, propargyl ether derivatives of adamantane have been shown to function as selective inactivators of some P450 enzymes (CYP2B1 and CYP2B5). In an attempt to improve the potency and selectivity of inhibition, we have designed and synthesized a series of naphthoflavone propargyl ethers. We report here the synthesis, X-ray crystal structures, and inhibition data (IC50 of EROD inhibition in CYP1A1 and CYP1B1 enzymes) of α-naphthoflavone 2′-propargyl ether, β-naphthoflavone 2′-propargyl ether, α-naphthoflavone 4′-propargyl ether, and β-naphthoflavone 4′-propargyl ether. Crystallographic data: α-naphthoflavone 2′-propargyl ether, , a=7.775(1) ?, b=8.062(1) ?, c=13.110(1) ?, α=84.32(1)°, β=75.42(1)°, γ=86.56(1)°, V=790.8(2) ?3; β-naphthoflavone 2′-propargyl ether, , a=7.605(2) ?, b=7.793(1) ?, c=14.167(2) ?, α=77.06(1)°, β=75.41(1)°, γ=89.54(1)°, V=790.9(2) ?3; α-naphthoflavone 4′-propargyl ether, P21/n, a=14.595(2) ?, b=4.708(1) ?, c=24.745(6) ?, β=106.31(2)°, V=1631.8(7) ?3; β-naphthoflavone 4′-propargyl ether, P1, a=4.8871(5) ?, b= 7.9597(7) ?, c=21.788(3) ?, α=81.771(9)°, β=89.918(10)°, γ=72.223(8)°, V= 797.9(2) ?3. 相似文献
11.
Abstract
The X-ray structures of two α-substituted α-(2-pyridyl-N-oxide)ethanols, the α-phenyl- (3a) and α-trifluoromethyl- (3b) derivatives, were determined. On dehydration of 3a, compound 4a was obtained. This study brought a clear proof that the α-(2-pyridyl-N-oxide)ethanols are formed following oxidation with peroxides of their corresponding pyridines. A different molecular packing was observed for the α-trifluoromethyl derivative due to an additional hydrogen bonding. Compound 3a crystallized in the monoclinic space group P 21/n with unit cell parameters a = 5.7416(1) ?, b = 14.3841(4) ?, c = 13.2821(3) ?, β = 94.918(2)°, V = 1092.90(4) ?3, Z = 4, D = 1.308 Mg/m3. Compound 3b crystallized in the triclinic space group P −1 with unit cell parameters a = 6.1209(2) ?, b = 8.1938(4) ?, c = 9.4675(4) ?, α = 73.363(3)°, β = 73.166(3)°, γ = 71.659(3)°, V = 421.32(3) ?3, Z = 2, D = 1.633 Mg/m3. Compound 4a crystallized in the monoclinic space group P 21/n with unit cell parameters a = 9.3579(3) ?, b = 12.7340(3) ?, c = 9.8579(3) ?, β = 117.3249(15)°, V = 1043.63(5) ?3, Z = 4, D = 1.255 Mg/m3. 相似文献12.
Yue-Fei Bai Lei Yuan Yu Chen Li-Juan Wang Chao Wang Tie-Min Sun 《Journal of chemical crystallography》2012,42(4):318-322
Abstract
The title compound, C25H21BrN2O3, was synthesized and structurally characterized by elemental analysis, IR, MS, 1H NMR and single crystal X-ray diffraction. The crystal is of orthorhombic system, space group Pbca with a = 11.706(2) ?, b = 18.038(4) ?, c = 20.369(4) ?, α = 90.00°, β = 90.00°, γ = 90.00°, V = 4301.0(15) ?3, Z = 8, Dc = 1.474 g/cm3, F (000) = 1952.0, μ(MoKα) = 1.941 mm−1, the final R 1 = 0.0670 and wR 2 = 0.2319 for reflections with I > 2σ(I). The crystal structure is stabilized by un-classical hydrogen-bonding C–H···O forming a three-dimensional network. The optimized geometric bond lengths and bond angles obtained by using density functional theory have been compared with X-ray diffraction values. In addition, the preliminary biological test showed that the title compound had anti-Mycobacterium phlei 1180 activity. 相似文献13.
Abstract
The crystal structures of the compounds 1-phenyl-2-(1H-1,2,4-triazolo-yl)-3-phenyl-propen-1-one (2), and 2,4-diphenyl-3-(1,2,4-triazolo-yl)-1H,4H-1,5-benzothiazepine (3) were obtained by single crystal X-ray diffraction. Compound 2 crystallizes in the triclinic system with space group P − 1, a = 8.5553(17) ?, b = 9.6229(19) ?, c = 9.924(2) ?, α = 106.16(3)°, β = 108.03(3)°, γ = 105.14(3)°, V = 690.1(2) ?3, Z = 2. The compound 3 crystallizes in the orthorhombic system with space group Pbca, a = 12.904(3) ?, b = 15.864(3) ?, c = 19.140(4) ?, α = 90°, β = 90°, γ = 90°, V = 3918.3(14) ?3, Z = 8. H-bonds and π–π stacking are the main non-bonding interactions in the molecular structure. Details of the synthesis, structures, and spectroscopic properties of the two compounds are discussed. 相似文献14.
Mohd Abdul Fatah Abdul Manan M. Ibrahim M. Tahir Karen A. Crouse Fiona N.-F. How David J. Watkin 《Journal of chemical crystallography》2012,42(2):173-179
Abstract
New tridentate nitrogen–oxygen–sulfur Schiff base has been prepared from the condensation reaction of S-methyldithiocarbazate and methylisatin. The compound crystallized in triclinic crystal system with space group P − 1, Z = 2, V = 612.92(3) ?3 and unit cell parameters a = 6.8540(2) ?, b = 8.3022(2) ?, c = 11.5243(4) ?, α = 79.8186(13)°, β = 90.5224(14)° and γ = 72.1362(13)°. Crystal structure reveals that the compound exists in the thione form with the methylisatin moiety is trans with respect to the C3–N2 and C3–S4 bonds whereas the methyl group of the dithiocarbazate moiety is cis with respect to the C3–N2 and C3–S5 bonds. The Schiff base was found to be selectively active against the selected Gram positive bacterial strains (Bacillus subtilis and Staphylococcus aureus) with the inhibition zones of 16 and 12 mm, respectively. 相似文献15.
Yan Ling Wang Mei Li Jun Yao Ye Fei Wang Jing Jing Zheng Li Ma 《Journal of chemical crystallography》2010,40(6):501-504
Abstract
A new crystal of 4,5-bis(cyclohexanecarbonylthio)-1,3-dithiolane-2-thione has been prepared at room temperature and characterized by elemental analysis, UV–Vis–NIR absorption spectrum and X-ray single crystal determination. The complex crystallized in triclinic space group P-1 with unit cell dimensions a = 5.37370(10) ?, b = 12.8618(2) ?, c = 15.2481(2) ?, α = 74.8530(10)°, β = 80.6000(10)°, γ = 85.9550(10)°, V = 1003.18(3) ?3, Z = 2, D x = 1.3861(1) g cm−3. The X-ray structure determination revealed that the crystal is centered-symmetrical and the molecules form dimers with a long intermolecular S···S interaction in the crystal. 相似文献16.
Aliakbar Dehno Khalaji Karla Fejfarova Michal Dusek 《Journal of chemical crystallography》2012,42(3):263-266
Abstract
New Schiff base compound bis[(2,3,4-trimethoxy-benzylidenepropylideneamino)phenyl]-ether (1) was synthesized and characterized by elemental analyses (CHN), FT-IR and 1H-NMR spectroscopy and single-crystal X-ray diffraction. The title compound 1 crystallizes in triclinic system, space group P-1, with a = 6.8255(4) Å, b = 10.4346(4) Å, c = 19.4166(8) Å, α = 86.588(3)°, β = 85.019(4)°, γ = 89.042(4)°, V = 1375.12(11) Å3 and Z = 2. It displays a trans configuration about the C=N double bonds. 相似文献17.
Abstract A novel thiazole-based iridium (III) complex (iridium(III)bis(2-p-tolyl-benzothiazolato-N,C2)(acetylacetonate)) has been prepared and fully characterized by EA, IR, 1H-NMR and MS. The molecular structure of the complex has been determined by single crystal X-ray diffraction analysis. The
iridium (III) center adopts a distorted octahedral geometry with cis-O–O, cis-C–C, and trans-N–N chelate disposition. The complex crystallizes in the orthorhombic Pbca space group with cell parameters a = 10.1388(7) ?, b = 18.3565(12) ?, c = 31.021(2) ?, α = β = γ = 90 ° and Z = 8. The electronic absorption and emission spectra of this complex have been investigated.
Index Abstract A novel thiazole-based phosphorescent iridium (III) complex (iridium(III) bis (2-p-tolyl-benzothiazolato-N,C2)(acetylacetonate)) has been prepared and fully characterized by EA, IR, 1H-NMR, MS and X-ray diffraction analysis. 相似文献
18.
Guo-Hua Liu Chuan-Shou Sun Yun-Ning Xue Mei Yao Han Yu 《Journal of chemical crystallography》2010,40(8):675-680
Abstract
Two of N′-N′-(4,6-disubstituted-pyrimidin-2-yl)-N-[2-(2,4-dichlorophenoxypropionyl)]thiourea (4a-4b) had been synthesized and their crystal structures had been determined by X-ray diffraction method. 4a crystallizes in the triclinic space group P-1, with a = 8.053(12) ?, α = 102.84(2)°, b = 10.541(16) ?, β = 106.99(2)°, c = 12.461(19) ?, γ = 94.615(19)°, and D c = 1.470 mg/m3 for Z = 2. 4b crystallizes in the triclinic space group P-1, with a = 7.939(5) ?, α = 105.302(10)°, b = 10.183(7) ?, β = 105.729(9)°, c = 12.764(9) ?, γ = 90.698(11)°, and D c = 1.517 mg/m3 for Z = 2. 相似文献19.
Li rong Yang Cai yun Shao Zi liang Wang Jiang tao Liu Lin fang Zhou 《Journal of chemical crystallography》2010,40(1):58-63
Abstract
The complex [Mn(PMBP)2(CH3OH)2] of manganese(II) with 1-phenyl-3-methyl- 4-benzoyl-5-pyrazolone (PMBP) was prepared and characterized by elemental analysis, thermal analysis, IR. The crystal structure of the complex determined by single crystal X-ray analysis, indicates that PMBP is a bidentate ligand in the complex and Mn(II) atom is six-coordinated and is in a meridional octahedral environment. The compound crystallizes in the monoclinic system, space group P 2(1)/c, with a = 11.038(10) ?, b = 16.254(15) ?, c = 9.540(9) ?, α = 90.00°, β = 105.112(10)°, γ = 90.00°, V = 1,652(3) ?3, D x = 1.354 g cm−3 and Z = 2. The thermal decomposition kinetics of the complex was investigated under nonisothermal conditions using the Achar differential method and the Coats–Redfern integral method. 相似文献20.
Peng-Cheng Lv Kai-Rui Wang Wen-Jun Mao Rui-Qin Fang Jin Chen Jing Xiong Hai-Liang Zhu 《Journal of chemical crystallography》2009,39(12):927-930