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1.
The title compound (Z)-1-(3-fluorobenzyl)-5-((3-fluorobenzylimino)(2-hydroxy-4- methoxyphenyl)methyl)pyridin-2(1H)-one (C27H22F2N2O3,Mr = 460.47) was synthesized and crystallized. The crystal belongs to the triclinic system,space group P1 with a = 9.951(6),b = 10.059(6),c = 12.927(7)A,α = 109.828(7),β = 102.304(7),γ = 104.898(7)°,Z = 2,V = 1110.2(11)A^3,Dc =1.377 Mg/m^3,μ(MoKα) = 0.102 mm^-1,F(000) = 480,the final R = 0.0449 and Rw = 0.1250 for 4595 observed reflections (I 〉 2σ(I)). X-ray analysis reveals that both m-fluorobenzyl groups are diorientationally disordered because of the rotation of C–C single bond which was represented as F(1),F(2) and F(1'),F(2'). The diorientational disorder was refined and gave the occupancies of 0.665(4) and 0.335(4) for F(1) and F(1'),0.631(3) and 0.369(3) for F(2) and F(2'). Hydrogen bonds existing in the cell link different components to stabilize the crystal structure. The active data proved that the title compound has good anti-HBV activity.  相似文献   

2.
The title compound (E)-2-[(4-tert-butyl-5-(4-methoxybenzyl)thiazol-2-ylimino)methyl]phenol was synthesized by the reaction of 5-(4-methoxybenzyl)-4-tert- butylthiazol-2-amine with salicylaldehyde, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 5.9362(8), b = 11.5070(15), c = 29.460(4)A, β= 97.326(3)°, V = 1995.9(5) A^3, Z = 4, F(000) = 808, C22H24N2O2S, Mr= 380.49, De= 1.266 g/cm^3, S = 1.031,μ = 0.181 mm^-1, the final R = 0.0474 and wR = 0.1441 for 4327 observed reflections (I 〉 2σ(I)). Intramolecular O-H…N hydrogen bond is observed in the crystal. The preliminary bioassay showed that the title compound exhibits 95% inhibition rate against Rhizoctonia solani at the test concentration of 500 mg/L.  相似文献   

3.
The crystal structure of the title compound (Z)-5-fluoro-3-(phenyl((5-(pyridin-3- ylmethyl)thiophen-2-yl)amino)methylene) indolin-2-one (C25H18FN3OS, Mr = 427.50) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of orthorhombic, space group P212121 with a = 5.931(1), b = 12.413(1), c = 28.102(2) A, V= 2090.4(3) A3, Z = 4, Dc = 1.358 g/cm3, F(000) = 888, μ= 0.186 mm-1, MoKa radiation (2 = 0.71073), R = 0.041 and wR = 0.105 for 4567 observed reflections with I 〉 2σ(I). X-ray diffraction analysis reveals that the indole and thiophene rings are not coplanar with a dihedral angle of 46.26(5)°. Intramolecular and intermolecular N-H'..O hydrogen bonds together with C-H...π interations can be observed in the lattice.  相似文献   

4.
The title compound, 2,6-bis(benzimidazo(1,2-c)quinazolin-6-yl)pyridine tetrahydrate, was synthesized by simple condensation of 2-(2-sminophenyl) benzimidazole with pyfidine- 2,6-dicarboxylic acid and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group C2/c with a = 22.226(8), b = 16.730(7), c = 16.820(5)A, β = 115.796(13)°, V = 5631(4)A^3, C33H27NTO4, Mr = 585.62, Z = 8, Dc = 1.381 g/cm^3, λ(MoKα) = 0.71073 A, F(000) = 2448 and μ = 0.09 mm^-1. The structure was refined to the final R = 0.0730 and wR = 0.1573 for 6346 independent reflections (Rint = 0.0801) and 3384 observed reflections (I 〉 2σ(I)). In the crystal, the molecules are linked through intermolecular O-H…O and O-H…N hydrogen bonds. Intermolecular π-π interactions (with distances of about 3.45 A) are pronounced in the crystal structure.  相似文献   

5.
The title compound 3-(2,4-dichlorophenyl)-4-dydroxy-3-(2,4-dichlorophenyl)-4- dydroxy-5-cyclohexanyl-A3-dihydrofuran-2-one 5 has been synthesized by the cyclization of methyl O-(2,4-dichlorophenyl-acetyl)-1-hydroxycyclo-hexane-carboxylate 4, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group Pi with a = 6.8192(3), b = 10.5053(5), c = 10.5811(5)A,α = 71.681(10), β = 78.905(12), γ = 81.036(12)°, C15H14C1203, Mr = 313.18, V= 702.44(6)A3, Z = 2, De= 1.481 g/cm^3, F(000) = 324,μ = 0.465 mm^-1, S = 1.006, the final R = 0.0331 and wR = 0.1363 for 2505 observed reflections with I 〉 2σ(I) and 183 variable parameters. The crystal analysis shows that the cyclohexene unit of the title compound has a quasi-chair conformation, and a one-dimensional chain structure is formed via the intermolecular hydrogen bond O(1)-H(101)…O(2).  相似文献   

6.
A novel compound 5-(p-tolyl)-4-[2-(2,4-dichlorophenoxy)acetamido]-1,2,4-tria zole- 3-thione 2a has been synthesized by the reaction of 5-(p-tolyl)-4-amino-1,2,4-triazole-3-thione 1 with 2-(2,4-dich/orophenoxy)acetyl ch/oride. Interestingly, the title compound 2 was obtained when 2a crystallizes from a mixed solution of petroleum ether and ethyl acetate, and it has been characterized by elemental analysis, IR, ^1H NMR spectra and single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 9.780(5), b = 10.876(6), c = 11.615(6) /A, a = 104.822(7), β= 94.105(6), ), = 94.305(6)°, V= 1185.7(11)/A3, Z = 2,μ = 0.397 mm^-1, Mr= 497.39, Dx= 1.393 g/cm^3, F(000) = 516, S = 1.097, the final R = 0.0730 and wR = 0.2133 for 4111 unique reflections (Rint = 0.0525) with 3212 observed ones. The dihedral angles made by the triazole ring with the methyl- and chloro-substituted benzene rings are 43.5(7) and 50.2(9)°, respectively. Some intra- and intermolecular hydrogen bonds together with C-H…π interactions existing in the lattice stabilize the crystal structure.  相似文献   

7.
4-(4,6-Dimethylpyrimidin-2-yl)-3-thio-allophanic acid methyl ester was synthesized with mixing 2-amino-4,6- dimethylpyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray diffraction measurement were obtained by recrystallization from dimethylformamide at room temperature. The crystal belongs to monoclinic symmetry with space group C2/m, and crystal parameters of a= 1.7537(5) nm, b= 0.6759(2) nm, c=1.1148(3) nm, β=118.557(4)°, V=1.1605(6) nm^3, Z=4, De= 1.375 g/cm^3,μ=0.271 mm^-1, F(000)=504, and 1519 [1〉2σ(I)] observable independent reflections were used for the determination and refmement of the crystal structures with final R1 of 0.0372 and wR2 of 0.0992. The theoretical investigation of the title compound was carried out with DRT-B3LYP/6-311G, HF/6-311G and MP2/6-311G methods, and the atomic net charges and the population were discussed.  相似文献   

8.
A novel coordination polymer [Nd2(PDB)2(CH3COO)2(H2O)3] (H2PDB = pyridine3,4-dicarboxylic acid) has been synthesized by the reaction of Nd(CH3COO)3 with pyridine3,4-dicarboxylic acid under hydrothermal conditions. Elemental analysis, IR spectra and X-ray crystal structure analysis were carried out to determine the composition and crystal structure of the title complex which belongs to the triclinic system, space group P^-1 with a = 6.9409(14), b = 7.5497(15), c = 22.530(5)A, α = 84.79(3), β = 88.15(3), γ= 75.55(3)^o, C18H18N2O15Nd2, Mr = 790.82, Z = 2, V = 1138.5(4) A^3, Dc = 2.307 g/cm^3,μ = 4.593 mm^-1, -6≤h≤8, -5≤k ≤8, -26≤l≤ 26, F(000) = 760, Rint = 0.0298, R= 0.0314 and wR= 0.0695 (I〉 2σ(I)). Nd(1) and Nd(2) are linked into zigzag chains by carboxylate groups of acetate with interesting μ3-η^2:η^2 fashion. The zigzag chains are bridged by PDB to form a 2D framework, and a 3D supramolecular network is further constructed via π-π stacking.  相似文献   

9.
A new Schiff base compound, 2-bromo-4-chloro-6-[(4-methylpyridin-2-ylimino)methyl]phenol (C13H10BrClN20), has been synthesized by the condensation of equimolar 3-bromo-5- chlorosalicylaldehyde and 4-methylpyridin-2-ylamine in a methanol solution. The compound was characterized by elemental analysis, IR spectra, and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21 with a = 6.048(3), b = 14.063(7), c = 7.623(4) A,β = 97.703(7)°, Z = 2, V = 642.5(6)A3, Dc = 1.683 g/cm3, Mr=325.59, 2(MoKa) = 0.71073A,μ = 3.395 mm^-1, F(000) = 324, R = 0.0370 and wR = 0.0662. A total of 3879 reflections were collected, of which 1970 with I 〉 2σ(I) were observed. As expected, the molecule adopts a trans configuration about the C=N double bond. The benzene and pyridine rings are nearly coplanar (mean deviation from the combined plane is 0.031(3)A), with their dihedral angle of 3.3(3)°. The preliminary biological tests show that the compound has excellent antibacterial activities.  相似文献   

10.
The title compound (Z)-ethyl-4-(4-methoxy)benzylidene-2-(3,5-dimethoxyphenyl)- tetrahydrofuran-3,3-dicarboxylate has been synthesized, and its crystal structure was characterized by X-ray single-crystal diffraction. The crystal belongs to triclinic, space group P1, with a = 8.140(3), b = 11.966(4), c = 13.771(5)Aα= 67.366(4), β= 85.165(5), γ= 75.806(4)°, V = 1200.1(7) A3, Z = 2, C26H3008, Mr = 470.50, Dc = 1.302 g/cm^3, F(000) = 500,λ(MoKa) = 0.71073 A, μ= 0.096 mm^-1, R = 0.0659 and wR = 0.1841 for 3080 observed reflections (I 〉 2σ(I)). As a key intermediate of HIV-1 integrase inhibitor, the synthesis and structure confirmation of the title compound are important for further studies.  相似文献   

11.
A novel compound N-(pyridine-2-methyl)-2-(4-chlorophenyl)-3-methylbutanamide, a racemic compound, has been synthesized with 2-(4-chlorophenyl)-3-methylbutyric acid and pyridin- 2-methylanamine as the raw materials, and its crystal structure (C17H19C1N2O, Mr = 302.79) was determined by single-crystal X-ray diffraction analysis. The crystal belongs to monoclinic, space group P21/n with a = 9.624(9), b = 23.14(2), c = 15.626(15)A, β = 106.199(14)°, V = 3342(5) A^3, Z = 8, Dc = 1.204 g/cm^3,μ = 0.23 mm^-1, F(000) = 1280, S = 1.032, R = 0.0681 and wR = 0.1508 for 6513 unique reflections (Rint = 0.0421) with 3375 observed ones. In the crystal structure, there are some intermolecular hydrogen bonds which stabilize the crystal structure. The preliminary bioassay shows that the title compound exhibits good antifungal activity against Botrytis cinerea, Gibberella zeae, Dothiorella gregaria and Colletotrichum gossypii.  相似文献   

12.
The new title compound N-(5-(4-chloro-2-(trifluoromethyl)phenyl)furan-2-carbon-yl)- N'-(4,6-dimethylpyrimidin-2-yl)thiourea (C19H14C1F3N4O2S) has been synthesized, and its crystal structure and biological behaviors were studied. The title compound crystallizes in the monoclinic system, space group P21/c with a = 7.932(5), b = 33.46(2), c = 7.556(5) A, β = 98.058(9)°, V = 1986(2) A^3 Mr = 454.85, Z = 4, Dc = 1.521 g/cm^3, μ = 0.349 mm^-1 and F(000) = 928. The structure was solved by direct methods and refined to R = 0.0724 and wR= 0.1429 for 3494 observed reflections (I 〉 2σ(I)). Intermolecular hydrogen bonds along the b axis together with the continuous π-π interactions construct the three-dimensional architecture of the title compound. The preliminary biological tests show definite herbicidalactivity for the title compound.  相似文献   

13.
The title compound [2-hydroxy-5-(4-hydroxy-3-phenyliminomethyl-benzyl)-benzylidene]-phenyl-amine (C27H22N2O2, Mr = 406.47) was synthesized by 5,5′-methylene-bissalicylal- dehyde with aminobenezene, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group C2/c with a = 4.4026(6), b = 1.501(13), c = 0.95818(12) nm, β = 90.868(2)°, V= 4.2813(9) nm^3, Z= 8, Dc= 1.292 g/cm^3,μ = 0.010, F(000) = 1744, R = 0.0576 and wR = 0.1450 for 3766 observed reflections with I 〉 2σ(I). X-ray analysis reveals that the molecule has a pair of intramolecular OH…N hydrogen bonds.  相似文献   

14.
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   

15.
The crystal structure of the title compound (C12H10ClN7OS, Mr= 335.78) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group Pi with a = 8.4093(11), b = 9.4430(12), c = 11.1454(14) A, α = 95.508(2), β = 111.366(2), γ = 115.259(2)°, V = 711.42(16) A3, Z = 2, Dc = 1.568 g/cm3, F(000) = 344, μ(MoKα) = 0.428 mm-1, the final R = 0.0476 and wR = 0.1243 for 2353 observed reflections (I 〉 2o(/)). The dihedral angles between the pyridine and triazole, thiazole and triazole, and pyridine and thiazole rings are 69.2(1), 9.2(1) and 72.7(1)°, respectively. Intramolecular C(8)--H(8B)...O(1) and N(5)-H(5A)..-N(4) as well as intermolecular C(5)-H(5)...S(1), C(3)-H(3).,.N(6) and N(5)-H(5A)...N(1) hydrogen bonds together with weak C-H...Ir hydrogen-bonding and π-π stacking interactions contribute to the stability of the structure. There is also evidence for significant electron delocalization in the triazolyl system.  相似文献   

16.
In order to shed light upon the nature and mechanism of 4f-3d magnetic exchange interactions, a series of binuclear complexes of lanthanide(3+) and chromium(3+) with the general formula [Ln(L)5(H2O)2Cr(CN)6]·mL· nH2O (Ln=La (1), Ce (2), Pr (3), Nd (4); x=5, y=2, m=1 or 2, n=2 or 2.5; L=2-pyrrolidinone) and [Ln(L)4(H2O)3Cr(CN)6] ·nH2O (Ln=Sm (5), Eu (6), Gd (7), Tb (8), Dy (9), Er (10); x=4, y=3, m=0, n= 1.5 or 2.0; L=2-pyrrolidinone) were prepared and the X-ray crystal structures of complexes 2, 6 and 7 were determined. All the compounds consist of a Ln-CN-Cr unit, in which Ln^3+ in a square antiprism environment is bridged to an octahedral coordinated Cr^3+ ion through a cyano group. The magnetic properties of the complexes 3 and 6-10 show an overall antiferromagnetic behavior. The fitting to the experimental magnetic susceptibilities of 7 give g= 1.98, J=0.40 cm^-1, zJ'= -0.21 cm^-1 on the basis of a binuclear spin system (Scd=7/2, Scr=3/2), revealing an intra-molecular Gd^3+-Cr^3+ ferromagnetic interaction and an inter-molecular antiferromagnetic interaction. For 7 the calculation of quantum chemical density functional theory (DFT), combined with the broken symmetry approach, showed that the calculated spin coupling constant was 20.3 cm^-1, supporting the observation of weak ferromagnetic intra-molecular interaction in 7. The spin density distributions of 7 in both the high spin ground state and the broken symmetry state were obtained, and the spin coupling mechanism between Gd^3+ and Cr^3+ was discussed.  相似文献   

17.
The title compound,bromo-(2-diphenylphosphino-N-(2-oxybenzylidene)-aniline)- nickel,was synthesized by simple condensation of 2-diphenylphosphino-N-(2-oxybenzylidene)- aniline with NiBr2·6H2O and characterized by elemental analysis,IR spectra and single-crystal X-ray diffraction. The crystal belongs to the triclinic system,space group P1 with a = 9.756(2),b = 10.232(2),c = 13.313(3)A,α = 95.09(3),β = 102.48(3),γ = 95.45(3)o,V = 1283.5(4) A^3,C29H23BrNNiO2P,Mr = 587.07,Z = 2,Dc = 1.519 g/cm^3,λ(MoKα) = 0.71073 A,F(000) = 596 and μ = 2.402 mm^-1. The structure was refined to the final R = 0.0408 and wR = 0.0965 for 4507 observed reflections (I 〉 2σ(I)). Intermolecular π-π interactions (with distances of about 3.705 A) are pronounced in the crystal structure. Under methylaluminoxane (MAO) activation,the title compound was able to catalyze norbornene polymerization,exhibiting good polymerization activities.  相似文献   

18.
A new dipeptide compound, (R)-2,4-dioxo-5-fluoro-1-[1-(methoxycarbonyl) ethylaminocarbonylmethyl]-1,2,3, 4-tetrahydropyrimidine (5-FUAPM), has been synthesized and identified by means of elemental analysis, IR, ^1H NMR and ^13C NMR spectra. The single crystal of compound 5-FUAPMoDMF was also obtained and characterized by DSC-TGA techniques. The crystal belongs to orthorhombic space group P212121 with the cell parameters: a= 0.4740(7) nm, b= 1.923(3) nm, c= 1.9229 nm, a=β=y=90°, V= 1.753 nm^3, Z=4, Dc= 1.312 g/cm^3, Mr=346.32, F(000)=728 and u=0.111 mm^-1. The final R and wR are 0.1378 and 0.2862, respectively. The result of the biological test showed that the compound 5-FUAPM has certain antitumor activities.  相似文献   

19.
A novel hydrochloride quaternary ammonium salt (E)-4-(benzyloxy)-2-(cinnamo- yloxy)-N,N,N-trimethyl-4-oxobutan-l-aminium chloride (Cz3HzgNO4Cl2, Mr = 454.37) has been synthesized via the sequence of acetylation and esterification by using L-carnitine (L-4-N-trimethy- lammonium-3-hydroxybutyric acid, LC) and cinnamic acid as the starting materials, and its crystal structure was determined by single-crystal X-ray diffraction method. The crystal belongs to monoclinic, space group P212121 with a = 10.1670(4), b = 10.4488(4), c = 22.9795(11)A, V = 2441.18(18)A3, Z = 4, Dc = 1.236 g/cm3,μ(MoKa) = 0.293 mm-1, F(000) = 960, Flack factor = -0.01(11), the final R = 0.0489 and wR = 0.1550 for 3350 observed reflections (I 〉 2σ(/)) and R = 0.0953 for all 5648 unique reflections. The crystal structure involves a conjugated system which shows a reverse olefin structure.  相似文献   

20.
The title compounds (S)-methyl-2-(4-R-phenylsulfonamido)-3-(1H-indol-3- yl)propanoate (R = H (1), Cl (2)) have been synthesized and their crystal structures also have been determined by X-ray single-crystal diffraction. Compound 1 (C18H18N2O4S) belongs to orthorhombic, space group P212121 with a = 9.6348(14), b = 11.1517(17), c = 16.412(3) A, V = 1763.4(5) A^3, Mr = 358.40, Z = 4, De = 1.350 g/cm^3,/t = 0.209 mm^-1, F(000) = 752, R = 0.0348 and wR = 0.0714. Compound 2 (CI8H17ClN2O4S) crystallizes in orthorhombic, space group P212121 with a = 9.3128(14), b = 10.9655(16), c = 17.783(3) A, V = 1815.9(5) A^3, Mr = 392.85, Z = 4, De = 1.437 g/cm^3, p = 0.352 mm^-1, F(000) = 816, R = 0.0389 and wR = 0.0845. The absolute structure Flack parameters X of compounds 1 and 2 are -0.03(8) and -0.06(7), respectively. X-ray analysis reveals that the crystal structures of these two compounds both involve two intermolecular N-H…O hydrogen bond's.  相似文献   

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