Theoretical study on the geometry and vibration of 1-[6-(4-Chlorophenyl)-1-[(6-chloropyridin-3-yl)methyl]-2-[(6-chloropyridin-3-yl)methylsulfanyl]-4-methyl-1,6-dihydropyrimidin-5-yl]ethanone

The solid phase FT-IR and FT-Raman spectra of 1-[6-(4-chlorophenyl)-1-[(6-chloropyridin-3-yl)methyl]-2-[(6-chloropyridin-3-yl)methylsulfanyl]-4-methyl-1,6-dihydropyrimidin-5-yl]ethanone (C25H21Cl3N4OS) were recorded in the region 4000-400 and 3500-100cm(-1), respectively. The vibrational spectra have been computed using density functional theory (B3LYP) and ab initio molecular orbital calculation (HF) with 6-31G(d, p) basis sets. A close agreement was achieved between the observed and calculated frequency by employing normal coordinate calculations. The observed and simulated spectra were found to be well comparable.     

Synthesis and Crystal Structure of N-(1,3,4-Thiadiazol-2-yl)-1-[1-(6-chloropyridin-3-yl)methy]-5-methyl-1H-[1,2,3]triazol-4-carboxamide

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 P1 with a=8.4093(11),b=9.4430(12),c=11.1454(14),α=95.508(2),β=111.366(2),γ=115.259(2)°,V=711.42(16) 3,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 > 2σ(I)). 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)o,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…π 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.     

Crystal structure of 1-(diphenylmethylene)-2-(thiazolo[4,5-b]pyridin-2-yl)hydrazine

The 1-(diphenylmethylene)-2-(thiazolo[4,5-b]pyridin-2-yl)hydrazine compound (IV) is synthesized based on a 3-amion-2-chloropyridine precursor and characterized by single crystal X-ray diffraction. The structural analysis reveals that compound IV belongs to the monoclinic system, space group P2₁/c, a = 11.869(5) Å, b = 13.155(6) Å, c = 10.970(5) Å, β = 102.431(5)°, V = 1672.6(12) ų, Z = 4. In the crystal structure, the molecular species are linked by intermolecular N-H...N hydrogen bonds into onedimensional chains.     

Crystal structure of 1-(4-chlorophenyl)-3-{4-[2-(5-ethyl-pyridin-2-yl)-ethoxy]-phenyl}-propenone

The title compound C₂₄H₂₂ClNO₂ belongs to the orthorhombic system, space group Pca2₁ with a = 12.1771(10) Å, b = 4.9305(4) Å, c = 34.419(3) Å, α = β = γ = 90°, V = 2066.5(3) ų, Z = 4, D_c = 1.260 g/cm³, F(000) = 824, R = 0.0402 and wR = 0.1144, S = 1.034, T = 293 K. The compound is a chalcone with 4-chlorophenyl and [(5-ethyl-pyridin-2-yl)-ethoxy]-phenyl substituents bonded at the opposite ends of a propenone group, the biologically active region. The propenone bridge makes dihedral angles of 10.61(23)° and 62.75(22)° respectively, with 4-chlorophenyl and the [(5-ethyl-pyridin-2-yl)-ethoxy]-phenyl group.     

Crystal and molecular structure of the ethanol solvate of 2-[bis(diphenylphosphoryl)methyl]phenol

Crystal and molecular structure of the ethanol solvate of 2-[bis(diphenylphosphoryl)methyl]phenol, C₃₁H₂₆O₃P₂·3/4 C₂H₅OH (I), was determined by X-ray diffraction analysis. Crystals I are monoclinic: a=11.896(3), b=17.207(3), c=28.421(6) Å, β=90.75(2)°, Z=8, space group P2₁/c. The structure of I was solved by direct methods and refined anisotropically by large-block least-squares analysis to R=0.066 (CAD-4 automatic diffractometer, λMoK_α radiation, 3650 independent reflections with I≥3σ). The crystal structure of I contains two independent molecules, Ia and Ib, of the basic substance and two independent solvate molecules of ethanol. The P atoms in molecules Ia and Ib have distorted tetrahedral environments; the average bond lengths are: P=O 1.476(3), P-C(sp³)=1.833(4) and P-C(Ar)=1.809(4) Å. Molecule Ia has an approximate symmetry plane C_s. The conformation of molecule Ib differs from that of Ia in rotation of one diphenylphosphoryl substituent around the P-C(sp³) bond by an angle of ≈34°. In molecule Ia, the O=P-C-P=O fragment has the form of a chela with two nearly parallel P=O bonds. In the crystal structure of I there are O-H...O=P intermolecular H-bonds; in molecules Ia and Ib there is an intramolecular H-bond of C-H...OH type.     

Crystal and molecular structure of 6-(p-bromobenzoyl)-6-azabicyclo[3.1.0]hexane

The molecular structure of 6-(p-bromobenzoyl)-6-azabicyclo[3.1.0]hexane has been determined by a single crystal, three-dimensional x-ray study. The compound crystallizes in the monoclinic space group (P) with four molecules in a unit cell of dimensions a = 8.83, b = 10.15, c = 12.63 ± 0.02Å and β = 94°55′ ± 5′. The aziridine ring is eis fused to the cyclopentane ring with the two rings together in a boat conformation. The fusion angle of the two rings is 110.8°. The aziridine ring has all angles of 60 ±1° and all bond distances of 1.48 ± 0.03Å. The cyclopentane ring has alternately long (1.61 ± 0.04Å) and short (1.52 ± 0.02Å) distances. Non-fusion angles in the cyclopentane ring are 106.0 ± 0.5°. Other molecular parameters are as anticipated. The 844 independent reflections obtained were refined to a final value of R = 0.11₆ using full-matrix least squares techniques.     

Synthesis of (Z)-4-hydroxytamoxifen and (Z)-2-[4-[1-(p-hydroxyphenyl)-2-phenyl]-1butenyl]phenoxyacetic acid

The synthesis of (Z)-4-hydroxytamoxifen and (Z)-2-[4-[1-(p-hydroxyphenyl)-2-phenyl]-1-butenyl]phenoxyacetic acid was accomplished using a McMurry reaction as the key step. The perfluorotolyl derivatives of the McMurry products enabled the separation of the minor undesirable geometrical isomer. The methodology proceeds without E,Z isomerization, employs a very mild final debenzylation step compatible with a large array of functional groups, and can be applied to the generation of a variety of 4-hydroxytamoxifen analogues.     

Monomeric cis-isothiocyanato complexes. Crystal and molecular structure of [Mn(mep)2(NCS)2] (mep=4-methoxy-2-(5-methoxy- 3-methyl-1H-pyrazol-1-yl)-6-methylpyrimidine)

The crystal and molecular structures of [Mn(mep)2- (NCS)2] ({ {mep}}=4-methoxy-2-(5-methoxy-3-methyl-1H-pyrazol-1-yl)-6-methylpyrimidine) have been determined by X-ray crystallography. The crystal structure of the title compound is built up of isolated [Mn(mep)2(NCS)2] molecules with the stereochemistry of a distorted octahedron for the MnN6 chromophore. The e.p.r. (Q-band) data are in agreement with the structural data.     

Synthesis and Crystal Structure of 1-（4-Bromobenzoyl）-3- [5-（E）-styryl-1,3,4-thiadiazol-2-yl]urea

1 INTRODUCTION 1,3,4-Thiadiazole derivatives represent an interes- ting class of compounds possessing broad spectrum biological activities[1~4]. Aroyl ureas are known to exhibit diverse biological effects, such as insecticidal, fungicidal, herbicidal and plant growth regulating activities[5~8]. Therefore, it is worthwhile to investi- gate the compounds incorporating both 1,3,4-thiadia- zole nucleus and aroyl urea group. In the previous paper[9], a series of aroyl ureas containing 1,3,4-t…     

4,4’-[1,n-亚烷基双[(E)-2-(4-氧苯基)乙烯基]]双吡啶的光化学性质(英文)

通过E-[4-[2-（4-羟基苯基）乙烯基]吡啶与1,n-二溴烷烃亲核取代反应合成了4,4’-[1,n-亚烷基双[（E）-2-（4-氧苯基）乙烯基]]双吡啶[n=2（Ia）,3（Ib）,4（Ic）,6（Id）].用元素分析、红外、紫外和质子核磁共振谱鉴定了Ia-Id的结构.将Ia-Id的稀溶液用中压汞灯和低压汞灯交替照射,发现其分子内光环加成反应的存在,并且随着亚烷基碳链的延长,反应速度加快.研究还发现锌离子可以与毗陡环上氮原子发生螯合作用使分子内光环加成反应加快.本文化合物荧光很弱,在较高浓度下有较强分子间激基缔合物荧光.     

Synthesis and Crystal Structure of 1-[4-(Pyrimidin-2-yl)piperazin-1-ylmethyl]-1H-benzotriazole

1 INTRODUCTION Based on the reported 1.65 ? high resolution crystal structure of spinach KARI (ketol-acid reduc- toisomerase) complex[1], we obtained 279 molecules with low binding energy toward KARI from MDL/ ACD 3D database searching, using program DOCK 4.0[2]. These potential structures provide further information for the design of new KARI inhibitors, one of novel derivatives of which as the title com- pound has been synthesized. Its crystal structure will provide us more inf…     

Synthesis and tautomerism of 2-[3(5)-aryl(methyl)pyrazol-4-yl]-1-benzimidazoles

An efficient method has been developed for the synthesis of 2-[3(5)-aryl(methyl)pyrazol-4-yl]-1H-benzimidazoles by cyclocondensation of 2-acylmethyl-1H-benzimidazoles benzoylhydrazones with DMF dimethylacetal. The tautomerism of the compounds obtained via migrations of a proton between the pyrazole nitrogen atoms has been studied by ¹H NMR. The more stable tautomers have electron acceptor aryl substituents placed at position 3 of the pyrazole ring and electron donor aryl substituents or a methyl at position 5. __________ Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 9, pp. 1370–1377, September, 2006.     

Crystal structure of 2-(6-chloro-4-P-tolylamino)pyrido[3,2-d]pyrimidin-1-ium-1-yl)acetate oxonium bromide

The crystals of 2-(6-chloro-4-(p-tolylamino)pyrido[3,2-d]pyrimidin-1-ium-1-yl)acetate (zwitterionic form) oxonium bromide, C₁₆H₁₃ClN₄O₂·Br⁻·H₃O⁺ (I) were prepared and studied by single-crystal X-ray diffraction method. The compound crystallizes in the triclinic space group P-1 with a = 8.3121(8) ?, b = 9.3885(8) ?, c = 13.2903(12)?, α = 106.788(2)°, β = 95.204(3)°, γ = 110.871(2)°, V = 905.81(14) ?³, Z = 2; final R = 0.053, wR2 = 0.150. It is interesting that methylene C in the BrCH₂COOH molecule binds to the N1 of the pyrimidine ring. In the crystal studied, two neighboring organic molecules are connected by hydrogen bonds through carboxylate oxygen, oxonium and bromide ions to form a dimer.     

Synthesis of 1-[2-Methyl-6(8)-R-quinolin-4-yl]thiosemicarbazides

1-(2-Methylquinolin-4-yl)thiocemicarbazides and S-(2-methylquinolin-4-yl)thiosemicarbazide hydrochlorides were synthesized by reaction of 6(8)-substituted 4-chloro-2-methylquinolines with thiosemicarbazide under different conditions. Alkaline hydrolysis of the hydrochlorides afforded substituted 1-(2-methylquinolin-4-yl)thiosemicarbazides.     

Crystal structure of 6-[(1-methyl-4-nitroimidazol-5-yl)thio] purine

6-[(l-methyl-4-nitroimidazol-5-yl)thio] purine, is an immunosuppressant derivative of the antitumour drug, 6-mercaptopurine. Crystals are monoclinic witha = 4.488(2),b = 31.886(4), c = 8.067(2)A and β= 105.99(2)° in the space group P2₁/c. The crystal structure was solved by direct methods using diffractometer data and refined by least squares to anR- index of 0.065 for 502 observed reflections. The molecule crystallizes in the N(9)-H tautomer form, in contrast to the N(7)-H tautomer form found in crystals of 6-mercaptopurine and assume a conformation in which the substituents on the sulphur atom are directed away from imidazole moiety of the purine NCL Communication number 3313