Synthesis and Crystal Structure of 2,5-Di- （pyridin-3-yl）-1,3,4-oxadiazolendium Nitrate

In order to continue our studies on the synthesis, properties and coordination of s-tetrazine, 3,6-di-(pyridin-3-yl)-s-tetrazine (II, 3-dptz) was synthesized and characterized by 1H- NMR, MS and IR spectra. And the coordination reaction of 3-dptz with nitrate of Cu(II) was studied. 3-dptz reacting with CuII salt [Cu(NO3)2·2H2O] generates a new salt, nitrate of 2,5-di-(pyridin-3- yl)-1,3,4-oxadiazolene (III). III was determined by IR spectra and single-crystal X-ray diffraction to give the following crystal data: space group P21/c, a = 4.9112(1), b = 8.4101(3), c = 29.499(1) , β = 93.266(2)o, V = 1216.44(7) nm3, Mr = 287.24, Z = 4, Dc = 1.568 g/cm3,μ= 0.122 mm-1, F(000) = 592, R = 0.0430 and wR = 0.1240. The results show that III is composed of one cation and one nitrate anion. The cation consists of one H+ and one 2,5-di-(pyridin-3-yl)-1,3,4-oxadiazol molecule, with the former being attached to the latter via electrovalent bond with N3 atom. And the O(42) atom in the nitrate anion is disordered. Intra- and intermolecular H-bonds are observed in the crystal of the title compound. The mechanism of metal-assisted decomposition was also discussed briefly.     

Synthesis and Crystal Structure of 1-（Trifluoromethyl）-1-（propioloyl）-（E）-3-oxo-（2-thienyl）-（2-naphthylamine）

1INTRODUCTIONTheSchiffbasesderivedfromb-diketonesandaliphaticamineshavebeenshowntoexistastheketo-amines.However,ifsubstituentseitherattheketooraminogrouparearomatic,itmaybeexpectedtheenoliminewillbethefavoredtautomericform[1].Recently,someSchiffbasesderivedfromTTA(4,4,4-trifluoro-1-(2-thienyl)-1,3-butanedione)andPMBPhavebeenstudiedbyWang[2]andYu[3]etal.Inordertostudytherelationshipbetweenthestructuresandperformancesofthesecompounds,thetitlecom-poundwillbereportedherein.2EXPERIMENT…     

Synthesis and Crystal Structure of 4-（4-Bromophenyl）- 3,4-dihydro-6-methyl quinolin-2（1H）-one

The title compound (C16H14BrNO) has been synthesized by the reaction of p-tolylamine, Meldrum’s acid and 4-bromo-benzaldehyde, and its structure was characterized by IR, 1H NMR and X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group P21/n with a = 7.6850(11), b = 8.3004(11), c = 21.301(3) , β = 95.110(2)°, V = 1353.4(3) 3, Mr = 316.19, Z = 4, Dc = 1.552 g/cm3, μ(MoKα) = 3.028 mm-1, F(000) = 640, the final R = 0.0345 and wR = 0.0768. X-ray analysis reveals that the atoms of C(1), C(2), C(3), C(4), C(5) and N(1) form a six-membered ring of boat conformation.     

Synthesis and Crystal Structure of a Novel Three-dimensional Supramolecular Compound [（AgI3）（4-HBPFA）2（H2O）]

1 INTRODUCTION In recent years, the rational design and synthesisof metal-directed supramolecular frameworks throughintermolecular hydrogen bonds, π-π stacking interac-tion or other weak interactions have received muchattention because of their interesting molecular topo-logies and various potential applications in catalysis,superconductor, magnetism, nonlinear optics, sen-sors and molecular recognition[1～4]. On the otherhand, the attachment of mono- or polypyridyl frag-ments to a ferr…     

Synthesis and Crystal Structure of the Complex [Zn（DBSHSH）（py）2]

1 INTRODUCTION Salicylaldehyde salicyloylhydrazone (SHSH) and their deviatives show moderate fungicidal and anti- bacterial activities[1]. Rao has reported some novel lanthanoid complexes of salicylaldehydrazone. Va- rious polyhedral geometries such as distorted octa- hedron, pentagonal bipyramid and distorted square antiprism were tentatively proposed for the com- plexes used as excellent semi-conducting materials[2]. Tang has studied spectrofluorimetric determination of hydrogen perox…     

Synthesis and Crystal Structure of 3-（2-Hydroxy-phenyl）-5-（2-methylphenyl）-6-thoxycarbonyl-cyclohexen-2-one

1 INTRODUCTION The molecular assembly of one- or multi-dimen-sional aggregation by hydrogen bonds is now an im-portant subject of supramolecular chemistry and crys-tal engineering[1, . Supramolecular structures formed 2]via intermolecular hydrogen bonds X–H…X or C–H…X (X = O, Cl, N, et al.) are very common inorganic compounds[3~12], and they generally possessdifferent properties due to these hydrogen bonds. Concerning about the spectra of benzene-contai-ning…     

Synthesis and Crystal Structure of Bi（2-nitrilethyl）aminoacetonitrile

1INTRODUCTIONTheresearchonorganicpolyaminesiscur-rentlyofgreatinterestbecauseoftheirpotentialapplicationsasusefulorganicligands,inwhichtheaminenitrogenatomshavestrongcoordinationabilitytothetransitionmetalions.Theirtransitionmetalcomplexesplayanexcellentr…     

Synthesis and Crystal Structure of Tetra（o-cyanobenzyl）tin

The tetra（o-cyanobenzyl）tin compound has been synthesized by the reaction of cyanobenzyl chloride with tin, and its molecular structure was characterized by elemental analysis, IR spectra, ^1H NMR and X-ray diffraction. Crystal data for this compound： monoclinic, space group C2/c, Mr = 583.24, a = 1.9629（2）, b = 1.05967（13）, c = 1.41249（18） nm, β= 118.180（2）^o, V = 2.5898（5） nm^3, Z = 4, Dc =1.496 g/cm^3, μ（MoKa） = 1.015 cm^-1, F（000） = 1176, R = 0.0189, wR = 0.0497 （observed reflections with I 〉 20（I）） and R = 0.0218, wR = 0.0513 （all reflections）. The molecular structure adopts a distorted tetrahedral geometry around the tin atom. The Sn＇＂N weak interaction between the Sn and N atoms of cyano forms an intermolecular H-bonding, and the bond length is 0.3570 nm; the interaction between hydrogen of methylene and benzene ring of benzyl forms C-H…C with its bond length of 0.2817 nm; and the interaction among hydrogen of benzene ring and carbon of cyano forms Ph-H…C bond （0.2897 nm） Of the σ…π interaction. A 3D chain structure is formed by the above weak intermolecular interactions.     

Synthesis and Crystal Structure of N-(2-(1-butyl-3-phenylureido)-1H-indol-3-yl)-N-(4-chlorophenyl)benzamide

<正>The title compound N-(2-(1-butyl-3-phenylureido)-1H-indol-3-yl)-N-(4-chloro- phenyl)- benzamide (C_(32)H_(29)ClN_4O_2, M_r = 537.04) was synthesized by a sequential Ugi four com- ponent condensation (4CC)/aza-Wittig/carbodiimide-mediated cyclization, and the structure was characterized by NMR, IR, MS, elemental analysis and X-ray single-crystal diffraction analysis. The crystal belongs to orthorhombic, space group P2_12_12_1 with a = 11.3663(9), b = 13.3248(10), c = 18.7887(15), V = 2845.6(4)~3, Z = 4, D_c = 1.254 mg/m3, μ = 0.170 mm~(-1), F(000) = 1128, the final R = 0.0538 and wR = 0.1187. X-ray analysis reveals that the new five-membered ring (C(14)-C(15)-N(2)-C(16)-C(21)) and the benzene ring (C(16)-C(21)) are nearly coplanar.     

Synthesis and Crystal Structure of 3-（1-Ethyl-1H-indole-3-carbonyl）aminopropionic Acid

3-(1-Ethyl-1H-indole-3-carbonyl)aminopropionic acid has been synthesized by alkylation of 3-(1H-indole-3-carbonyl)aminopropionic acid methyl ester with bromoethane,follo-wed by saponifying and acidating,in 89.0% yield.Its crystal structure was gotten and determined by X-ray diffraction method.The crystal is of orthorhombic,space group P212121 with a = 8.9490(12),b = 11.1010(15),c = 13.0475(18) ,V = 1296.2(3) 3,Z = 4,Dc = 1.334 g/cm3,λ = 0.71073 ,μ(MoKα) = 0.095 mm-1,Mr = 260.29 and F(000) = 552.The structure was refined to R = 0.0306 and wR = 0.1445 for 2612 observed reflections with I 2σ(I).In the crystal structure,molecules are linked to each other through hydrogen bonds of N(2)-H(2)···O(1) and O(3)-H(3)···O(1),generating a three-dimensional network.     

Synthesis and Crystal Structure of (Z)-N-(2-(diethylamino)ethyl)-7-(5-fluoro-2-oxoindolin-3-ylidene)-2-methyl-4,5,6,7-tetrahydro-1H-indole-3-carboxamide Methanol Solvate

The crystal structure of a new compound (Z)-N-(2-(diethylamino)ethyl)-7-(5- fluoro-2-oxoindolin-3-ylidene)-2-methyl-4,5,6,7-tetrahydro-1H-indole-3-carboxamidemethanol solvate (C24H29FN4O2CH4O, Mr = 456.55) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 14.560(3), b = 7.3200(2), c = 22.233(4) , β = 101.78(3)°, V = 2319.7(8) 3 , Z = 4, Dc = 1.307 g/cm 3 , F(000) = 976, μ = 0.092 mm -1 , MoKa radiation (λ = 0.71073), R = 0.0604 and wR = 0.1644 for 4262 observed reflections with I > 2 (I). X-ray diffraction analysis reveals that the indole and pyrrole are almost coplanar. Intramolecular C-H···O and N-H···O hydrogen bonds together with π-π interactions are found in the structure.     

Synthesis and Crystal Structure of Methyl 3-（5- Bromo-1-ethyl-1H-indole-3-carbonyl）aminopropionate

Methyl 3-(5-bromo-1-ethyl-1H-indole-3-carbonyl)aminopropionate has been syn-thesized by the acylation of 5-bromo-3-trichloroacetylindole with β-alanine methyl ester,followed by alkylation with ethyl iodide,in 82.6% yield.Its crystal structure was gotten and determined by X-ray diffraction method.The crystal is of monoclinic,space group P2 1 /c with a=11.7927(8),b=14.9342(8),c=9.0060(5),β=101.558(6)°,V=1553.93(16)3,Z=4,D c=1.510 g/cm 3,λ=0.71073,μ(MoKα)=2.656 mm-1,M r=353.22 and F(000)=720.The structure was refined to R=0.0401 and wR=0.0825 for 1704 observed reflections with I > 2σ(I).In the crystal structure,intermolecular N(2)-H(2)···O(1) hydrogen bond and weak intermolecular bonds (C(1)-H(1) O(1) and C(10)-H(10B) O(2)) are formed,and π-π stacking also exists.     

3-苯基喹唑啉-4(3H)-酮的合成及晶体结构

标题化合物C14H10ON2是由邻硝基苯甲酰苯胺与原甲酸三乙酯在低价钛试剂作用下反应而得。结构通过单晶X-射线衍射分析确定, 其晶体属于单斜晶系, 空间群P21/c, a = 12.080(2), b = 7.793(1), c = 11.599(1) ? b = 97.56(1), Mr = 222.24, V = 1082.4(2) ?, Dc = 1.364 g/cm3, Z = 4, m(MoKa) = 0.88 mm-1, F(000) = 464, R = 0.0385, wR = 0.0851。X-衍射分析表明: 平面I (C(1)~C(6))与平面II (C(9)~C(14))之间的夹角为124.38; 平面I与平面III (ON(1)?N(2)C(7)C(8)C(9)C(14))之间的两面角为125.47; 平面II与平面III之间的两面角为2.76。     

Synthesis and Crystal Structure of （S）-Ethyl-2-（2-methoxy-phenylsulfenamido）-3-（1H-indol-3-yl）propanoate

With an aim to discover novel AHAS inhibitors,the title compound (S)-ethyl-2(2-methoxy-phenylsulfenamido)-3-(1H-indol-3-yl)propanoate (C 21 H 22 N 2 O 4 S,M r=398.47) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis.The crystal belongs to orthorhombic,space group P2 1 2 1 2 1 with a=8.078(2),b=12.824(4),c=18.788(6),V=1946.2(10) 3,Z=4,F(000)=840,D c=1.360 mg/m 3,μ=0.197 mm-1,the final R=0.0433 and wR=0.1035 for 3075 observed reflections with I > 2σ(Ⅰ).The absolute structure Flack parameter X of this compound is 0.00(8).A total of 14375 reflections were collected,of which 3431 were independent (R int=0.0437).X-ray analysis reveals that the crystal structure involves two intermolecular N-H···O and one N-H···S intermolecular hydrogen bonds with the neighboring molecules.The crystal structure was compared with our previously reported (S)-methyl 2-(4-R-phenylsulfonamido)-3-(1H-indol-3-yl)propanoate (R=H(1) and Cl(2)),which provided some useful information of these compounds.     

2-(N-环己胺)-6-三氟甲氧基苯并噻唑的合成及其晶体结构

以利鲁唑为原料,与硫酸肼经回流反应制得2-肼基-6-三氟甲氧基苯并噻唑(2); 2经氯化亚砜氯代制得2-氯-6-三氟甲氧基苯并噻唑(3);3与环己胺经取代反应合成了新化合物2-(N-环己胺)-6-三氟甲氧基苯并噻唑(4),其结构经¹H NMR, IR,元素分析和X-射线单晶衍射表征。4 (CCDC：1 440 686)属三斜晶系,P-1空间群,晶胞参数a=10.617(3) , b=13.607(4) , c=16.619(5) , V=2 201.8 ³, Dc=1.422 g·cm^-3, Z=6, R₁=0.082 0, wR₂=0.235 1。     

Novel Synthesis and Crystal Structure of 2-(4-Methylphenyl)-3-ferrocenyl-4,4-dicyanpyrrolizidine

A novel ferroenyl pyrrolizidine derivative containing cyano groups, 2-(4-methylphenyl)-3-ferrocenyl-4,4-dicyanpyrrolizidine (C26H25FeN3 , Mr=435.34), was synthesized in moderate yields via a facile 1.3-dipolar cycloaddition in refluxing toluene and its crystal structure was determined by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21/c with a=10.3792(10), b=11.4485(11), c=19.1243(15), β=109.496(4)°, V=2142.2(3)3, Dc=1.350 g/cm3, μ(MoKα)=0.721 mm-1 , Z=4, T=113(2)K, F(000)=912, the final R=0.0586 and wR=0.1664.     

A Facile Synthesis and Crystal Structure of 1-Amino-3-(2''-methylphenyl)isoquinolin Hydrochloride

The title compound(C16H15ClN2)has been synthesized by a facile self-condensation of ο-tolunitrile promoted by potassium tert-butanolate in DMPU,and its structure was characterized by 1H NMR,13C NMR,IR,UV,HRMS and X-ray single-crystal diffraction.The crystal belongs to orthorhombic.space group Pna21 with a=19.560(3),b=7.8500(14),c=18.428(3)(A),Dc=1.271g/cm3,Z=8,λ=0.71073(A),μ(MoKα)=0.257 mm-1,Mr=270.75,V=2829.5(8)(A)3,Hack parameter=0.12(12),F(000)=1136,the final R=0.0571 and wR=0.1445 for 2701 observed reflections with I＞2σ(I).The intermolecular N-H…Cl hydrogen bonds link the molecules into a one-dimensional chain running along axis a.