Synthesis and Crystal Structure of 3-（4-Chlorophenyl）-8-cyano-2-（di-isopropylamino）-5-methyl-7-（methylthio）-pyrido[4,3-d]pyrimidine-4（3H）-one

The crystal structure of the new title compound 3-(4-chlorophenyl)-8-cyano-2-(di-iso-propylamino)-5-methyl-7-(methylthio)-pyrido[4,3-d]pyrimidine-4(3H)-one(C22H24ClN5OS,Mr = 441.97)has been determined by single-crystal X-ray diffraction. The crystal is of orthorhombic,space group Pna21 with a = 7.6721(5),b = 18.9370(11),c = 15.6260(9),V = 2270.2(2)3,Z = 4,Dc = 1.293 g/cm3,F(000)= 928,μ = 0.283 mm-1,MoKa radiation(λ = 0.71073 ),R = 0.0494 and wR = 0.1062 for 3278 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that all ring atoms in the py-ridopyrimidinone moiety are almost coplanar. Intramolecular C(20)-H(20)···N(4),C(19)-H(19A)···N(3),C(18)-H(18C)···N(3)and C(16)-H(16B)···O(5)hydrogen bonds together with weak C···π interactions are found in the structure.     

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, Crystal Structure and Bioactivities of 1-（4-Chlorophenyl）-3- [ 5-（pyrid-4-yl）- 1,3,4-thiadiazol-2-yl] urea

The title compound 1-(4-chlorophenyl)-3-[5-(pyrid-4-yl)-1,3,4-thiadiazol-2-yl]urea (C14H10ClN5OS, Mr = 331.79) has been synthesized by the reaction of 2-amino-5-(pyrid-4-yl)- 1,3,4-thiadiazole with 4-chlorobenzoyl azide, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to triclinic system, space group P with a = 5.8550(8), b = 7.5668(10), c = 16.416(2) , α = 78.364(2), β = 81.204(2), γ = 84.749(2)°, V = 702.58(16) 3, Z = 2, Dc = 1.568 g/cm3, μ = 0.429 mm-1, F(000) = 340, the final R = 0.0442 and wR = 0.1092 for 2001 observed reflections (I > 2σ(I)). X-ray diffraction analysis reveals that the title molecule is nearly planar. In the crystal structure, the molecules are linked by strong intermolecular N-H…N hydrogen bonds together with weak nonclassical intermolecular (C-H…Y, Y = N, O and Cl) hydrogen bonds and stacked through π-π interactions. The preliminary bioassay shows that the title compound exhibits good fungicidal activities against Rhizoctonia solani, Botrytis cinerea and Dothiorella gregaria.     

Synthesis and Crystal Structure of S-（＋）-N＇-Tertbutylaminocarbonyl-N- [3-methyl-2-（4-chlorophenyl）butyryl] Thiourea

The title compound S-( )-N'-tertbutylaminocarbonyl-N-[3-methyl-2-(4-chlorophenyl)butyryl] thiourea has been synthesized and its crystal structure was determined by singlecrystal X-ray diffraction an alysis. There exist intramolecular N(2)-H(2A)… O(1), C(17)-H(17A)…O(2) and N(3)-H(3A)…S(1) hydrogen bonds as well as intermolecular N-H…O interaction between the carbonyl and amidogen groups. Crystallographic data: C17H24ClN3O2S, Mr = 369.90,monoclinic, space group C2/c with a = 22.9922(19), b = 14.4844(12), c = 12.4618(11) (A),β =92.608(2)°, V= 4145.8(6) (A)3, Z = 8, Dc = 1.185 g/cm3, F(000) = 1568,μ(MoKa) = 0.298 mm-1, R =0.0578 and wR = 0.1308.     

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.     

Synthesis and Crystal Structure of 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

The title compound trans-4-[(5-(2,4-dichlorophenoxy)-3-methyl-1-phenyl-1H-pyra-zol-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) , α = 112.566(1), β = 92.324(2), γ = 102.91(1)o, V = 1315.65(10) 3, Z = 2, Dc = 1.344 g/cm3, μ(MoKα) = 0.282 mm-1, λ = 0.71073 , 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.     

Synthesis and Crystal Structure of 2[1-（1,1-Dimethylethyl）-5-methyl-1-H-pyrazol-4-ylcarbonyl]-N-phenyldrazinecarbothioamide

1INTRODUCTIONThiosemicarbazidespossessingNC=Sgroupareanessentialstructurefeatureresponsibleforvariousbiocidalproperties[1～7].Moreover,theyaretheconvenientandkeyintermediatesforthesyn-thesisofheterocycliccompoundssuchas1,3,4-thiadiazoles,1,2,4-triazoleand…     

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…     

Synthesis and Crystal Structure of 3,3''-(2,2''-(Ethane-1,2-diylbis(oxy))bis(ethane-2,1-diyl))bis(2-(4-chlorophenylamino)quinazolin-4(3H)-one)

The title compound 3,3'-(2,2'-(ethane-1,2-diylbis(oxy))bis(ethane-2,1-diyl))bis(2- (4-chlorophenylamino)quinazolin-4(3H)-one) 3 (C34H30Cl2N6O4, Mr = 657.54) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in space group P1 with a = 9.9185(8), b = 10.6124(9), c = 15.4064(13) , α = 92.896(2), β = 103.813(2), γ = 94.635(2)°, V = 1565.5(2) 3, Z = 2, Dc = 1.395 g/cm3, μ = 0.257 mm–1, F(000) = 684, the final R = 0.0580 and wR = 0.1284 f...     

Synthesis and Crystal Structure of （4S）-5-（2-Methoxy-2-oxoethylamino）-5-oxo-4-（3,4,5-trimethoxybenzamido） Pentanoic Acid

1 INTRODUCTION Aminopeptidase N (APN), a member of mem- brane-bound zinc-dependent exopeptidase, is known to be high expression on the brush border membran- es of the small intestine and renal proximal tubules[1]. The over-expression of APN has been involved in several pathological conditions including cancer[2], leukemia, diabetic nephropathy[3], rheumatoid arth- ritis[4], angiogenesis[5] and central nervous system di- seases, such as Alzheimer’s disease[6]. This has led to the sear…     

Synthesis, Crystal Structure and Fluorescent Properties of 1-（4-（Dimethylamino）benzylidene）- 4-（naphthalen- 1-yl） Thiosemicarbazide

1 INTRODUCTION Recently, for the fluorescent properties, Schiff base has been more and more important and widely studied in density optical memories, nonlinear op- tics (NLO), organic light-emitting diodes (OLED), polymer LED and electrogenerated chemilumines- cence (ECL)[1~5]. Thiosemicarbazones are a kind of Schiff bases with thiourea and good ligands easily chelating with transition metal ions. Although they have been studied extensively for a long time due to their chemical and b…     

Synthesis and Crystal Structure of 4-（2-Bromophenyl）-3,4,7,8-tetrahydro- 7,7-dimethyl-1-p-tolylquinoline-2,5（1H,6H）-dione

The title compound 4-（2-bromophenyl）-3,4,7,8-tetrahydro-7,7-dimethyl-1-p-tolylquinoline-2,5（1H,6H）-dione 1 （C24H24BrNO2, Mr = 438.35） was synthesized and characterized by IR, 1H NMR and elemental analysis. The crystal belongs to monoclinic, space group C2/c with a = 27.565（14）, b = 10.079（5）, c = 15.917（8） A,β = 111.059（9）°, Z = 8, V = 4127（4）A3, Dc = 1.411 g·cm^-3,μ（MoKa） = 2.011 mm^-1, F（000） = 1808, the final R = 0.0417 and wR = 0.1032 for 2393 observed reflections （I 〉 2σ（I））. X-ray analysis reveals that the pyridine ring adopts a distorted boat conformation, while another six-membered ring takes a half-chair conformation. In addition, there are non-classical hydrogen bonds of C-H…O and C-H…Br in the structure. The short distance （3.481A） between the adjacent 2-bromophenyl rings indicates the existence of π-π interaction.     

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 12-（2,4-Dichlorophenyl）-7,8,9,10,11,12-hexahydrobenzo[f]pyrimido [4,5-b]quinoline-9,11-dione DMF Solvate

The title compound 12-(2,4-dichlorophenyl)-7,8,9,10,11,12-hexahydrobenzo-[f]pyrimido[4,5-b]quinoline-9,11-dione DMF solvate 1(C24H20Cl2N4O3,Mr=483.34) was synthesized and crystallized.The crystal belongs to the monoclinic system,space group P21/n with a=6.4798(16),b=20.595(5),c=16.723(4),β=95.267(7)o,Z=4,V=2222.3(9)3,Dc=1.445 g/cm3,μ(MoKα)=0.328 mm-1,F(000)=1000,the final R=0.0530 and wR=0.1388 for 3484 observed reflections(I2σ(I)).X-ray analysis reveals that the central 1,4-dihydropyridine ring is slightly distorted,adopting a half-chair conformation,which is obviously different from the boat conformations of other similar compounds.In addition,the classical hydrogen bonds of N(2)-H(2A)…O(2) are presented in the crystals,and link the adjacent molecules to form dimmers.Atom O(3) in the DMF solvent forms two hydrogen bonds of O(3)…H(1H)-N(1) and O(3)…H(3H)-N(3) with a pyrimidoquinoline moiety,forming an interesting half-chair-like conformation.The hydrogen bonds link the molecules to form dimmers,while intermolecular π-π interaction connects the above-mentioned dimmers to yield a one-dimensional structure.     

Synthesis and Structure of 5-Amino-6-(4-fluorophenylamino)-3-methylthio-1-phenyl-1H-pyrazolo[3,4-d]pyrimidin-4(5H)-one

The title compound (C18H15FN6OS) has been synthesized and its crystal structure was determined by X-ray analysis. The crystal belongs to monoclinic system, space group P21/n with a = 13.983(10), b = 7.337(5), c = 16.702(12) (A), α = 90, β = 98.277(12), γ = 90°, V = 1696(2)(A)3, Z = 4, Dc= 1.498 g/cm3, Mr = 382.42,μ = 0.224 mm-1, F(000) = 792, the final R = 0.0362 and wR = 0.0878 for 2579 observed reflections with I ＞ 2σ(Ⅰ). In the title compound, the atoms of C(1),C(2), C(3), C(4), C(5), N(1), N(2), N(3), N(4), N(5), N(6), O(1) and S(1) form a fully delocalized system with the average deviation of 0.0307(A). There exists a part of electron delocalization over the planes of Ⅰ (pyrazolo[3,4-d]pyrimidin-4-one moiety), Ⅱ (phenyl moiety) and Ⅲ (p-fluorophenylamine moiety). In the molecule, intermolecular hydrogen bonds between N(6)-H(6)…O(1)and C( 15)-H( 15)…O( 1 ) are observed.     

Synthesis,Spectroscopic Properties and Crystal Structure of 3,3＇-（Anthracene-9,10-diyl）bis（1-phenylpropan-1-one）

The compound 3,3'-(anthracene-9,10-diyl)bis(1-phenylpropan-1-one)(C32H26O2,Mr=442.55) has been synthesized by the reaction of 2,2'-(anthracene-9,10-diylbis(methy-lene))bis(1,3-diphenylpropane-1,3-dione) with CsCO3,and its structure was characterized by 1H NMR and single-crystal X-ray diffraction.The crystal of the title compound belongs to monoclinic,space group P21/c with a=9.154(3),b=5.2777(16),c=24.897(7) nm,β=107.337(10)°,Z=2 and V=1.1482 nm3.X-ray analysis indicates that an intermolecular hydrogen bond C(8)-H(8A)…O(1),weak C-H···π between H(9A) and the centre of anthracene rings and weak π-π interactions between two anthracene ring planes are observed.     

Synthesis and Crystal Structure of a 2-D Framework Supramolecular Complex [Cd2（phen）2（adip）（NO3）2]

1 INTRODUCTION In the design of crystal molecule, inorganic crystal engineering is one of the focused fields that are ever developing[1]. The introduction of different metal ions and bridging ligands often gives rise to novel physical and chemical properties[2~4]. Conse- quently, the supramolecular compounds constructed from weak interactions, such as hydrogen bond, π-π stacking, C–H???O interaction, ion-π interaction and hy- drophobing interaction, have become the new focus of cryst…     

Synthesis and Crystal Structure of Isonicotinic Acid [1-（3,5-Dibromo-2- hydroxyphenyl）methylidene]hydrazide Methanol

A new Schiff base compound, C13H9Br2N3O2·CH3OH, isonicotinic acid [1-(3,5- dibromo-2-hydroxyphenyl)methylidene]hydrazide methanol, has been synthesized and characterized by elemental analysis, IR spectra, and single-crystal X-ray diffraction. The compound comprises a Schiff base moiety isonicotinic acid [1-(3,5-dibromo-2-hydroxyphenyl) methylidene]hydrazide and a methanol molecule. The crystal belongs to the triclinic system, space group P1 with a = 8.464(1), b = 9.511(2), c = 10.901(2) , α = 92.940(2), β = 110.456(2), γ = 96.040(2)o, Z = 2, V = 814.0(2) 3, Dc = 1.759 g/cm3, Mr = 431.09, λ(MoKα) = 0.71073 , μ = 4.994 mm-1, F(000) = 424, R = 0.0440 and wR = 0.1061. A total of 3284 unique reflections were collected, of which 2197 with I > 2σ(I) were observed. The molecule adopts a trans configuration about the C=N double bond. The dihedral angle between the benzene and pyridine rings is 22.0(4)o. The crystal structure is stabilized by intermolecular O-H···N and C-H···O hydrogen bonds, forming layers parallel to the ac plane. The preliminary biological tests show that the compound has potential antibacterial activities.     

Synthesis and Crystal Structure of (1-Naphthyl){[3- (2,6-dibromo-4-methylphenylimino)methyl]-5-chloro- 2-hydroxy-benzaldehyde}(triphenylphosphine) Nickel(II) Triphenylphosphine

1INTRODUCTION Over the past decades,olefin oligomerization and polymerization based on late transition metal catalysts have been the most exciting developments in the area of organometallic chemistry and polymer science[1～3].In this broad context,neutral nickel(II)complexes have attracted much attention for their less sensitivity to protonic solvents and polar mon-mers.The most typical one is the SHOP-type cata-lyst[4～6],which contains an anionic[P,O]chelate ring and shows high activ…     

Synthesis and Crystal Structure of [2-Hydroxy- 5-（4-hydroxy-3-phenyliminomethylbenzyl）-benzylidene]-phenyl-amine

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.