Molecular and Crystal Structure of 1- ( 2- chloro) - Benzoyl - 3- (4- methylphenyl ) Thiourea

1　INTRODUCTIONBenzoylphenyltioureas having a generalformula( ) were reported to have in secticidalactivity〔1〕,which isclosely related to theirstructures,particularly tothedi hedralangle between the- CONH- plane and phenylring〔2〕.Surprisingly there islittle reported in the literature,only three related structures stored in CSD〔3〕 until1 998.In thispaper,we reportthe crystalstructure ofthe title compound.R CONHCSNHR2　EXPERIMENTAL2 .1　Synthesis　　The synthesisofthetitl…     

丙酰皮考林酰肼(C_9H_(11)N_3O_2 )的合成和晶体结构

合成了标题化合物(C9H11N3O2,Mr=193.21),晶体属于单斜晶系,空间群为C2/c, a=13.703(1),b = 9.142(1), c = 16.437(2)?, ( = 105.547(3)(,V = 1983.8(4)?,Z = 8, Dc=1.294g/cm3, F(000)= 816,(??o?α)=0.094 mm-1,R=0.0527, wR=0.1517,I(2((I)的可观察衍射点1596个。有机分子间以氢键相联并形成网状结构,N(2)-H...N(1a)(a: -x+1, y, -z+1/2)和N(3)-H…O(2b)(b: -x+1/2, y-1/2, -z+1/2)键键长分别为3.007(2)和2.786(2)?。     

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 2-Amino-3-ethoxycarbonyl-4-（4-chlorophenyl）-4H, 5H-pyrano-[3,2-c]-benzopyran-5-one

1 INTRODUCTION The coumarins constitute an important class of bioactive natural products[1]. They have been found to possess diverse biological properties including antimicrobial, insecticidal, estrogenic, anticoagulant and antithrombotic activities. Som…     

Synthesis,Crystal Structure and Magnetic Behavior of a New Manganese（Ⅱ） Coordination Polymer [Mn（DPPZ）（PZDC）（H2O）] （DPPZ = Dipyrido[3,2-a：2＇,3＇-c] -phenazine and H2PZDC = Pyrazine-2,3-dicarboxylic Acid）

The title complex, [Mn（DPPZ）（PZDC）（H2O）] 1 （DPPZ = dipyrido[3,2 -a：2＇,3＇- c]phenazine and H2PZDC = pyrazine-2,3-dicarboxylic acid）, has been hydrothermally synthesized and structurally characterized by X-ray single-crystal diffraction, elemental analyses, IR, TG- DTA and magnetic susceptibility measurement. It crystallizes in triclinic, space group P1^- with a = 6.6842（5）, b = 7.5741（6）, c = 20.5755（15）A, α = 90.1160（10）, β = 97.0560（10）, γ = 97.3350（10）°, V= 1025.16（13）A^3, Z = 2, MnC24H14N6O5, Mr= 521.35, Dc= 1.689 g/cm^3, F（000） = 530, μ（MoKa） = 0.699 mm^-1, R = 0.0366 and wR = 0.0810. Compound 1 contains one- dimensional chains which are further stacked through π-π interactions to form a 3D supramolecular architecture. The water molecule O（1W） is involved in hydrogen bonding interactions with symmetric carboxylate oxygen atom 0（4） at （x＋ 1, y＋1, z） and symmetric PZDC nitrogen atom N（6） at （1-x, 1-y, 1-z）, which completes the structure of 1. Magnetic susceptibility measurement indicates that the compound behaves a weak antiferromagnetic exchange interaction.     

Synthesis, Crystal Structure, and Biological Activity of Naphthalen-2-y1-4-methyl-1,2,3-thiadiazole-5-carboxylate

The title compound naphthalen-2-y1-4-methy1-1,2,3-thiadiazole-5-carboxylate(C14H10N2O2S,Mr = 270.31)was synthesized by the reaction of 4-methyl-1,2,3-thiadiazole-5-carbonyl chloride with 2-naphthol,and its structure was characterized by IR,1H NMR,high-resolution mass spectrometry and single-crystal X-ray diffraction.The crystal belongs to orthorhombic,space group Pbcn with a = 23.475(5),b = 9.6640(19),c = 10.814(2)(A°),β = 90.00°,Z= 8,V= 2453.2(9)(A°)3,Mr = 270.30,Dc = 1.464 g/cm3,μ= 0.262 mm-1,F(000)= 1120,R = 0.0444 and wR = 0.1099.X-ray analysis revealed that the thiadiazole and naphthalene rings were non-planar,while,the thiadiazole ring and the ester group were essentially planar,and two intermolecular hydrogen bonds C(6)-H(6)…O(1)and C(14)-H(14)…O(1)were observed.The preliminary biological test showed that the title compound had antifungal and antivirus activities against tobacco mosaic virus.     

Crystal Structure of 3-(4'-Methoxyl)-phenyl-5-cyano- 6-methylthio Pyrimidine-2, 4-diones

1 INTRODUCTIONIt has been reported that various heterocyclic compounds containing nitrogen atoms, especially uracils, have biologically interesting properties in medicinal and pesticidal chemistry as fungicides and herbicides [1]. In our recent research, a novel substituted pyrimidione was synthesized in order to look for new inhibitors with Hill inhibitory [2~4].Preliminary bioassay indicates that some of analogs of the title compound have good Hill inhibitory activity [5].In an attempt…     

Synthesis and Crystal Structure of α-(N-Protected amino) β-lactam Derivative of 1,5-Benzothiazepine

The crystal of the title compound C, C30H30N2O3S has been prepared by reaction of 1,5-benzothiazepine with N-protected glycine and determined by X-ray single crystal diffraction. Crystal data: Mr=498.62, triclinic with P space group, a=10.880(2), b=13.955(3), c=9.537(2)(A), α=99.34(3)°, β=110.43(3)°, γ=88.56(3)°, V=1338.2(5)(A)3, F(000)=528, λ(MoKα)=0.71073(A), Z=2, Dc=1.237g/cm3, μ=0.154mm-1. Final R=0.0453, wR=0.1256 for 3491 observed reflections [I>2σ(I)]. Structure analysis reveals that the substituents at C(23) and C(7) in four-membered ring are located on the same side. The conformation of seven-membered ring is chair-like.     

Synthesis and Crystal Structure of 2-（ 4-Decarboxydehydroabietyl）- 5-p-tolyl-[ 1,3,4 ]-oxadiazole

2-（4-Decarboxydehydroabietyl）-5-p-toyl-[1,3,4]-oxadiazole, C28H34N2O, has been synthesized and characterized by IR, NMR, elemental analysis and single-crystal X-ray diffraction method. The crystal belongs to the orthorhombic system, space group P212121 with a = 6.1351（5）, b = 14.8495（19）, c = 25.9050（2） A, V = 2360.0（4） A3, Z = 4, Mr = 414.57, Dc = 1.167 Mg/m^3, 2 = 0.71073 A,μ（MoKa） = 0.070 mm^-1, F（000） = 896, the final R = 0.0452 and wR = 0.1076 for 1647 observed reflections with I 〉 2σ（I）. There are five rings in the crystal structure of the title compound, but the oxadiazole ring is non-coplanar with the benzene ring D.     

Photocycloaddition of （4－methyl－7－coumarinyl） Oxyacetic Acid Propanediol Diester and X－ray Crystal Structure of Product

Ｐｈｏｔｏｃｙｃｌｏａｄｄｉｔｉｏｎｏｆ（４－ｍｅｔｈｙｌ－７－ｃｏｕｍａｒｉｎｙｌ）ＯｘｙａｃｅｔｉｃＡｃｉｄＰｒｏｐａｎｅｄｉｏｌＤｉｅｓｔｅｒａｎｄＸ－ｒａｙＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＰｒｏｄｕｃｔＤｕＤａ－Ｍｉｎｇ；ＷａｎｇＹｏｎｇ...     

Crystal Structure of Nicotinic Acid(3,5-dinitrobenzoic Acid Organic Adduct

The title compound nicotinic acid(3,5-dinitrobenzoic acid(NDNT)has been obtained by the reaction of nicotinic acid with 3,5-dinitrobenzoic acid in deionic water at room temperature.The crystal is of monoclinic,space group P21/n with a=14.053(6),b=5.046(2),c=20.105(8)A,β=103.573(8)°,C13H9N3O8,Mr=335.23,Z=4,V=1385.8(10)A3,Dc=1.607g/cm3,μ(MoKα)=0.137 mm－1,F(000)=688,R=0.0435 and wR=0.0993 for 1239 observed reflections (I>2σ(I)).In the crystals,the asymmetric unit contains one nicotinic acid (C6H5NO2)and one 3,5-dinitrobenzoic acid (C7H4N2O6)molecules which are linked by some hydrogen bonds to form a twenty-membered hydrogen-bonded ring and an extended linear structure.     

Synthesis and Crystal Structure of 2-Fluoro-4-methyl-3-oxo-4-aza-5α-androst-1-ene-17β-carboxylic Acid Methyl Ester

Synthesis and Crystal Structure of 2-Fluoro-4-methyl-3-oxo-4-aza-5α-androst-1-ene-17β-carboxylic Acid Methyl EsterAuthorJANG Yin-Zhi XIANG Zuo LIANG Da-Wei (Department of Applied Chemistry, Zhejiang Sci-Tech. University, Hangzhou 310018, China)AbstractThe title compound VII, 2-fluoro-4-methyl-3-oxo-4-aza-5α-androst-1-ene-17β-carboxylic acid methyl ester (C21H30FNO3, Mr = 363.46), was prepared through a seven-step reaction from pregnenolone, and characterized by elemental and single-crystal X-ray diffraction analyses as well as IR, MS and 1H-NMR spectra. It is of monoclinic system, space group P21/c with a = 6.3882(7), b = 9.9033(11), c = 15.4925(17) , β = 91.923(2)°, V = 979.57(19) 3, Z = 2, Dc = 1.232 mg/m3, μ = 0.088 mm-1, F(000)= 392, R = 0.0465, wR = 0.0989 and λ(MoKα) = 0.71073 . The structure indicates that the four cycles (A: C(1)-C(2)-C(3)-N(1)-C(5)-C(10), B: C(5)-C(6)-C(7)- C(8)-C(9)-C(10), C: C(8)-C(14)-C(13)-C(12)-C(11)-C(9), D: C(14)-C(15)-C(16)-C(17)-C(13)) are in chairand trans-configurations. The results of crystal structure determination show that there exist weak intra-molecular hydrogen bonds, resulting in a two-dimensional supramolecular frame-work of the title compound.Keywordsfluoro-sterol, synthesis, crystal structure, supramolecule     

Synthesis and Crystal Structure of α-( N-Protected a mino)β- lactam Derivative of 1 ,5-Benzothiazepine

１　ＩＮＴＲＯＤＵＣＴＩＯＮＲｅｃｅｎｔｌｙ,ａｎｕｍｂｅｒｏｆｄｅｒｉｖａｔｉｖｅｓｏｆｂｅｎｚｏｔｈｉａｚｅｐｉｎｅｈａｖｅｂｅｅｎｐｒｅｐａｒｅｄａｎｄｓｔｕｄｉｅｄｆｏｒｔｈｅｉｒｐｈａｒｍａｃｏｌｏｇｉｃａｌａｃｔｉｖｉｔｉｅｓ〔１５〕．Ｉｎｏｕｒｐｒｅｖｉｏｕｓｗｏｒｋ,ｗｅｈａｖｅｉｎｃｏｒｐｏｒａｔｅｄｔｈｅβｌａｃｔａｍｒｉｎｇｉｎｔｏ１,５ｂｅｎｚｏｔｈｉａｚｅｐｉｎｅｂｙｒｅａｃｔｉｏｎｏｆ１,５ｂｅｎｚｏｔｈｉａｚｅｐｉｎｅｗｉｔｈｓｏｍｅａｃｙｌｃｈｌｏｒｉｄ…     

Synthesis and Crystal Structure of (4R, 5R)(5-Hydroxymethyl-2,2-dimethyl- [1,3]dioxolan-4-yl)-bis-(4-methoxy-phenyl)-methanol

1　ＩＮＴＲＯＤＵＣＴＩＯＮＴｈｅα ,α ,α′,α′ ｔｅｔｒａａｒｙｌ 1 ,3 ｄｉｏｘｏｌａｎｅ 4,5 ｄｉｍｅｔｈａｎｏｌｓ (ＴＡＤＤＯＬＳ)ｄｉｏｌｓｗｈｉｃｈａｒｅｒｅａｄｉｌｙａｖａｉｌａｂｌｅｆｒｏｍａｌｋｙｌｔａｒｔｒａｔｅｓ ,ｈａｖｅｂｅｅｎｗｉｄｅｌｙｕｓｅｄａｓｃｈｉｒａｌｌｉｇａｎｄｓｉｎｅｎａｎｔｉｏｓｅｌｅｃｔｉｖｅａｄｄｉｔｉｏｎｒｅａｃｔｉｏｎｓｏｆｃａｒｂｏｎ ｃｅｎｔｅｒｅｄｎｕｃｌｅｏｐｈｉｌｅｓｔｏａｌｄｅｈｙ ｄｅｓ[1 ] ,ｉｎ [2 +2 ]ｃｙｃｌｏａｄｄｉｔｉｏｎｓ[2 ] …     

Synthesis and Crystal Structure of cis - 1,2- Dicy ano- 1,2- b is（ 2- me thyl- 4-bromo-3-thienyl）ethane

The title compound cis-1,2-dicyano-1,2-bis（2-methyl-4-bromo-3-thienyl）ethane has been synthesized and structurally characterized by X-ray single-crystal diffraction method. Crystal data： triclinic, space group P1^1, Z = 2, C14H8Br2N2S2, Mr = 428.16, a = 6.9410（5）, b = 11.0150（9）, c = 11.1760（8） A, α = 70.3390（10）,β = 76.1860（10）, γ = 79.5490（10）°, V= 776.59（10） A^3, Dc = 1.831 g/cm^3, μ（MoKα） = 5.478 mm^-1, F（000） = 416, R = 0.0487 and wR = 0.1453 for 2456 observed reflections with I 〉 2σ（/）. X-ray analysis reveals that the two thiophene rings are significantly twisted with an average dihedral angle of 57.45°. The molecule adopts a photo-active antiparaUel conformation and the distance between the two reactive C atoms of thiophene rings is 3.465（8）A. These structural elements which exhibit a suitable geometry are extensively explored for photochromic behavior in the crystalline state.     

Molecular and Crystal Structure of 4-[2-(4-Dimethy aminophenyl)ethenyl]-1-methypyridinium tetraphenylborate

The title compound, C40H39N2B, Mr=558.54, crystallizes in space group P21/c, monoclinic, a=18.013(3), b=10.821(2), c=17.321(3),β=112.20(1)°, V=3125.9(9)3, Z=4, Dc=1.187g/cm3, μ(MoKα)=0.068mm-1, F(000)=1192. The final R and wR(F2) are 0.0467 and 0.0972 for 2353 observed reflections (I>2σ(I)), respectively. In the title molecule, the pyridyl ring of the cation makes dihedral angle of 19.94° with the phenyl ring. The anion takes a slightly distorted tetrahedral geometry. In the crystal, along the screw axis b, the centrosymmetric anion pairs form double chains, which are in turn related by the glide plane c, forming double layers. The centrosymmetric cation pairs are related by screw axis b and located between the double sheets of the anion.     

Synthesis,Crystal Structure,and Biological Activity of Naphthalen-2-yl4-methyl-1,2,3-thiadiazole-5-carboxylate

The title compound naphthalen-2-yl-4-methyl-1,2,3-thiadiazole-5-carboxylate (C 14 H 10 N 2 O 2 S,M r=270.31) was synthesized by the reaction of 4-methyl-1,2,3-thiadiazole-5-carbonyl chloride with 2-naphthol,and its structure was characterized by IR,1 H NMR,high-resolution mass spectrometry and single-crystal X-ray diffraction.The crystal belongs to orthorhombic,space group Pbcn with a=23.475(5),b=9.6640(19),c=10.814(2),β=90.00°,Z=8,V=2453.2(9) 3,M r=270.30,D c=1.464 g/cm 3,μ=0.262 mm-1,F(000)=1120,R=0.0444 and wR=0.1099.X-ray analysis revealed that the thiadiazole and naphthalene rings were non-planar,while the thiadiazole ring and the ester group were essentially planar,and two intermolecular hydrogen bonds C(6) H(6)···O(1) and C(14) H(14)···O(1) were observed.The preliminary biological test showed that the title compound had antifungal and antivirus activities against tobacco mosaic virus.     

Synthesis and Molecular Structure of 5, 5-Dimethyl-2- (4' -methoxy)phenyl-1, 3, 2- thiazaphospholidine-4-thione 2-sulfide

1 INTRODUCTION In our previous study [1], we found that 1, 3, 2-thiazaphospholidine-4-thione 2-sulfide deriva- tives possessed various bioactivities such as herbicidal, antiviral, fungicidal activity, Which the is strongly held our interest to exploit new method for the synthesis of such phosphorohe- terocycles and investigate their biological activities. Different method for the preparation of 1, 3, 2-thiazaphospholidine-4-thione (one) 2-sulfides have been reported [2~4]. According to …     

Synthesis and Crystal Structure of 5-Nitro-4-salicylideneamino-3-methyl-1,2,4-triazol-5-thione

The crystal structure of 5-nitro-4-salicylideneamino-3-methyl-1,2,4-triazole-5-thione ([C10H9N5O3S]·HCON(CH3)2, Mr=352.38)(CCDC No. 216094) was determined by the single crystal X-ray diffraction method. The crystal belongs to a triclinic system, the space group is P1 with unit cell constants a=0.6113(2) nm, b=1.0836(4) nm, c=1.3132(5) nm, α=74.523(7)°, β=117.68(3)°, γ= 79.769(7)°, V=0.8245(5) nm3, Z=2, Dc=1.419 g/cm3, μ=0.228 mm-1, F(000)=368, R and wR are 0.0579 and 0.1040, respectively, beasd on 3348 unique reflections of which 1925 reflections were observed[I>2σ(I)]. The results indicate that the title compound can be assigned to the thione tautomeric form rather than the thiol tautomeric form. It contains a five membered triazole ring and a phenyl ring with a dihedral angle of 4.35°. The intermolecular hydrogen bond N3-H3…S1, O1-H1…O4 can be observed.     

Crystal Structure and Binding Properties of a New Molecular Clip Based on Diethoxycarbonyl Glycoluril： C42H36N6O6

A new molecular clip based on diethoxycarbonyl glycoluril 5: C42H36N6O6 , has been synthesized and characterized by single-crystal X-ray diffraction. The crystal belongs to orthorhombic, space group Pbca with a=12.7639(5), b=16.9727(7),c=34.2069(14) , V=7410.5(5)3 , Z=8, Dc=1.292 g/cm3 , μ(MoKα)=0.088 mm-1 , F(000)=3024, the final R=0.0655 and wR=0.1566 for 5123 observed reflections with I>2σ(I). The crystal structural analysis shows that intermolecular c-H…O and C-H…N hydrogen bonds stabilized the whole crystal structure. The binding study by fluorescence spectroscope titration showed that the title molecule can selectively recognize Fe3+ with fluorescence quenching.