Synthesis and Crystal Structure of 1,2-Bis-（p-nitrophenylsulfonamido）-4,5-dinitrobenzene

The title compound, 1,2-bis-(p-nitro-phenylsulfonamido)-4,5-dinitrobenzene, was synthesized and characterized by elemental analysis, IR and 1H NMR. A pale yellow prism crystal of C23H26N8O13S2 (Mr = 686.64) was obtained in DMF solution and determined by single-crystal X-ray diffraction method. It crystallizes in triclinic system, space group P1 with a = 10.346(4), b = 12.210(5), c = 12.976(5) , α = 108.220(8), β = 99.482(4), γ = 95.490(4)°, V = 1516.7(10) 3, Z = 2, Dc = 1.504 g/cm3, F(000) = 712, μ = 0.254, Mr = 686.64, the final R = 0.0561 and wR = 0.1487. One sulfonamido group of the title compound is deprotoned and forms N(3)=C(13). The crystal involves N,N-dimethylamine from the decomposition of DMF and the proton is transferred to N,N- dimethylamine. It is a strong proof for the characterization of deprotoned recognition compound by X-ray single-crystal structure.     

Crystal Structure of (R)-3,3′-Bis(benzyloxymethyl)-1,1′-bi-2,2′-naphthol and Its Applications in Enantioselective Lewis Acid Catalyzed Addition of Diethylzinc to Aldehydes

The title compound (R)-3,3′-bis(benzyloxymethyl)-1,1′-bi-2,2′-naphthol (R)-3 has been synthesized through the deprotection of MOM group by iPrOH/HCl in 83% isolated yield and the suitable single crystals for X-ray diffraction were obtained by recrystallization at room temperature from the mixture solvents. Crystallographic data for (R)-3: C36H30O4, Mr = 526.60, triclinic, space group P1, a = 10.057(6), b = 11.934(7), c = 12.314(6) , α = 85.52(2), β = 70.245(13), γ = 76.554(11)o, Z = 2, V = 1352.8(13)3, Dc = 1.293 g/cm3, F(000) = 556, R = 0.0745, wR = 0.1933 and μ(MoKα) = 0.083 mm-1. The title compound (R)-3 was found to be effective in the enantioselective addition of diethylzinc to aldehydes both in the presence and absence of Ti(OiPr)4. In the latter case, (R)-3 showed much higher catalytic activity and enantioselectivity than (R)-BINOL′s.     

Synthesis,Crystal Structure and Antitumor Activity of N-（4-tert-butyl-5-（4-chlorobenzyl）thiazol-2-yl）-2,6-difluorobenzamide

The title compound was synthesized by the reaction of 4-tert-butyl-5-(4-chlorobenzyl)-2-aminothiazole with 2,6-difluorobenzoic acid. The crystal structure of the title compound, C21H19ClF2N2OS, was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group Pbca with a = 12.6479(13), b = 13.1204(13), c = 14.1341(15), Z = 4, V = 2011.5(4)3, Mr = 420.89, Dc = 1.390 g/cm3, S = 1.023, μ = 0.326 mm-1, F(000) = 872, the final R = 0.0365 and wR = 0.0880 for 6101 observed reflections(I 2σ(I)), and R = 0.0507, wR = 0.0978 for 7779 independent reflections. X-ray crystal structure displays that the hydrogen bonding interactions observed link the molecules to form a dimeric unit. The preliminary biological test of the title compound shows good antitumor activity, with IC50 of 0.046 μmol/mL against the Hela cell line.     

Synthesis, Crystal and Molecular Structure and Biological Activity of Dimethyl Trans-3-（2- bromophenyl）-2-methylisoxazolidine-4,5-dicarboxylate

The compound of dimethyl trans-3-(2-bromophenyl)-2-methylisoxazolidine-4,5-dicarboxylate has been synthesized and characterized by IR, 1H-NMR, 13C-NMR, 2D-NMR (COSY, NOESY, HMQC, HMBC) and UV-vis. spectroscopy techniques and single-crystal X-ray diffraction (XRD). The biological activities of the title compound have been investigated in detail. The new compound crystallizes in monoclinic, space group C2/c with a = 26.9263(10), b = 7.0970(2), c = 19.8554(7) ?, and β = 126.630(2). In addition to the single crystal structure, the molecular geometry, vibrational frequencies, chemical shifts, molecular electrostatic potential and frontier molecular orbital analysis of the title compound in the ground state have been calculated by Density Functional Theory (DFT) method.     

Crystal Structure and Biological Activities of N-（5-（4-Chloro-2-（trifluoromethyl）phenyl）furan-2-carbonyl）-N＇-（4,6,dimethylpyrimidin-2-yl）thiourea

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.     

Synthesis, Crystal Structure and DNA Binding Studies of α,α'-Bis(3,5-bismethyl-1-pyrozolyl)- carbene-acetyl-isopropenyl Hydrazine

The title compound α,α'-bis(3,5-bismethyl-pyrozole-N-yl)-carbene-acetyl-isopro-penyl hydrazine (C16H22N6O, Mr = 314.40) has been prepared. It was characterized by elemental analysis as well as IR, MS, 1H-NMR and 13C-NMR spectra. Its crystal structure was determined by single-crystal X-ray diffraction, getting the following data: triclinic, space group P1 with a = 6.9734(16), b = 10.773(3), c = 12.001(3) A, α = 75.311(4), β = 82.695(4), γ = 77.143(4)°, Z = 2, V = 847.9(3) A3, Dc : 1.231 g/cm3, F(000) = 336 and μ(MoKα) = 0.082 mm-1 (λ = 0.71073 A). The results of crystal structure determination show that there exist intermolecular and intramolecular hydrogen bonds, resulting in a two-dimensional supramolecular framework of the title compound. The binding of the title compound to DNA was investigated by absorption, emission, and viscosity measurements. The title compound shows absorption hyperchromicity accompanied by a blue shift at about 254 nm. The binding constant Kb for the title compound has been determined to be 1.89 × 104 M-1 from absorption measurements. The addition of the title compound to DNA pretreated with EB causes appreciable reduction in the emission intensity, indicating that the DNA-bound EB fluorophore is partially replaced by the title compound. The value of K is 3.093 × 104 M-1. The relative viscosity of DNA decreased with the addition of the title compound. Results suggest that the title compound binds to DNA with a non-classical intercalative or groove interaction mode. The observed efficient nuclease activity of the title compound is interesting and may have further influences on the chemistry of DNA minor groove binders.     

Synthesis and Crystal Structure of 1-（N,N-Di-（p-toluenesulfonyl））-amino- 2-（N＇-p-toluenesulfonyl）-amino-3,5-dinitrobenzene

The title compound, 1-(N,N-di-(p-toluenesulfonyl))-amino-2-(N'-p-toluenesulfonyl)-amino-3,5-dinitrobenzene, was synthesized and structurally determined by single-crystal X-ray diffraction method. It crystallizes in orthorhombic, space group Pna21 with a = 13.723(2), b =25.354(4), c = 8.6565(12)(A), V= 3011.9(8)(A)3, Z= 4, Mr = 660.68, F(000) = 1368, Dc = 1.457 g/cm3,μ = 0.309, the final R = 0.0609 and wR = 0.1042. The H atom of N2-H group, which is the unique recognition site to anion, is enveloped by two oxygen atoms and one benzene from two and one p-toluenesulfonyl moieties, respectively.     

Synthesis and Crystal Structure of（2E,6E）-2,6-bis（2,3-dimethoxybenzylidene）cyclohexanone

The new title compound (2E,6E)-2,6-bis(2,3-dimethoxybenzylidene)cyclohexanone (C 24 H 26 O 5,M r=394.45) has been synthesized,and its crystal structure was studied.The title compound crystallizes in the orthorhombic system,space group Pca2 1 with a=17.536(2),b=14.8515(16),c=8.0512(9),V=2096.8(4) 3,Z=4,D c=1.250 g/cm 3,λ=0.71073,μ=0.087 mm-1 and F(000)=840.The structure was solved by direct methods and refined to R=0.0533 and wR=0.1248 from 2727 observed reflections (I > 2σ(Ⅰ)).The title molecules are connected through hydrogen bonds to generate a 3-D supramolecule.The preliminary biological tests showed definitely biological activity for the title compound.     

Synthesis and Crystal Structure of 2-[（2-Chloropyridin-4-yl）oxy]-3,3-diphenyl-3-methoxypropionic Acid

The title compound was synthesized and its crystal structure was determined by single-crystal X-ray diffraction.The crystal is of orthorhombic system(C21H18ClNO4,Mr = 383.81),space group Pca21 with a = 13.913(3),b = 10.273(2),c = 26.488(5),V = 3786.1(13) 3,Z = 8,Dc = 1.347 g/cm3,F(000) = 1600,μ = 0.228 mm-1,the final R = 0.0550 and wR = 0.1278 for 5065 observed reflections(I > 2σ(I)).The title compound in a racemic form was found to exist as a mixture of two enantiomers in an equal ratio in the unit cell.The intermolecular hydrogen bonds link the molecules in a head-to-end manner to generate an infinite chain.     

Synthesis, Crystal Structure and Fluorescene of a One-dimensional Compound {CdI2（2,2＇-bipy）}n

The title compound, {CdI2(2,2'-bipy)}n, was prepared by the hydrothermal reaction of CdI2 and 2,2'-bipy in an aqueous solution, and its crystal structure was determined by X-ray single-crystal analysis. Crystallographic data for 1: C10H8N2CdI2, monoclinic system, space group C2/c, a = 16.927(1), b = 10.0925(7), c = 7.7422(3) (A), β = 106.0629(4)°, V = 1271.00(14)(A)3, Z = 4, F(000) = 944, μ = 6.546 mm-1, Dc= 2.730 g/cm3, Mr = 522.38, the final R = 0.0309 and wR = 0.0805 for 1310 observed reflections (I＞2σ(Ⅰ)). X-ray crystal structure analysis shows that the Cd atom is coordinated by four iodines and two N atoms from one 2,2'-bipy to form an 1-D chain-like structure through bridging iodines. The fluorescene of the title compound was also discussed.     

Synthesis and Crystal Structure of Tert-butyl 4-[(E)-4-(1,3 -Dioxo-1,3-dihydro-2H-isoindol-2-yl)-1-butenyl] Benzoate

1 INTRODUCTION Phthalimide and its derivatives are synthetic mate- rials, which are widely used as important chemical intermediates of biosensors[1] and many drugs such as Citalopran[2], luminal[3], Beta-Lactam[4] and the No. three generation quinolones[5], and they have been identified as active groups of some drugs and chemical luminescence reagents[6, 7]. Tert-butyl 4- [(E)-4-(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)-1- butenyl] benzoate is an intermediate of a new type of insulin sen…     

Crystal Structure and Biological Activities of (R)-N''-[2-(4-Methoxy-6-chloro)-pyrimidinyl]-N-[3-methyl-2-(4-chlorophenyl)butyryl]-urea

The title compound (R)-N'-[2-(4-methoxy-6-chloro)-pyrimidyl]-N-[3-methyl-2-(4-chlorophenyl)butyryl]-urea has been synthesized, and its crystal structure and biological behaviors were studied. Crystallographic data: C17H18Cl2N4O3, Mr = 397.25, monoclinic, space group P21/c, a = 12.331 (2), b = 14.025(3), c = 23.085(5) (A), β = 99.607(4)°, Z = 8, V = 3936.2(13) (A)3, Dc = 1.341 g/cm3, F(000) = 1648, R = 0.0718, wR = 0.1585 and μ(MoKα) = 0.353 mm-1. The preliminary biological tests showed that the title compound has definite insecticidal and fungicidal activities.     

Synthesis and Crystal Structure of 2-(Diphenylphosphine oxide)-3-(diphenylphosphine oxide ethynyl) spiro [bicyclo[2.2.1]hepta-2,5-diene-7,1''''-cyclopropane]

1 INTRODUCTION Organic phosphine compounds always attract great interest for their unique properties and extensive uses in biochemistry, pesticide chemistry and synthetic organic chemistry. In the last two decades, much attention has been paid to phosphorus-containing olefin and acetylenic compounds for their applications in transition metal chemistry, asymmetric catalysis and photorearrang- ement [1~7 ]. Previously, we have reported the crystal structure of a novel host compound which …     

Synthesis and Crystal Structure of 5,5-Dimethyl-2-(4-chlorophenyl)(3-hydroxy-5,5-dimethyl-2-cyclohexen-1-one-2-yl)methyl-3-(4-methoxyphenylamino)-2-cyclohexene-1-one

The title compound 5,5-dimethyl-2-(4-chlorophenyl)(3-hydroxy-5,5-dimethyl-2-cyclohexen-1-one-2-yl)methyl-3-(4-methoxyphenylamino)-2-cyclohexen-1-one has been synthesized,and its crystal structure was characterized by X-ray single-crystal diffraction. The crystal belongs to monoclinic,space group P21/c with a=9.4193(13),b=26.915(4),c=21.188(3),β =101.906(3)°,V =5256.2(13)3,Z =4,C60H68Cl2N2O8,Mr=1016.06,Dc=1.284 g/cm3,F(000)=2160,λ(MoKα)=0.71073,μ=0.182 mm–1,R=0.0530 and wR=0.1131 for 4128 observed reflections (I>2σ(I)). X-ray analysis reveals that there are two independent molecules in the unit and the cyclohexenone rings adopt different conformations. In addition,there are four intramolecular hydrogen bonds in the title molecule.     

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 (9S,13R,14S)-7,8-Dehydro-4-(4'-bromobenzyloxy)-3,7-dimethoxy-17-methyl-morphinan-6-one Monohydrate

The title compound (9S,13R,14S)-7,8-dehydro-4-(4'-bromo-benzyloxy)-3,7-dime- thoxy-17-methyl-morphinan-6-one monohydrate (O-4-bromobenzylsinomenine) was synthesized by the reaction of (9S, 13R, 14S)-7,8-dehydro-4-hydroxy-3,7-dimethoxy- 17-methyl-morphinan-6-one with 4-bromobenzyl alcohol.Its chemical structure was determined by X-ray single-crystal diffraction.The crystal belongs to the monoclinic system, space group P2<,1> with a = 8.890(2), b = 14.757(4), c = 9.205(2) (A), β = 91.577(4)°, C<,26>H<,30>BrNO<,5>, M<,r> = 516.42,μ = 1.740 mm<'-1>, V = 1207.2(5) (A)<'3>, Z = 2, D<,c> = 1.421 mg/m<'3>, F(000) = 536, R = 0.0785 and wR = 0.1889.     

Cooperative C-H…O H-bonds in ''Bay Area'' and Crystal Structure of 1-(4-Methylphenyl)- 3-(4-methoxyphenyl)-2-propene-1-one

The title compound (C17H16O2, Mr = 252.30) crystallizes in the monoclinic system, space group P21/c with a = 11.5763(14), b = 11.0321(11), c = 11.5094(13) (A),β = 114.581(3)°, V= 1336.7(3) (A)3, Z = 4, Dc = 1.254 g/cm3, μ(MoKa) = 0.081 cm-1 and F(000) = 536.00. The final R and wR are 0.0527 and 0.1285, respectively for 3058 observed reflections (I ＞ 2σ(I)). In the title molecule, two phenyl rings are rotated oppositely with respect to the central part C(1)-C(2)=C(3)- C(4) (plane 3) and the dihedral angle between them is 14.8°. The phenone O(1) atom deviates from plane 3 by 0.291(A). In the crystal the molecules form H-bond chains of R21(6) and R21 (5) types similar crystals are also presented.     

Synthesis and Crystal Structure of the First Diaza-spirobifluorene：2-（Spirobifluorene-2-yl）-3,4-diaza-spirobifluorene

The title compound 2-(spirobifluorene-2-yl)-3,4-diaza-spirobifluorene(C48H28N2,Mr = 632.72) has been synthesized and characterized by 1H NMR,13C NMR and single-crystal X-ray diffraction.The crystal crystallizes in the monoclinic system,space group Cc with a = 13.8523(6),b = 29.3297(13),c = 8.6397(4) ,β = 111.8760(10)°,V = 3257.4(3) 3,Z = 4,Dc = 1.290 mg/m3,μ = 0.075 mm-1,F(000) = 1320,the final R = 0.0425 and wR = 0.1110 for 5288 observed reflections(Ⅰ 2σ(Ⅰ)).     

Synthesis, Crystal Structure, Antibacterial Activities and Theoretical Computation of 3-（2-Hydroxybenzly）-4-（4-isopropylbenzylideneamino）-（1H）-1,2,4-triazole-5-thione

1INTRODUCTION Recently,compounds containing pyrazole,imida-zole,triazole(including benzotriazole),pyridine,tetrazole and indole have attracted much interest because they exhibit some fungicidal activity,plant-growth regulating activity and antibacterial acti-vity[1～10].Schiff bases also constitute a good type of biologically active substructure[11～14],and the sulfur-containing Schiff bases are particularly effective.Studies of pyrazole Schiff base-type fungicides andtriazole compounds c…