Synthesis, Crystal Structure and Inhibition of N-2-Thiophenesulfonyl-a-L-phenylalanine Ethyl Ester on K562 Cell Proliferation

The title compound N-2-thiophenesulfonyl-a-L-phenylalanine ethyl ester has been synthesized. Complete assignments were achieved by IR, MS, ^1H NMR and single-crystal X-ray diffraction analyses. Using MTT assay, the inhibitory rate of the title compound on K562 cells （chronic myeloid leukemic cells） was measured and the result of preliminary bioassay showed that the title compound possesses antiproliferation effects on K562 cells. In order to investigate the relationship between structure and activity of the target compound, we report its crystal structure and biological behavior in the present paper. Crystallographic data： C15H17NO4S2, Mr = 339.42, monoclinic, space group P21, flack = -0.15（12）, a = 5.7916（10）, b = 11.5078（19）, c = 12.924（2） A, β = 97.781（3）°, Z = 2, V = 853.4（2） A^3, De = 1.321 g/cm^3, F（000） = 356, -7≤h≤7, -10≤k≤14, -15 ≤ l≤15, R = 0.0628, wR = 0.1540 and μ（MoKa） = 0.327 mm^-1. The molecule comprises a benzene and a thiofuran rings, and the intramolecular N（1）-H（1A）…O（1） makes a five-membered ring of O（1）--C（6）-C（5）--N（1）--H（1A）.     

Synthesis, Crystal Structure and Inhibition of N-2-Thiophenesulfonyl-α-L-phenylalanine Ethyl Ester on K562 Cell Proliferation

The title compound N-2-thiophenesulfonyl-α-L-phenylalanine ethyl ester has been synthesized. Complete assignments were achieved by IR, MS, 1H NMR and single-crystal X-ray diffraction analyses. Using MTT assay, the inhibitory rate of the title compound on K562 cells (chronic myeloid 1eukemic cells) was measured and the result of preliminary bioassay showed that the title compound possesses antiproliferation effects on K562 cells. In order to investigate the relationship between structure and activity of the target compound, we report its crystal structure and biological behavior in the present paper. Crystallographic data: C15H17NO4S2, Mr = 339.42, monoclinic, space group P21, flack = –0.15(12), a = 5.7916(10), b = 11.5078(19), c = 12.924(2) , β = 97.781(3)o, Z = 2, V = 853.4(2) 3, Dc = 1.321 g/cm3, F(000) = 356, –7≤h≤7, –10≤k≤14, –15≤l≤15, R = 0.0628, wR = 0.1540 and μ(MoKα) = 0.327 mm-1. The molecule comprises a benzene and a thiofuran rings, and the intramolecular N(1)–H(1A)…O(1) makes a five-membered ring of O(1)–C(6)–C(5)–N(1)–H(1A).     

Synthesis, Crystal Structure and Inhibition of the K562 Cell Proliferation of N＇-Tertbutylaminocarbonyl-N-2-chlorophenoxyacetylthiourea

The title compound N'-tert-butylaminocarbonyl-N-2-chlorophenoxyacetylthiou- rea has been synthesized for the first time. Complete assignments were achieved by IR, 1H NHR and single-crystal X-ray diffraction analyses. The inhibitory rate of the cellular growth of K562 cells (chronic myeloid 1eukemic cells) was measured using MTT [3-(4,5-dimethylthiazo-2-y1)-2,5-di- phenyltetra-zolium bromide] assay. The cell apoptosis was assessed by agarose gel electrophoresis to find that the title compound has antiproliferation and apoptosis inducing effects on K562 cells. In order to investigate the relationship between structure and activity of the target compound, we report its crystal structure and biological behavior in the present paper. Crystallographic data: C14H18- ClN3O3S, Mr = 343.82, orthorhombic, space group Pnma, a = 19.786(6), b = 6.789(2), c = 12.938(4) , V = 1738.0(9) 3, Z = 4, Dc = 1.314 g/cm3, F(000) = 720, μ(MoKα) = 0.354 mm-1, R = 0.0378 and wR = 0.0941. The molecule is a planar structure.     

Synthesis, Crystal Structure and Inhibition Corrosion Effect of Bis-（1,1＇-benzotriazoly）-a,w-decoyldiamide

The title compound bis-(1,1’-benzotriazoly)-α,ω-decoyldiamide was synthesized by the reaction of benzotriazole with sebacoyl dichloride, and its structure was characterized by IR, 1H NMR and single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P with a = 5.5290(11), b = 7.9410(16), c = 12.401(3), α = 72.19, β = 78.87(3), γ = 82.82(3)°, V = 507.36(20) 3, C22H24N6O2, Mr = 404.47, Dc = 1.324 g/cm3, Z = 1, μ = 0.089 mm-1, F(000) = 214, the final R = 0.0481 and wR = 0.1342 for 1347 observed reflections with I > 2σ(I). X-ray analysis revealed that the benzotriazole ring and carbonyl group were essentially planar. Potentiodynamic polarization study showed that inhibitor inhibited the anodic corrosion reactions, and it was an anodic type inhibitor.     

Synthesis and Crystal Structure of （E）-Ethyl 3-Keto-18β-glycyrrhetinate 3-Oxime

A novel derivative of glycyrrhetinic acid, (E)-ethyl 3-keto-18β-glycyrrhetinate 3- oxime C32H49NO4 (Mr = 511.72), was synthesized and structurally characterized by IR, 1H NMR and single-crystal X-ray diffraction. It belongs to monoclinic, space group P21, with a = 12.4897(12), b = 7.3190(7), c = 15.9944(14) , β = 94.833(2)o, V = 1456.9(2) 3, Z = 2, Dc = 1.167 g/cm3, μ = 0.075 mm-1, F(000) = 560, the final R = 0.0449 and wR = 0.1122. A total of 7486 reflections were collected, of which 2785 were independent (Rint = 0.0199) and 2605 were observed with I > 2σ(I). There exists an intermolecular hydrogen bond which helps to stabilize the crystal structure.     

Synthesis and Crystal Structure of 4,5-Bis（2-chloroethylthio）phthalonitrile

A novel phthalonitrile compound,[C12H10Cl2N2S2],has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction.The crystal belongs to the monoclinic system,space group P21/n with a = 10.6417(8),b = 7.5737(6),c = 18.2758(14),β = 105.2480(10)°,Mr = 317.24,V = 1421.12(19)3,Z = 4,Dc = 1.483 g/cm3,F(000) = 648,μ = 0.733 mm-1,R = 0.0173 and wR = 0.2183.In the structure,the C atoms of the aromatic ring,the two cyanide groups and the two S atoms are almost coplanar(maximum deviation from the mean plane = 0.049(7) ).Two potential weak intermolecular interactions of C-H…N and one type of π…π stacking interaction with a centroid-centroid separation of 3.751(8) stabilize the crystal structure.     

Synthesis and Crystal Structure of 2-Nitro-9,9-bis（methylpropionate）fluorine

The title compound of 2-nitro-9,9-bis(methylpropionate)fluorine (C21H21NO6 , Mr=383.39) was synthesized for the first time. Complete assignments were achieved by 1H NMR, IR, EI-MS, elemental analysis and single-crystal X-ray diffraction technique. The crystal belongs to monoclinic, space group P21/c with a=11.4581(15), b=10.3624(14), c=16.573(2) , β=96.629(2) o , V=1954.6(5) 3 , Z=4, Dc=1.303 g/cm 3 , μ=0.096 mm -1 , F(000) = 808, R =0.0493 and wR=0.1499 for 3107 observed reflections with I > 2σ(I). X-ray analysis reveals that three fused rings of the fluorene system are almost coplanar and the two ester groups are nearly perpendicular to the fused-ring system. Weak C-H O hydrogen bonding connects the molecules into centrosymmetric dimmers.     

Synthesis and Crystal Structure of 1,2-Dis（1,3-diphenylpropan-2-yl）disulfane

A novel compound of 1,2-dis(1,3-diphenylpropan-2-yl)disulfane(C30H30S2,Mr=454.27)was synthesized in ethanol with 1,3-diphenyl-2-propanone as raw materials,giving high yield of product(90%).Its structure was determined by IR,1H NMR,MS,elemental analysis and X-ray diffraction.The crystal belongs to monoclinic,space group C2 with a=18.727(3),b=6.5179(9),c=13.7576(18),β=131.0610(10)o,V=1266.2(3)3,Z=2,Dc=2.136 g/cm3,μ=1.078 mm-1,F(000)=843,R=0.0490 and wR=0.1247 for 3211 observed reflections with I>2(I).X-ray analysis reveals that the molecule is not symmetrical.There exist no classical hydrogen bonds andπ-πstacking interactions.Moreover,the thermal stability of compound 3 was investigated.     

Synthesis,Crystal Structure,and Photoluminescence Properties of One Novel D-π-D Type α-Cyanostilbene Derivative

Researches on α-cyanostilbene derivatives demonstrated them to be promising AIE or AIEE structural molecules and potential photoelectric materials. One novel α-cyanostilbene derivative, namely(E)-2-(4-butoxyphenyl)-3-(4-(diethylamino)phenyl)acrylonitrile(BPDPA), has been designed, synthesized and characterized. The crystalline structure of BPDPA has been studied in detail. The single-crystal X-ray diffraction revealed BPDPA crystallizes in triclinic space group P1, with a = 12.860(5), b = 13.327(5), c = 15.016(5) , α= 72.650(5), β = 66.969(5),γ = 62.897(5), Mr = 696.95, V = 2085.6(13) 3, Z = 2, Dc = 1.110 g/cm-3, μ = 0.068 mm-1, F(000) = 752, Rint = 0.0264, R(I 2σ(I)) = 0.0649, wR(I 2σ(I) = 0.1724, R(all data) = 0.1321, wR(all data) = 0.2158, completeness to theta = 25.00 is 99.4% and GOF = 1.067. Like most reported α-cyanostilbene derivatives, BPDPA possesses a somewhat twisted molecular structure. UV-Vis and FL measurements showed an obviously bathochromic effect of BPDPA with increasing the polarity of the solvents.     

Neutron Diffraction Study on Structure of α－LiIO_3 Single Crystal under DC Voltage

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Synthesis and Crystal Structure of O,O-Dimethyl-N-(β-triphenylgermanyl)propionyl-α- aminobenzylphosphonates

1 INTRODUCTION Both β-triphenylgermanyl propionic acid and its derivatives have recently attracted a great deal of attention due to their strong anti-inflammatory as well as antibiotic properties[1~3]. α-aminobenzyl- phosphonates are also reported to exhibit diverse biological activities[4~6].It is conceivable that the incorporation of the two moieties into one structural unit might produce an unexpected effect on the activity of such a compound, and the studies on this type of novel s…     

Synthesis, Crystal Structure and Electrochemical Property of 5,10,15,20-Tetrakis（4-chlorophenyl）porphyrin

The title compound 5,10,15,20-tetrakis(4-chlorophenyl)porphyrin was synthesized and structurally characterized by X-ray single-crystal diffraction method. Crystal data: triclinic, space group P, Z=1, C50H32Cl4N4, Mr=830.60, a=6.4316(13), b=11.322(2), c=13.833(3) , α =91.44(3), β=91.06(2), γ=92.67(3)°, V=1005.7(3)3 , Dc=1.371 g/cm3 , μ(MoKα)=0.34 mm-1 , F(000)=428, R=0.0563 and wR=0.0867 for 2712 observed reflections with I > 2σ(I). X-ray analysis reveals the phenyl rings and the pyrrole rings are not in the same plane. The dihedral angles between adjacent phenyl rings and pyrrole rings are 66.1 and 66.8°, respectively.     

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,Bioactivity and Crystal Structure Analysis of N-（2-ethoxyphenyl）-3-oxobenzo[d]isothiazole-2（3H）-carboxamide

The title compound N-(2-ethoxyphenyl)-3-oxobenzo[d]isothiazole-2(3H)-carboxa-mide(C16H14N2O3S,Mr = 314.35) has been synthesized and structurally characterized by IR,1H NMR and single-crystal X-ray diffraction.The crystal belongs to triclinic,space group P with a = 4.6395(15),b = 8.689(3),c = 17.917(7),α = 87.763(9),β = 84.625(9),γ = 82.344(9)°,V = 712.4(4)3,Z = 2,Dc = 1.465 Mg·m-3,λ(MoKa) = 0.71073,F(000) = 328,μ(MoKa) = 0.242 mm-1,the final R = 0.038 and wR = 0.089.A total of 3702 unique reflections were collected,of which 2762 with I > 2σ(I) were observed.X-ray analysis revealed that the benzisothiazolone ring and benzene moieties were essentially planar,and three intramolecular hydrogen bonds N(2)-H(2N)…O(1),N(2)-H(2N)…O(3) and C(10)-H(10)…O(2) were observed.The preliminary biologi-cal test showed that the title compound had antifungal and antibacteria activities against Bacillus subtilis(CMCC63003),Aeromonas hydrophila(ATCC7966),Staphylococcus aureus(ATCC6538),Escherichia coli(JM103),Blastomyces albicans,Gloeosporium papaya P.Henn,Colletotrichum gloeosporioides Penz and Botryodiplodia theobromae.     

Synthesis and Crystal Structure of 3-（4-Bromobenzyloxy）-6-morpholinopyridazine

The title compound 3-(4-bromobenzyloxy)-6-morpholinopyridazine(C15H16BrN3O2) was synthesized,and its crystal structure was studied.It crystallizes in the triclinic system,space group P with a = 8.3408(17),b = 8.8620(18),c = 10.832(2) ,α = 108.09(3),β = 91.28(3),γ = 100.90(3)°,Dc = 1.562 g/cm3,Z = 2,λ = 0.71073 ,μ(MoKα) = 2.769 mm-1,Mr = 350.22,V = 744.5(3) 3,F(000) = 356,the final R = 0.0522 and wR = 0.1366 for 2016 observed reflections with I > 2σ(I).In the crystal structure,the morpholine ring adopts a chair conformation with O(2) and N(3) atoms at the flap positions-0.656(7) and 0.622(6)  out of the mean plane formed by the other four C atoms,respectively.These molecules generate centro-symmetric dimers through intermolecular π-π interaction.     

Synthesis and Crystal Structure of a Novel Fe(Ⅲ) Schiff Base Complex

A novel Fe(Ⅲ) Schiff base complex,FeⅢ(HL) {H4L = 1,1,1,1-tetrakis[(salicylaldimino)methyl]methane},has been prepared and characterized by elemental analyses,IR spectrum,and single-crystal X-ray diffraction analysis.The crystal belongs to the monoclinic system,space group P21/n with a = 12.569(3),b = 12.955(3),c = 17.647(4) ,β = 91.896(9)°,V = 2871.9(1) 3,Z = 4,Dc = 1.391 g/cm3,F(000) = 1252.0,Mr = 601.45,R = 0.0383 and wR = 0.1025.The structural analysis reveals that the Fe(Ⅲ) ions are six-coordinated by imine nitrogen atoms and phenolic oxygen atoms form three pendant arms of Schiff base ligands,and one of the salicylaldimine chelating units remains uncoordinated.Discrete complex molecules were further assembled into 1D supramolecular aggregations by C-H…O hydrogen bonding and C-H…π interactions.     

Hydrothermal Synthesis and Crystal Structure of a One-dimensional Cadmium（Ⅱ） Complex

A metal-organic coordination polymer [Cd2(cbba)4(bix)2] n·nH2O (Hcbba=2-(4′-chlorine-benzoyl)-benzoic acid, bix=1,4-bis(imidazol-1-ylmethyl)-benzene) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. Colorless crystals crystallize in the triclinic system, space group Pī with a=12.9891(15), b=15.3211(19), c=21.154(3), α=108.476(3), β=90.148(2), γ=105.429(3)°, V=3831.5(8)3 , C84H60Cd2Cl4N8O13 , Mr=1756.00, Dc=1.522g/cm3 , F(000)=1776, Z=2, μ(MoKα)=0.765 mm-1 , the final R=0.0724 and wR=0.1208 for 6916 observed reflections (I > 2σ(I)). The structure of 1 exhibits a one-dimensional infinite chain-like structure.     

Synthesis and Crystal Structure Analysis of 5′-O-Tosyl-2,3′-anhydrothymidine

In this paper=5′-O-tosyl-2,3′-anhydrothymidine has been synthesized and its crystal structure was analyzed. The crystal belongs to the triclinic system=space group P1=with a=5.397(2)=b=6.1886(18)=c=3.507(5) =α =87.74(2)=β =89.84(4)=γ =73.79(2)°=C17H18N2O6S=Mr=378.39=Z=1=V=432.8(3)3=Dc=1.452 g/cm3=F(000)=198 and Flack =-0.11(14). No intermolecular hydrogen bonds exist in the crystal=and the angle between benzene ring and pyrimidine planes is 32.23°.     

Synthesis and Crystal Structure of N-（（6-chloropyridin-3-yl）methyl）-6-ethoxy-N-ethyl-3-nitropyridin-2-amine

The title compound N-((6-chloropyridin-3-yl)methyl)-6-ethoxy-N-ethyl-3-nitropyri-din-2-amine(4) was synthesized by reacting the mixture of 6-chloro-2-ethoxy-3-nitropyridine(1) and 2-chloro-6-ethoxy-3-nitropyridine(2) with 3,and its structure was determined by X-ray single-crystal diffraction.The crystal belongs to the monoclinic system,space group P21/n with a = 7.3441(2),b = 9.9041(3),c = 11.7368(3) ,α = 101.410(2),β = 102.1340(10),γ = 99.594(2)o,μ = 0.260 mm-1,Mr = 336.78,V = 798.58(4)3,Z = 2,Dc = 1.401g/cm3,F(000) = 352,T = 296(2) K,R = 0.0210 and wR = 0.1053.     

Synthesis, Crystal Structure and Properties of a Novel Tetranuclear Nickel（II） Complex with Azo-enolic-2-hydroxybenzamide

A novel tetranuclear nickel(Ⅱ) complex [Ni4L2(DMF)2(H2O)2·2DMF] (1,H4L=azo-enolic-2-hydroxybenzamide, DMF=N,N-dimethyl-formamide) has been synthesized and characterized by elemental analysis, UV, IR and X-ray single-crystal diffraction characterization. Complex 1 crystallizes in the monoclinic system, space group P21/n with a=8.8944(11), b=14.4583(18), c=18.097(2) , β=90.00(2)o, Z=2 , V=2327.2(5)3 , C40H48N12Ni4O14 , Mr=1155.66, Dc=1.649g/cm 3 , μ=1.672 mm-1 , F(000)=1192, R=0.0392 and wR=0.0958. The local coordination environment around the nickel ions exist a distorted octahedral and quadrangle geometry in the molecular structure. Complex 1 exhibits strong photoluminescent emission in the ultraviolet region at room temperature. The electrochemical studies reveal that redox of Ni 3+ /Ni 2+ in the complex is a quasi-reversible process.