Synthesis,Crystal Structure and Anti-integrase Activity of 25,27-Bis[(Z)-4-(p-methoxyphenyl)-4-hydroxybut-3-en-2-one-1-methyl]-26,28-dihydroxycalix [4] arene

The title compound(C50H44O10) was synthesized and structurally determined by single-crystal X-ray diffraction method. It crystallizes in monoclinic, space group P21/c with a = 16.713(4), b = 13.189(3), c = 19.434(5) , β = 104.411(4)°, Mr = 804.85, Dc = 1.288 g/cm3, V = 4149.2(17) 3, Z = 4, F(000) = 1696, μ(MoKa) = 0.089 mm-1, T = 296(2) K, 7279 independent reflections with 3172 observed ones(I 2σ(I)), R = 0.0520 and wR = 0.1203 with GOF = 0.928(R = 0.1464 and wR = 0.1657 for all data). The calixarene moiety maintains the symmetric cone conformation through intramolecular O–H···O hydrogen bonds. Preliminary bioassays indicated that the title compound has a potent inhibitory activity against the strand transfer process of HIV-1 integrase.     

Isolation, Crystal Structure and Inhibitory Activity against Magnaporthe Grisea of （2R,3R）-3,5,7-trihydroxyflavanone 3-Acetate from Myoporum Bontioides A. Gray

The title compound, (2R,3R)-3,5,7-trihydroxyflavanone 3-acetate, is a flavanonol derivative which was first isolated from Myoporum bontioides A. Gray and characterized by MS, NMR and CD spectra. In addition, the structure was determined by X-ray single-crystal diffraction analysis. It crystallizes in the triclinic lattice, space group P21 with a = 10.686(3), b = 6.862(2), c = 11.267(3) , β = 107.46(1), V = 788.3(4) 3, Z = 2, C17H16O7, Mr = 332.30, Dc = 1.400 g/cm3, μ(MoKα) = 0.110 mm-1, F(000) = 348, the final R = 0.0283 and wR = 0.0826 for 3428 independent reflections (Rint = 0.017) and 1500 observed ones (I > 2σ(I)). The structure consists of one flavone and one water molecule. The flavone molecules form a 1D column by the p…π stacking interactions and C–H…O hydrogen bonds. The weak intermolecular/intermolecular O–H…O hydrogen bonds observed in the crystal give further rise to a complicated network structure. Primary bioassay showed that the title compound has high inhibitory activity against Magnaporthe grisea with the EC50 values of 199.41 μg/mL.     

Synthesis,Characterization and Antitumor Activity in Vitro of Cd（Ⅲ）Complex with Chelidamic Acid

A novel complex [Cd4(HCAM)4(H2O)8] of Cd(Ⅲ) withchelidamic acid (H3CAM) was synthesized by the hydrothermal method and characterized with IR and emission spectra.The crystal structure was determined based on single-crystal X-ray diffraction data.It crystallizes in monoclinic,space group C2/c with a=17.538(5),b=12.916(4),c=16.505(7),β=100.690(14)o,V=3674(2) 3,Z=8,C14 H14 Cd2N2O14,Mr=659.07,Dc=2.383 g/cm 3,μ=2.400 mm-1,S=1.000,F(000)=2560,the final R=0.0242 and wR=0.0581 for 3656 observed reflections with I>2σ(I).The inhibition of the complex against K562 and HL60 cells was determined by MTT assay.The results showed that the concentration of complex was positively correlated with inhibitions against K562 and HL60 cell lines,but inhibitory effects are relatively weak.IC 50 concentration of the title complex on K562 and HL60 cells is 15 and 5 μg/mL,respectively.     

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.     

Hydrothermal Synthesis and Crystal Structure of a Copper Complex

The title compound [Cu(IB)2]n·n(H2O) 1 was synthesized via the hydrothermal reaction of CuSO4·5H2O and NaOH with 4-(1H-Imidazol-1-yl)benzoic acid(HIB),and character-rized by elemental analysis and infrared spectra.The crystal of 1 crystallizes in monoclinic,space group C2/c with a = 14.349(7),b = 5.977(3),c = 21.368(9) ,β = 104.956(9)o,V = 1770.5(2)3,Z = 4,C20H16CuN4O5,Mr = 455.92,Dc = 1.710 g/cm3,F(000) = 932 and μ(MoKα) = 1.279 mm-1.The final R = 0.0337 and wR = 0.0888 for 1972 observed reflections with Ⅰ 2σ(Ⅰ) and R = 0.0369 and wR = 0.0926 for all data.X-ray diffraction reveals that the IB ligand links the Cu(Ⅱ) atoms into a double stranded chain.The extensive supramolecular interactions lead to the formation of an infinite 2D structure.     

A Zn(Ⅱ) 5-Aminoisophthalate Coordination Polymer

The title compound, [Zn(AIP)(4,4-bipy)0.5(H2O)]n·0.75nH2O 1, was synthesized via the hydrothermal reaction of Zn(OAc)2 with 5-aminoisophthalic acid (H2AIP) and characterized by elemental analysis and infrared spectra. The complex crystallizes in monoclinic system, space group P21/c with a = 12.672(1), b = 7.6557(4), c = 16.181(1) (A),β = 109.187(2)o, V = 1482.6(2) (A)3, Z = 1, C52H52N8O23Zn4, Mr = 1418.58, Dc = 1.589 g/cm3, F(000) = 724 and μ(MoKα) = 1.685mm-1. The final R = 0.0702 and wR = 0.1524 for 1847 observed reflections with Ⅰ ＞ 2σ(I), and R = 0.0873 and wR = 0.1664 for all data. X-ray diffraction studies reveal that the title compound has an interesting 2D microporous architecture with guest water molecules inside the channel.     

Synthesis and Crystal Structure of Salicylyl-4-phenyl Thiosemicarbazide Lead with a Two-dimensional Network

A two-dimensional lead complex, [Pb(C14N3O2H12S)(NO3)]n·nH2O, was prepared by the reaction of salicylyl-4-phenyl thiosemicarbazide and lead nitrate. The compound (C14H13N4O6PbS, Mr=572.53) crystallizes in the monoclinic space group P21/c with a=11.2984(2), b=15.6628(7), c=11.1118(2), β= 113.564(2)n, V=1802.43(10)3, Dc=2.110 g/cm3, Z=4, μ(MoKα)= 9.515 mm·1, F(000)=1084, the final R=0.0394 and wR=0.0701 for 2552 observed reflections with I > 2σ(I). The Pb(II) ion displays a distorted octahedron in which the hypothesized stereochemically active lone pair occupies the apex. The compound exhibits a two-dimensional network structure formed by the zigzag one-dimensional chains joined by two μ-O of two nitrate groups in overlapping. A large ring exists in the two-dimensional layers. The TGA of the title compound has been studied.     

Synthesis and Crystal Structure of a New Complex [Cu（C_（14）H_9O_3）_2（C_5H_5N）_2（C_2H_5OH）_2]

The title compound of Cu(C14H9O3)2(C5H5N)2(C2H5OH)2(1) was synthesized via the hy- drothermal reaction of CuCl2·2H2O and 9-hydroxy-fluorene-9-carboxylic acid(HHF) with pyridine, and characterized by elemental analysis and infrared spectra. The crystal belongs to triclinic, space group P1 with a = 8.8302(12), b = 10.1625(14), c = 12.2708(17), α = 86.207(2), β = 69.562(2), γ = 64.932(2)o, V = 930.3(2) 3, Z = 1, Mr = 764.30, Dc = 1.364 g/cm3, F(000) = 399, S = 1.059 and μ(MoKα) = 0.644 mm-1. The final R = 0.0459 and wR = 0.1274 for 3414 observed reflections with I 2σ(I). The copper atom is six-coordinated by two oxygen atoms from two different 9-hydroxy-fluorene-9-carboxylate ligands, two pyridine nitrogen atoms and two ethanol oxygen atoms, forming a distorted octahedral coordination geometry. The extensive O–H···O hydrogen bonding connects the molecules to form a one-dimensional chain structure. Between adjacent one-dimensional chains, a two-dimensional layered structure was formed by fluorene ring π-π packing interaction. Between the layers, a three-dimensional structure was formed through the π-π packing interaction of the pyridine ring. Moreover, the thermal stability and photoluminescent property of the complex has been investigated.     

A Zn(II) 5-Aminoisophthalate Coordination Polymer

The title compound, [Zn(AIP)(4,4-bipy)0.5(H2O)]n·0.75nH2O 1, was synthesized via the hydrothermal reaction of Zn(OAc)2 with 5-aminoisophthalic acid (H2AIP) and characterized by elemental analysis and infrared spectra. The complex crystallizes in monoclinic system, space group P21/c with a = 12.672(1), b = 7.6557(4), c = 16.181(1) , β = 109.187(2)o, V = 1482.6(2) 3, Z = 1, C52H52N8O23Zn4, Mr = 1418.58, Dc = 1.589 g/cm3, F(000) = 724 and μ(MoKα) = 1.685mm-1. The final R = 0.0702 and wR = 0.1524 for 1847 observed reflections with I > 2σ(I), and R = 0.0873 and wR = 0.1664 for all data. X-ray diffraction studies reveal that the title compound has an interesting 2D microporous architecture with guest water molecules inside the channel.     

Synthesis and Crystal Structure of N-((3-(2-nitrophenyl) propanoyl)oxy)-N-phenylbenzamide

The title compound N-((3-(2-nitrophenyl) propanoyl)oxy)-N-phenylbenzamide(C22H18N2O5,Mr = 390.38) was synthesized with nitrobenzene as the starting materials and structurally characterized by 1H NMR,13 C NMR,IR,H RMS(E-SI) and single-crystal X-ray diffraction.The crystalline structure of the title compound was studied in detail.The single-crystal X-ray diffraction revealed that the compound crystallizes in monoclinic,space group P21/n,with a = 14.4481(7),b = 8.0089(5),c = 16.6808(9) ?,α = 90.00(5),β = 100.069(5),γ = 90.00(5)°,Mr = 390.38,V = 1900.46(18) ?3,Z = 4,Dc = 1.364 g/cm-3,μ = 0.098,F(000) = 816.0,the final R = 0.0530 and w R = 0.1141 for 2525 observed reflections(I 2σ(I)),R(all data) = 0.0813,w R(all data) = 0.1335,completeness to theta of 26.020 is 99.8% and GOF = 1.085.The crystal structure contains three branched chains with its center placed at the midpoint of N.The phenyl ring(C(8)~C(13)) makes a dihedral angle of 83.5(1) ℃ with the phenyl ring(C(1)~C(6)),and 80.5(1) ℃with the nitro-substituted benzene ring(C(17)~C(22)),indicating that the three rings are not coplanar.Hydrogen bonds(C(10)–H(10)···O(3)),(C(15)–H(15B)···O(4) and C(16)–H(16B)···O(4)) together with π-π stacking interactions stabilize the structure of the molecule.The preliminary biological test shows that the title compound has good antitumor activity against A549 in vitro with the IC50 value of 3.17 μmol.     

Synthesis,Crystal Structure and Herbicidal Activity of Methyl(E)-α-(Methoxyimino)-2-((4-(3-chloro-5-(trifluoromethyl)-pyridine-2-yl)phenoxy)methyl)benzeneacetate

The title compound methyl(E)-α-(methoxyimino)-2-((4-(3-chloro-5-(trifluoromethyl) pyridine-2-yl)phenoxy)methyl)benzeneacetate(C23 H18 ClF3 N2 O4) has been synthesized and structurally characterized by 1 H and 13 C NMR, and HRMS. Its absolute molecular configuration was investigated by X-ray crystallography. The crystal crystallizes in monoclinic system, space group P21/c with a = 15.0928(7), b = 19.6070(10), c = 7.5535(5) ?, β = 98.176(5)°, V = 2212.6(2) ?3, Z =4, Dc = 1.438 g/cm3, F(000) = 984, μ(Mo Kα) = 0.231 mm-1, the final R = 0.0619 and wR = 0.1681 with 4034 observed reflections with I 2σ(I). The title compound has significant inhibitory rate against broadleaf weeds. They are all 100% under the dose of 37.5 g.a.i/ha, which was better than mesotrione.     

Crystal Structure and Anticancer Properties of Cinobufagin 3-Hemisuberate Methyl Ester

The title compound cinobufagin 3-hemisuberate methyl ester(1) was isolated from the venom of Bufo bufo gargarizans CANTOR. The crystal structure of 1, C35H48O9, was determined by single-crystal X-ray diffraction analysis. It belongs to orthorhombic, space group P212121 with a = 8.9338(3), b = 16.2970(4), c = 22.4019(6) , V = 3261.59(16) 3, Mr = 612.73, Z = 4, Dc = 1.248 g/cm3, μ = 0.725 mm-1, F(000) = 1320, S = 1.040, the final R = 0.0374 and wR = 0.0412 for 4458 unique reflections, of which 4088 were observed(I 2σ(I)). In the solid state, short intermolecular C-H...O interactions involving a methine and the ester carbonyl group in cinobufagin moiety and a methyl in the suberate moiety linked adjacent molecules into a three-dimensional network. Detailed analysis of the 1H-NMR data showed that X-ray structure of 1 would be expected to closely resemble the solution conformation in chloroform. Compound 1 was inactive for the inhibition of PC3 and HepG2 cancer cells, but the parent compound cinobufagin showed potent inhibition with IC50 values of 0.145 and 5.48 μM, respectively, indicating that esterification at C(3) decreased the cytotoxic effect of 1.     

Synthesis,Crystal Structure and Antitumor Activities of N-(2-(1H-indol-3-yl)ethyl)-2-nitroaniline

The title compound, N-(2-(1H-indol-3-yl)ethyl)-2-nitroaniline(C16H15N3O2, Mr = 281.31), has been synthesized by the multicomponent reaction of milder Ullmann, and its structure was characterized by 1H NMR, 13 C NMR, IR, H RMS(ESI) and single-crystal X-ray diffraction. It crystallizes in monoclinic, space group I2/c with a = 15.0212(10), b = 9.4911(6), c = 20.3075(13) A, β = 100.776(7)o, V = 2844.1(3)A3, Z = 8, Dc = 1.314 g/cm3, F(000) = 1184.0, μ = 0.089 mm-1, the final R = 0.0574 and w R = 0.1688 for 1701 observed reflections(I 2σ(I)). X-ray analysis indicates three major N(2)–H(2)···O(2), C(13)–H(13)···O(2), N(2)–H(2)···N(3) hydrogen bonds and π-π stacking interactions in the crystal structure. The preliminary biological test shows that the title compound has a good antitumor activity against A549 in vitro with the IC50 value of 35 μmol/L.     

Synthesis and Crystal Structure of 1-Ethyl 3-Methyl 6-Benzyl-2-methyl-5-oxo-5,6-dihydropyrrolo[1,2-c]quinazoline-1,3-dicarboxylate

The crystal structure of the title compound(C24H22N2O5, Mr = 418.44) has been determined by single-crystal X-ray diffraction. The crystal is of orthorhombic, space group P21/c with a = 7.751(2), b = 12.392(4), c = 21.326(6), V = 2048.4(1)3, Z = 4, Dc = 1.357 g/cm3, F(000) = 880, μ(MoKα) = 0.096 mm-1, the final R = 0.0731 and wR = 0.1982 for 3335 observed reflections(I 2σ(I)). Intermolecular C(24)–H(24B)···O(1) hydrogen bond is observed in the structure.     

Synthesis,Crystal Structure and Bioactivity of N-（phenethylcarbamothioyl）cyclopent-1-enecarboxamide

The compound N-(phenethylcarbamothioyl)cyclopent-1-enecarboxamide was synthesized by the reaction of cyclopent-1-enecarbonyl isothiocyanate with phenethylamine in acetone, and its structure was characterized by IR, 1H NMR and X-ray crystal structure determination. The crystal of the title compound belongs to triclinic, space group P1 with a = 6.9500(7), b = 9.4618(9), c = 11.3256(11), α = 71.522(9), β = 81.830(8), γ = 89.237(8)o, Z = 2, V = 698.80(12)3, Dc = 1.304 g/cm3, μ = 0.225 mm-1, F(000) = 292, R = 0.0413 and wR = 0.1073 for 1996 observed reflections with I 2σ(I). Intramolecular N(2)–H(2)···O(1) interactions as well as intermolecular N(2)–H(2)···O(1), N(1)–H(1)···S(1) and C(12)–H(12)···S(1) hydrogen bonds help to stabilize the crystal structure. X-ray diffraction analysis reveals that the structure of the new compound exhibits a one-dimensional infinite chain-like structure. The cytotoxicity of the compound was investigated by MTT assay. The results show that the compound is toxic to A549 tumor cell.     

Synthesis and Crystal Structure of 4-Arylamino-6-chloropyrido[3,2-d]pyrimidine

The title compounds 4a～c were synthesized and characterized by IR,NMR and MS.The crystal structure of C16H13ClN4O2·HBr·H2O(I),the quaternary ammonium salt of 4c,was determined by X-ray diffraction analysis.I crystallizes in triclinic,space group P1 with a = 8.3121(8),b = 9.3885(8),c = 13.2903(12),α = 106.788(2),β = 95.204(3),γ = 110.871(2)o,V = 905.81(14)3,Z = 2,C16H16BrClN4O3,Mr = 427.68,Dc = 1.568 g/cm3,F(000) = 432.00,μ = 2.446 mm-1,R = 0.0496 and wR = 0.127.X-ray analysis reveals that C(15) in the BrCH2COOH molecule binds to the N(1) of pyrimidine ring to form the quaternary ammonium salt.Two adjacent I molecules are connected by hydrogen bonds through carboxylate oxygen,water molecule and hydrobromic acid.     

Synthesis,Structure and Norbornene Polymerization Catalyzed by Bis{(2-benzhydryl-4,6-dimethyl-phenyl)-(3,5-di-tert-butyl-2-methyl-benzylidene)-amine-N,O}nickel(Ⅱ)

The title complex bis{(2-benzhydryl-4,6-dimethyl-phenyl)-(3,5-di-tert-butyl-2-methyl-benzylidene)-amine-N,O}nickel has been synthesized by the reaction of(2-benzhydryl-4,6-dimethyl-phenyl)-(3,5-di-tert-butyl-2-methyl-benzylidene)-amine with Ni(CH_3COO)_2·4H_2O, and characterized by IR spectrum and single-crystal X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P2_1/c with a = 12.373(4), b = 18.434(7), c = 27.814(10) ?, β = 92.291(6)o, V = 6339(4) ?~3, C7 2H8 0N2 Ni O_2, M_r = 1064.09, Z = 4, D_c = 1.115 g/cm~3, μ = 0.350 mm~(-1), F(000) = 2280, the final R = 0.0846 and wR = 0.2926(I 2s(I)). This title compound was used as homogeneous catalysis of polymerization of norbornene, and the complex exhibited good catalytic activity to catalyze norbornene polymerization using MAO as a cocatalyst.     

6,8-Di-tert-butyl-3-（2,4-dimethyl-quinolin-7-yl）-3,4-dihydro-2H-benzo[e][1,3]oxazine： Synthesis,Crystal Structure and Luminescent Properties

6,8-Di-tert-butyl-3-(2,4-dimethyl-quinolin-7-yl)-3,4-dihydro-2H-benzo[e][1,3]oxa- zine(1) was obtained by one-pot reaction starting from 2,4-di-tert-butylphenol, 7-amino-2,4- dimethyl-quinoline and paraformaldehyde. The compound was structurally characterized by NMR, IR and single-crystal X-ray diffraction along with the elemental analysis. Compound 1 crystallizes as solvate with chloroform. The solvate 1·CHCl3(C28 H35 Cl3 N2 O, Mr = 521.93) belongs to the triclinic system, space group P1 with a = 10.852(2), b = 11.352(2), c = 13.050(3), α = 101.95(3), β = 92.94(3), γ = 114.64(3)o, V = 1412.4(5)3, Z = 2, Dc = 1.227 g/cm3, F(000) = 552, μ = 0.347 mm–1, R = 0.0959 and wR = 0.2725(I 2?(I)). The chloroform molecule displays a rotational disorder as one chloro atom can be located at two different positions. The packing of 1·CHCl3 was further stabilized by intramolecular C–H···O interactions, intermolecular C–H···N interactions, C–H···π interactions, and π···π interactions. The luminescent properties of compound 1 in both methylene chloride solution and the solid state were studied.     

Synthesis and Crystal Structure of（3S,4R,Z）-3,6-dimethyl-2-（3-methylbut-2-enylidene）-2,3,3a,4,7,7a-hexahydrobenzofuran-3,4-diol

The title compound of(3S,4R,Z)-3,6-dimethyl-2-(3-methylbut-2-enylidene)-2,3,3a,4,7,7a-hexahydrobenzofuran-3,4-diol,C15H22O3,as a potential gastric cytoprotective agent has been synthesized by the reduction of bisabolangelone in methanol with sodium borohydride.The title compound was characterized by IR and NMR spectra.Meanwhile,the crystal was obtained and determined by X-ray single-crystal diffraction.Crystal data:monoclinic system,space group P21 with a = 6.0692(12),b = 8.9954(18),c = 13.182(3) ,β = 92.59(3)°,V = 718.9(2) 3,Z = 2,F(000) = 272,Dc = 1.156 g/cm3,μ = 0.633 mm-1,R = 0.0362 and wR = 0.1051 for 9490 independent reflections(Rint = 0.0172) and 2461 observed reflections(I > 2σ(I)).Intermolecular O-H…O interactions link the molecules into one-dimensional infinite chains running along the b axis,which contributes to the stability of the crystal structure.     

Crystal Structure and Antitumor Activity of Tri[2-[N-（4′-methyl-benzylsulfonyl）amino]ethyl]-amine

The crystal structure of the title compound (C27H38N4O7S3, Mr = 626.79) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group Pīwith a = 9.411(1), b = 11.645(2), c = 14.672(2) (A。), α = 91.80(1), β = 95.36(1), γ =104.56(1)o, V = 1547.0 (A。)3, Z = 2, Dc = 1.346 g/cm3, λ = 0.71073 (A。), μ(MoKα) = 0.289 mm－1 and F(000) = 664. The structure was refined to R = 0.0406 and wR = 0.1177 for 4103 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the title compound is a practically distorted tetrahedron and each molecule contains one lattice H2O by hydrogen bond. The antitumor activity of the title compound against HL-60 human leukemia cells has also been studied by MTT method.