A New Terbium（III） Coordination Compound with 2-Thiophenecarboxylic Ligand： Synthesis and Crystal Structure①

A new coordination compound with formula [Tb（2-TC）3（DMF）]n （1, 2-TC = 2-thio- phenecarboxylic ligand and DMF = dimethylformamide） was synthesized by solvothermal method. The structure of compound 1 was determined by single-crystal X-ray diffraction analyses, and characterized by elemental analyses, IR and powder X-ray diffraction. Structure analysis reveals compound 1, exhibiting a one-dimensional chain structure, crystallizes in triclinic space group P21/c, with a = 9.2751（19）, b = 16.490（3）, c = 15.865（5） A, β = 118.98（2）°, V= 2122.7（9）A3, D,. = 1.916 g/cm3, Mr= 612.45 （C18H15NO7S3Tb）, F（000） = 1196,μ（MoKa） = 3.67 mm-1, Z = 4, R = 0.0616 and wR = 0.0962 for 3865 observed reflections （I 〉 2o（I））, and R = 0.1092 for all data. Meanwhile, the photoluminescent properties of compound 1 were also investigated in the solid state at room temperature.     

Study on the Synthesis and Properties of Metal-organic Complex Containing Samarium

A new rare earth organic complex with a double interleaved structure,namely[Sm(BDC)_(1.5)(DMF)(H_2O)]_n (H_2BDC=1,4-benzenedicarboxylic acid,DMF=N,N?-dimethyl formamide) was synthesized.The crystal structure is of triclinic,space group P1 with a=8.6343(6),b=10.1470(5),c=11.2073(6)?,α=65.495(5),β=71.626(5),γ=78.130(5)°,V=844.70(9)?~3,C_(15)H_(15)NO_8Sm,M_r=487.64,Z=2,D_c=1.917g/cm~3,F(000)=476,μ=3.519 mm~(-1),R=0.0380 and w R=0.0864 for 3504 observed reflections (I2?(I)).The structure has been determined by single-crystal X-ray diffraction analyses and displays a 2-fold interpenetrated 3D network with the classical pcu topology.The compound was analyzed by X-ray powder,infrared spectroscopy,thermogravimetric analysis and fluorescent spectroscopy.The fluorescent property makes it a good candidate for photoactive materials.     

Synthesis,Crystal Structure and Antifungal Activity of 4-(5-((2,4-Dichlorobenzyl)thio)-4-phenyl-4H-1,2,4-triazol-3-yl)pyridine

The title compound 4-(5-((2,4-dichlorobenzyl)thio)-4-phenyl-4H-1,2,4-triazol-3-yl)pyridine(C20H14Cl2N4S) was synthesized, and its structure was confirmed by 1H NMR, MS, elemental analyses and X-ray diffraction. It crystallizes in the monoclinic system, space group P21/c with a = 14.885(5), b = 8.597(2), c = 16.144(5) A, β = 114.505(4)o, V = 1879.8(10) A3, Z = 8 and R = 0.0320 for 3108 observed reflections with I 2σ(I). The preliminary biological test shows that the title compound has activities against Stemphylium lycopersici(Enjoji) Yamamoto, Fusarium oxysporum. sp. cucumebrium, and Botrytis cinerea with inhibitory to be 53.57%, 66.67% and 24.44%, respectively.     

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.     

Synthesis,Crystal Structure and Antifungal Activity of 2-((2-Fluorobenzyl)thio)-5-(pyridin-4-yl)-1,3,4-oxadiazole

The title compound 2-((2-fluorobenzyl)thio)-5-(pyridin-4-yl)-1,3,4-oxadiazole(C_(14)H_(10)FN_3OS) was synthesized,and its structure was confirmed by ~1H NMR,MS,elemental analyses and X-ray diffraction. It crystallizes in the monoclinic system,space group P21/n with a = 11.541(16),b = 8.226(12),c = 13.683(19) ?,β = 94.872(17)o,V = 1294(3) ?~3,Z = 4 and R = 0.0648 for 2198 observed reflections with I 2σ(I). The preliminary biological test shows that the title compound has good activity against Pythium ultimum with inhibitory to be 100%.     

Synthesis and Crystal Structure of 2-(4-Nitrophenyl)-1,2-benzisoselenazol-3(2H)-one DMF (1:1) Solvate

The title compound (C13H8N2O3Se-C3H7NO) has been synthesized by a simple synthetic route and by recrystallization from DMF. The molecular structure of this compound was obtained by single-crystal X-ray diffraction. The compound crystallized in the triclinic space group P with a = 7.450(6), b = 8.150(7), c = 13.859(12) , α = 75.014(14), β = 83.072(18), γ = 84.409(14)°, V = 805.0(12)3, Z = 2 and R = 0.0271 for 2575 observed reflections with I > 2σ(I). X-ray analysis reveals that not only intermolecular Se…O and C-H…O interactions, but also π…π stacking interactions exist in the adjacent molecules. The above three kinds of intermolecular interactions extend the complex into an infinite three-dimensional layered network.     

Synthesis and Crystal Structure of Compound [ZnS6 (C12H8N2)]

The title compound ZnS6(C12H8N2) was obtained by reaction of zinic powder with sulfur and 1,10-phenathtroline in DMF solvent, and its structure has been determined by single crystal X-ray diffraction analysis. The crystal data for the compound: triclinic, P-1, Z = 2, a = 8. 159(2), b = 9. 485(2), c = 11. 997(2)A , α =110. 00(3)°,β = 99.22(3)°, γ = 100.57(3)°, V = 832A3, Dc =1. 748g/cm3, μ(MoKa)=0. 2219 cm-1, F(000)=440. The structure was refined to R = 0. 0723 and Rw = 0. 0865 for 1427 independent observed reflections. The tilte crystal consists of a discrete molecules, in which the core of ZnS2N2 shows a distorted tetrahedral geometry.     

Synthesis,Crystal Structure and Electronic Structure of Novel Semiconducting KCdAsS_3

A new compound of KCdAsS_3(Mr = 322.60) was successfully synthesized using thiourea reactive flux method. The crystal structure was determined by single-crystal X-ray diffraction. The title compound crystallizes in a monoclinic system of space group P21/n with a = 5.9537(7), b = 16.633(3), c = 6.093(1) ?, b = 90.781(3)°, V = 610.0(1) ?3, Z = 4, Dc = 3.513 g/cm3, m(Mo Kα) = 10.52 mm-1, F(000) = 592, R = 0.057 and w R = 0.136 for 899 observed reflections with I 2σ(I). The crystal structure of KCdAsS_3 features [Cd As S3]-layers, which are separated by K+ ions. First-principles calculations show that KCdAsS_3 is an indirect band gap semiconductor with a band gap of 2.3 e V. The novel layered compound of tetrahedra CdS_4 and pyramids AsS_3 is potentially useful for photoluminescent, photocatalytic and photoelectric applications.     

Synthesis and Crystal Structure of a Luminescent Compound 5-（1H-benzoimidazol-2-yl）- 3H-[ 1,2,3 ] triazole-4-carboxylic Acid

The title compound, 5-(1H-benzoimidazol-2-yl)-3H-[1,2,3]triazole-4-carboxylic acid (C10H7N5O2·C3H7NO, Mr=302.30), has been synthesized and characterized by FT-IR and ESI-MS, 1 H-NMR spectroscopy and X-ray single-crystal diffraction. Crystal structure of the title compound was grown from DMF by slow diffusion at room temperature. Crystal data: orthorhombic structure, space group Pna21 with a=6.9635(3), b=19.4398(7), c=30.6165(12), V=4144.5(3)3, Z=12, Dc=1.454 g/cm 3, μ(MoKα)=0.108 mm-1, and F(000)=1896. The structure was refined to R=0.0450 and wR=0.0975 for 3578 observed reflections with I>2σ(I). The intermolecular hydrogen bonds and π-π stacking further stabilize the structure.     

CRYSTAL AND MOLECULAR STRUCTURE OF HUMOSINE A

<正> The structure of humosine A, C20H19NO5, which represents a new kind of phthalide isoquinoline alkaloid,has been determined by X-ray diffraction analysis. The compound crystallized in the space group P212121 with a=7.654(2), b=12.926(2), c= 17.018(8) A, Z=4, V=1681.7A3, Dx=1.459g.cm-3, μ(Moke(?))=1.014 cm-1, F(000)=776. The structure was solved by direct methods, and refined by full-matrix least-squares with final R = 0.032 for 1517 observed reflections (I≥3σ).     

A Zinc(Ⅱ) Coordination Framework Based on Terpyridine and 5-Nitroisophthalic Acid Mixed Ligands: Synthesis,Crystal Structure and Fluorescence Property

A new coordination framework, {[Zn(L1)(5-nipc)]·H2O}n(1, L1 = 4ˊ-(4-pyridyl)-4,2ˊ:6ˊ,4ˊˊ-terpyridine, 5-nipc = 5-nitroisophthalic acid), has been prepared under hydrothermal conditions, and determined by single-crystal X-ray diffraction analyses and further characterized by elemental analyses, IR and powder X-ray diffraction. Complex 1 crystallizes in monoclinic, space group C2/c with a = 29.983(9), b = 13.709(3), c = 14.391(3)A, β = 114.93(4)°, V = 5364(2) A3, Dc = 1.493 g/cm3, C28H19N5O7 Zn, Mr = 602.85, F(000) = 2464, μ(Mo Kα) = 0.972 mm-1, Z = 8, R = 0.0935 and w R = 0.1509 for 4724 observed reflections(I 2σ(I)). The structure of 1 exhibits a three-dimensional(3D) network with a layer-pillar structure. The fluorescence property of 1 is also investigated.     

Microwave Assistant Synthesis and Dimeric Crystal Structure of 2-(((6-Chloropyridin-3-yl)-methyl)thio)-5-(pyridin-4-yl)-1,3,4-thiadiazole

The title compound 2-(((6-chloropyridin-3-yl)methyl)thio)-5-(pyridin-4-yl)-1,3,4-thiadiazole 5(C26H18Cl2N8S4) was synthesized, and its structure was confirmed by 1H NMR, MS and elemental analyses and X-ray diffraction. It crystallizes in the triclinic system, space group P1 with a = 9.452(4), b = 12.335(4), c = 13.017(5) A, α = 90.624(5), β = 110.541(5), γ =104.879(4)°, Dc = 1.561 g/cm3, Z = 2, V = 1364.9(9) A3, F(000) = 656, the final R = 0.0300 and w R = 0.0635 for 4206 observed reflections with I 2σ(I). The preliminary biological test showed that the title compound has activities against Stemphylium lycopersici(Enjoji) Yamamoto, Fusarium oxysporum. sp. cucumebrium, and Botrytis cinerea with inhibitory activities to be 9.82%, 44.44% and 20.00%, respectively.     

Synthesis,Crystal Structure and Anticoagulant Activity of 5-Chloro-N-[[（5S）-2-oxo-3-[4-（2- oxopyridin-1 （2H）-yl）phenyl] oxazolidin-5- yl] methyl] thiophene-2-carboxamide①

The title compound(zifaxaban 2, C20H16ClN3O4 S, Mr = 429.87) was synthesized and its crystal structure was determined by single-crystal X-ray diffraction. Zifaxaban crystallizes in monoclinic, space group P21 with a = 5.7900(12), b = 13.086(3), c = 12.889(3) A, β = 100.86(3)°, V = 959.1(3) A3, Z = 2, Dc = 1.489 g/cm3, F(000) = 444, μ = 0.342 mm-1, the final R = 0.0320 and wR = 0.0640 for 2717 observed reflections(I 2σ(I)). The absolute configuration of the stereogenic center in the title compound was confirmed to be S by single-crystal X-ray diffraction. Four existing intermolecular hydrogen bonds help to stabilize the lattice and the molecule in the lattice to adopt an L-shape conformation. Zifaxaban was slightly more active than rivaroxaban 1 in in vitro assay against human FXa and therefore is promising as a drug candidate.     

Synthesis and Crystal Structure of a Novel 14,20-Annulated Pentacyclic Steroid 17(S)-Methyl-13β-hydroxyl-14(R),20(S)-epoxy-pregn-4-en-3-one

The title compound 17(S)-methyl-13β-hydroxyl-14(R),20(S)-epoxy-pregn-4-en-3-one was synthesized by an improved tandem reaction, and its structure was determined by IR, NMR, HR MS and X-ray single-crystal diffraction. The crystal belongs to orthorhombic, space group P212121 with a = 10.55248(15), b = 12.14700(16), c = 14.56841(18) ?, V = 1867.39(4) ?3, Z = 4, Dc= 1.175 g/cm3, μ= 0.604 mm-1, F(000) = 720, the final R = 0.0400 and w R = 0.1072 for 3610 observed reflections with I 2σ(I).     

Synthesis and Crystal Structure of Methyl 2-(Diphenylamino)-4-phenyl-1,3-thiazole-5-carboxylate

The title compound, methyl 2-(diphenylamino)-4-phenyl-1,3-thiazole-5-carboxylate, was synthesized and studied by single-crystal X-ray diffraction method. The structure of the product was confirmed by IR, 1H- and 13C-NMR spectroscopy and elemental analysis. These experimental studies were supported by quantum mechanical calculations. The structure was solved in monoclinic, space group P21/c with a = 9.573(3), b = 19.533(7), c = 9.876(3), β = 92.35(4)°, V = 1845.2(10)3, T = 85(2) K, Z = 4, R = 0.040 and wR = 0.089 for 6424 observed reflections withI>2σ(I).     

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,Crystal Structure and Fungicidal Activity of 2-Chloro-N-(o-tolylcarbamoyl)nicotinamide

The title compound 2-chloro-N-(o-tolylcarbamoyl)nicotinamide(C_(14)H_(12)ClN_3O_2) was synthesized, and its structure was confirmed by ~1H NMR, H RMS and X-ray diffraction. It crystallizes in the monoclinic system, space group P21/n with a = 7.8356(7), b = 12.7949(8), c = 13.6326(10) ?, β = 91.929(7)°, V = 1365.97(18) ?~3, Z = 4, the final R = 0.0416 and wR = 0.0971 for 2467 observed reflections with I 2σ(I). The preliminary biological test shows that the title compound has certain fungicidal activities.     

Crystal Structure and Molecular Docking of a Novel 4-(2-Acetonyl-selanyl-benzamido) Benzoic Acid as a Potential Anti-ischemic Stroke Candidate

The title compound 4-(2-acetonyl-selanyl-benzamido) benzoic acid was synthesized and its structure was determined by NMR, HR MS and X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group P2_(1/n), with a = 5.18537(19), b = 18.9308(7), c = 16.6586(5) ?, b = 95.857(3)°, V = 1626.72(10) ?~3, Z = 4, D_c = 1.536 g/cm~3, m = 3.302 mm~(-1), F(000) = 760, the final R = 0.0466 and wR = 0.1353 for 2308 observed reflections with I 2σ(I). In silico docking studies were carried out to evaluate the anti-ischemic stroke activities for twenty-one ischemic stroke associated proteins by Autodock 4.2 software. The title compound has better activity against ischemic stroke than Ebselen.     

2-D Supramolecular Network and Photoluminescence of a Coupled 1,4-Dihydrylpyridine

A coupled 1,4-dihydrylpyridine compound(C40H48N2O10,1) has been synthesized.Its structure was determined by single-crystal X-ray diffraction.The crystal is of monoclinic system,space group P21/c with a = 8.3300(2),b = 15.720(3),c = 14.480(3) ,β = 90.08(3)°,V = 1896.1(7) 3,Z = 2,Mr = 716.80,Dc = 1.255 g/cm3,and F(000) = 764.The structure was solved by direct methods and refined by full-matrix least-squares method to the final R = 0.0556 and wR = 0.1499(I > 2σ(I)).There exist several supramolecular motifs in the crystal structure.The compound exhibits strong photoluminescence in the solid state at room temperature.     

Crystal Structure of cis—2—[P,P—Diethoxy） phosphono（m—nitro）benzyloxy]

The crystal structure of the title compound cis-2-[(P, P-Diethoxy)phosphono(m-nitro)benzyloxy]-4-Phenyl-5,5-Dimethyl-1,3,2-Dioxaphosphorinane 2-Sulfide, C22H29NO8P2S, was determined by single crystal X-ray diffraction. It crystallizes in the monoclinic system, space group P21/c, with Mr=529.49, a=9.888(2), b=20.831(4), c=12.797(3) , β=94.42(3)°, V=2628(1) 3, Z=4, Dx=1.338 g/cm3, λ=0.71073, μ=0.2796 mm-1 and F(000)=556. The structure was solved by direct methods. The final R factor is 0.052 and Rw is 0.057 for 1793 unique observed reflections [I≥3σ(I)]. A cis-configuration and a preferred chair conformation for the molecule have been established by X-ray diffraction analysis. The results presented also give a good explanation to the correlation between the configurational assignments and the regularity in the chemical shifts of C4-H and 31P NMR.