Solvent-free Synthesis and Crystal Structure of 2,2＇-Dialkyl Bis(3-methyl-6,7- dihydrobenzofuran-4(5H)-one) Derivatives

A series of 2,2＇-dialkyl bis（3-methyl-6,7-dihydrobenzofuran-4（5H）-one） derivatives was prepared through H2SO4·SiO2 catalyzed condensation reaction under solvent-free conditions as potential anti-tumor agents. All of them were characterized by ESI-MS, IR and NMR spectra. Meanwhile, the single crystal of the target compound （4b）, C24H28O4, was also obtained and determined by X-ray crystallography. Crystal data： triclinic system, space group P , a = 8.463（10）, b = 9.612（11）, c = 13.828（15） , α = 74.29（5）, β = 80.93（5）, γ = 69.90（3）°, V = 1014（2） 3, Z = 2, F（000） = 408, Dc = 1.246 g/cm3, μ = 0.084 mm？1, R = 0.0883 and wR = 0.2440 for 4616 independent reflections （Rint = 0.1200） and 3490 observed ones （I 〉 2σ（I））.

A 2D Cobalt(Ⅱ) Coordination Polymer [Co(iqnc)_2]_n: Synthesis, Crystal Structure and Characterization

A new cobalt（Ⅱ） coordination polymer with the formula of [Co（iqnc）2]n（1, iqnc = l-isoquinolinecarboxylate） has been synthesized through hydrothermal synthesis and structurally characterized by single-crystal X-ray diffraction method. The title coordination polymer represents a two-dimensional layer structure featuring adjacent one-dimensional [Co（iqnc）2]n chains connected with each other by uncoordinated oxygen atoms of carboxylate. Crystal data： monoclinic, space group P21/c, a = 15.4302（2）, b = 5.6743（7）, c = 9.2307（1） A, β = 98.459（2）o, V = 799.41（2） A3, Z = 2, S = 1.019, the final R = 0.0346, w R = 0.0876（I 2σ（I）） and R = 0.0477 and wR = 0.1159 for all reflections. In addition, elemental analysis, IR, and magnetism properties are presented.

Zirconium-mediated Synthesis and Crystal Structure of 3,6-Diiodo-4,5-dialkyl-phthalic Acid Dimethyl Ester

A novel series of para-diiodobenzene derivatives, 3,6-diiodo-4,5-dialkyl-phthalic acid dimethyl esters, were prepared via cycloaddition of two TMS-substituted alkynes and dimethyl acetylenedicarboxylate, which was mediated by zirconocene. After iodination, three new compounds of 3,6-diiodo-4,5-dimethyl（dipropyl, dibutyl）-phthalic acid dimethyl esters （3a, 3b, 3c） were synthesized in high region-selectivity and yields, and characterized by NMR. The crystal structures were determined by single-crystal X-ray diffraction. The crystal of 3a （C12H121204, Mr = 474.02） belongs to the triclinic system, space group Pi with a = 7.6238（10）, b = 9.4571（12）, c = 10.8221（14） A, a = 66.611（10）, fl = 88.511（12）, 7 ： 77.604（11）% V= 697.93（16） A3, Z= 2, F（000） = 444, Dc = 2.256 mg/m3, g = 4.509 mm-1, T=133（2） K, S = 1.014, R = 0.0229 and wR = 0.0547 for 2644 observed reflections with I 〉 20（/）; the crystal of 3b （C16H201204, Mr - 530.12） is of triclinic system, space group Pi with a = 9.4122（19）, b = 10.626（2）, c = 11.353（2） A, a = 97.90（3）, fl = 113.83（3）, y = 110.22（3）°, V= 922.6（3） A3, Z- 2, F（000） = 508, Dc - 1.908 mg/m3, g = 3.422 mm-1, T = 113（2） K, S = 1.115, R = 0.0428 and wR = 0.1072 for 3971 observed reflections with I〉 20（/）; the crystal of 3c （ClsH241204, Mr = 558.17） belongs to the monoclinic system, space group P21/c with a = 26.396（2）, b = 8.7560（8）, c = 25.7970（18） A, fl = 91.721（4）o, V= 5959.6（8） A3, Z = 12, F（000） = 3240, Dc = 1.866 mg/m3,/z = 3.184 mm-l, T= 113（2） K, S = 1.154, R = 0.0424 and wR = 0.0766 for 13056 observed reflections with I 〉 20（/）.

Stereoselective Synthesis and Crystal Structure Analysis of N-Naphthyl-2-deoxy-α-D-ribopyranosylamine

A new compound N-naphthyl-2-deoxy-α-D-ribopyranosylamine was synthesized and structurally determined. It crystallizes in the orthorhombic system, space group P212121 with a = 8.361（2）, b = 12.432（3）, c = 12.791（4） A^°, Z= 4, V= 1329.6（6） A^°^3, Dc= 1.295 g/cm^3, F（000） = 552, Cl5H17NO3 and Mr= 259.30. All the active hydrogen atoms are involved in the formation of hydrogen bonds in the molecule.

Ba_2SbGaS_5 : Solid-state Synthesis, Crystal and Electronic Structures, and Property Characterization

Single crystal of Ba2SbGaSs has been synthesized by the high temperature solidstate reaction method. The compound crystallizes in the orthorhombic space group Pnma with a = 12.177（4）, b = 8.880（3）, c = 8.982（3） A, V= 971.4（6） A3, Z = 4, De = 4.284 g/cm3,μ = 14.487 mm-1, F（000） - 1096, the final R = 0.0171 and wR = 0.0384 for all data. The structure comprises an infinite one-dimensional 1∞[SbGaS5]4- anionic chain constructed from the GaS4 tetrahedra and the SbS5 polyhedra via sharing edge alternately. The paralleled 1∞[SbGaS5]4anionic chains engage with each other and form the two-dimensional Sb-Ga-S layer perpendicular to a-axis with the isolated Ba2＋ cations arranged between layers. The IR spectrum and the UV-Vis spectrum have been investigated. Also, the first-principles band structure and density of states calculations indicate that the compound belongs to indirect semiconductor with the band gap of 2.1 eV, which is supported by the UV-Vis diffuse reflectance results.

Synthesis, Crystal Structure and Biological Activity of 1,5-Bis(4-methoxyphenyl)-3-(4-methyl-1,2,3-thiadiazol-5-yl)pentane-1,5-dione

The title compound 1,5-bis（4-methoxyphenyl）-3-（4-methyl-1,2,3-thiadiazol-5-yl）-pentane-1,5-dione （C22H22N2O4S, Mr=410.49） has been synthesized by the reaction of 4-methyl-1,2,3-thiadiazole-5-carbaldehyde with 4-methoxyacetophenone, and its structure was characterized by IR, 1H NMR, H RMS, elemental analysis and single-crystal X-ray diffraction. The crystal of the title compound belongs to monoclinic, space group P21/c with a=11.159（3）, b=9.002（3）, c=20.192（6）, β=93.393（5）°, Z=4, V=2024.6（10） 3 , Dc=1.347 g/cm3 , μ=0.191 mm-1 , F（000）=864, R=0.0333 and wR （I〉2σ （I））=0.0840. In this molecule, the 1,2,3-thiadiazol ring is nearly vertical with both phenyl rings, and intermolecular weak hydrogen bonds of C-H…O and C-H…N types together with π-π stacking interactions and interactions between S（1）…N（2） are observed. The above three kinds of interactions extend the molecules into a two-dimensional layer framework. The preliminary biological test showed that the title compound had fungicidal activity.

Synthesis and Crystal Structure of 3,6-Bis(4-methyl-1,2,3-thiadiazol-5-yl)-1,2,4-triazolo[3,4-b][1,3,4]thiadiazole

The compound 3,6-bis（4-methyl-1,2,3-thiadiazol-5-yl）-1,2,4-triazolo[3,4-b][1,3,4] thiadiazole（C9H6N8S3,Mr = 322.40） has been synthesized by the reaction of 4-amino-3-（4-methyl-1,2,3-thiadiazolyl）-5-mercapto-1,2,4-triazole with 4-methyl-1,2,3-thiadiazol-5-carboxylic acid and phosphorus oxychloride,and its structure was characterized by IR,1H NMR,EI-MS,elemental analysis and single-crystal X-ray diffraction.The crystal of the title compound belongs to monoclinic,space group C2/c with a = 2.0053（4）,b = 1.3081（3）, c = 1.0556（2） nm, β = 112.69（3）°,Z = 4, V= 2.5548（9） nm^3, Dc = 1.676 g/cm^3, μ= 0.582 mm^-1, F（000） = 1312, R = 0.0546 and wR = 0.1523. X-ray analysis indicates that all rings are essentially planar in this molecule, and an intermolecular hydrogen bond C（9）-H（9）…N（2） and weak intramolecular interactions between S（1）…N（7）, S（3）…N（1） and S（2）…N（4） are observed.

Synthesis and Crystal Structure of N-methyl-N-((2-(p-tolyl)quinolin-4-yl)methyl)aniline

Compound 1, N-methyl-N-（（2-（p-tolyl）quinolin-4-yl）methyl）aniline （C24H22N2）, as a potential drug for the treatment of acid-related diseases has been synthesized via palladium- catalyzed intramolecular hydroarylation. The compound was characterized by MS and NMR spectra. Meanwhile, the crystal of I was obtained and determined by X-ray single-crystal diffrac- tion. Crystal data： triclinic system, space group P1, a = 5.548（5）, b = 11.545（10）, c = 14.546（12）A, a = 90.427（15）, β = 90.727（14）, γ = 101.099（16）°, V= 914.1（13） A3, Z = 2, F（000） = 360, Dc = 1.230 g/cm3,μ = 0.072 mm-1, R = 0.0564 and wR = 0.1616 for 9768 independent reflections （Rint = 0.0447） and 3003 observed ones （I 〉 2σ（I））.

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.

Synthesis and Crystal Structure of(Z)-2-Methyl-5,6-dihydrobenzo[d]thiazol-7(4H)-one O-Prop-2-yn-1-yl Oxime Derivatives

Compound（Z）-2-methyl-5,6-dihydrobenzo[d]thiazol-7（4H）-one O-prop-2-yn-1-yl oxime, C11H12N2 OS, as a synthetic precursor of cytotoxic triazoles has been prepared and characterized by NMR spectra. Meanwhile, the crystal of IV was obtained and determined by X-ray single-crystal diffraction. Crystal data： monoclinic system, space group P21/c, a = 9.725（9）, b = 8.068（7）, c = 14.452（13）A, β = 98.68（2）°, V = 1120.9（17）A3, Z = 4, F（000） = 464, Dc = 1.305 g/cm^3, μ = 0.263 mm^-1, R = 0.0457 and w R = 0.1298 for 11511 independent reflections（Rint = 0.0709） and 2289 observed ones（I 〉 2σ（I））.

Synthesis, Crystal Structure and Biological Activity of N-(tert-butyl)-N'-(2-(4-chlorophenyl)acetyl)-5-methyl-1,2,3-thiadiazole-4-carbohydrazide

The title compound N-（tert-butyl）-N＇-（2-（4-chlorophenyl）acetyl）-5-methyl-1,2,3-thiadiazole-4-carbohydrazide （C16H19ClN4NaO2S, Mr = 366.86） has been synthesized, and its structure was characterized by IR, 1H NMR, H RMS and single-crystal X-ray diffraction. The crystal of the title compound belongs to triclinic, space group Pī with a = 8.464（2）, b = 10.192（2）, c = 11.757（2）, α = 68.48（3）, β = 76.31（3）, γ = 80.86（3）°, Z = 2, V = 2024.6（10） 3, Dc = 1.333 g/cm3, μ = 0.339 mm-1, F（000） = 384, R = 0.0450 and wR （Ⅰ 〉 2σ（Ⅰ）） = 0.1234. X-ray analysis indicates one N-H…N intermolecular hydrogen bond and no π-π stacking interactions are observed in this crystal structure. The preliminary biological test shows that the title compound has fungicidal activity and antivirus activities against tobacco mosaic virus.

Synthesis and Crystal Structure of (E)-2-phenyl-6,7dihydrobenzofuran-4(5H)-one O-cyanomethyl Oxime

A pair of E/Z-isomers of 2-phenyl-6,7-dihydrobenzofuran-4（5H）-one O-cyanomethyl oxime,C16H14N2O2,as potential drugs for treating peptic ulcer and other acid-related diseases have been synthesized and characterized by IR,MS and NMR spectra.Meanwhile,the crystal of IIIa was obtained and determined by X-ray single-crystal diffraction.Crystal data： monoclinic system,space group P21 /c,a = 8.423（8）,b = 19.596（16）,c = 8.770（8）,β = 107.750（12）°,V = 1379（2）3,Z = 4,F（000） = 560,Dc = 1.283 g/cm3,μ = 0.086 mm 1,R = 0.0681 and wR = 0.2029 for 14472 independent reflections（Rint = 0.0782） and 2428 observed ones（I 2σ（I））.

Synthesis and Crystal Structure of(Z)-5-fluoro-3-(phenyl((5-(pyridin-3-ylmethyl)thiophen-2-yl)amino)methylene)Indolin-2-one

The crystal structure of the title compound （Z）-5-fluoro-3-（phenyl（（5-（pyridin-3- ylmethyl）thiophen-2-yl）amino）methylene） indolin-2-one （C25H18FN3OS, Mr = 427.50） has been prepared and determined by single-crystal X-ray diffraction. The crystal is of orthorhombic, space group P212121 with a = 5.931（1）, b = 12.413（1）, c = 28.102（2） A, V= 2090.4（3） A3, Z = 4, Dc = 1.358 g/cm3, F（000） = 888, μ= 0.186 mm-1, MoKa radiation （2 = 0.71073）, R = 0.041 and wR = 0.105 for 4567 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals that the indole and thiophene rings are not coplanar with a dihedral angle of 46.26（5）°. Intramolecular and intermolecular N-H＇..O hydrogen bonds together with C-H...π interations can be observed in the lattice.

Synthesis and Crystal Structure of 3-(2-Hydroxybenzly)-4-(4-Hydroxybenzylideneamino)-(1H) -1,2,4-Triazole-5-Thione and Its Antibacterial Activities

The title compound C15H12N4O2S was synthesized by the reaction of 3-（2-hydroxybenzyl）-4-amino-（1H）-1,2,4-triazole-5-thione with 4-hydroxybenzaldehyde in ethanol and characterized by IR, ^1H NMR spectra and elemental analysis. Its structure has been determined by X-ray diffraction analysis. The crystal belongs to monoclinic, space group C2/c with a = 27.990（3）, b = 13.1326（14）, c = 7.9770（8） A, β= 105.787（2）°, V = 2821.6（5）A^3, Z = 8, Mr= 312.35,μ= 0.243 mm^-1, Dc = 1.471 g/cm^3 and F（000） = 1296. The structure was solved by direct methods.and refined to a Rint value of 0.0388. The crystal structure involving in intermolecular N-H…S and O-H…S hydrogen bonds is observed, meanwhile intramolecular O-H…N hydrogen bond is also found. Their biological activities have been measured. The results show that this type of compound has certain antibacterial activity for Staphylococous aureus and Bacillus subtilis.

Synthesis and Crystal Structure of 1-[4-(Pyrimidin-2-yl)piperazin-1-ylmethyl]-1H-benzotriazole

The crystal structure of the title compound （C15H17N7, Mr = 295.36） has been determined by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P1^- with a = 6.370（2）, b = 9.830（3）, c = 11.821（4） A, α = 89.603（6）, β = 86.018（6）, γ = 85.850（6）°, V = 736.5（4） A^3, Z= 2, F（000） = 312, Dc = 1.332 g/cm^3, μ = 0.087 mm^-1, the final R = 0.0476 and wR = 0.1079 for 1494 observed reflections with Ⅰ 〉 2σ（Ⅰ）. X-ray analysis reveals that the piperazine ring of the title compound is in a chair conformation. In addition, in the crystal structure there also exist intramolecular C-H…N hydrogen bonds and intermolecular π-π interactions between benzotriazole rings.

Synthesis and Crystal Structure of 2-Amino-4- chloro-5-(4-methylbenzyl)-6-methylpyrimidine

The title compound 2-amino-4-chloro-5-（4-methylbenzyl）-6-methylpyrimidine （C26H28Cl2N6, Mr = 495.44） has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. The crystal belongs to monoclinic, space group P21/c with a = 14.892（7）, b = 6.129（3）, c = 14.889（7）A, β = 109.795（8）°, V = 1278.7（10）A^ 3, Z = 2, F（000） = 520, Dc = 1.287 g/cm^3, μ = 0.280 mm^-1, the final R = 0.0577 and wR = 0.1589 for 1357 observed reflections with I 〉 2σ（I）. A total of 6091 reflections were collected, of which 2257 were independent （Rint = 0.033）. The X-ray analysis reveals that the chlorine atom and methyl of the title compound are disordered.

Synthesis and Crystal Structure of N-[4-(4-Methyl-phenylsulfamoyl)-phenyl]- 4-methyl-1,2,3-thiadiazole-5-carboxamide

The crystal structure of the title compound （C17H16N4O3S2, Mr = 388.46） has been determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c with a = 13.688（2）, b = 16.704（3）, c = 8.3308（12）A, β = 99.474（6）°, V = 1878.8（5） A^3, Mr = 388.46, Z = 4, Dc = 1.373 g/cm3, μ = 0.308 mm^–1, F（000） = 808, R = 0.0389 and wR = 0.0917. X-ray analysis reveals that the crystal structure involves intermolecular N–H…O and N–H…N hydrogen bonds, which link the molecules into a layer parallel to the ac plane.

Synthesis and Crystal Structure of 1-Phenyl-2-acetoxy-2-methyl-1-propanone

1-Phenyl-2-acetoxy-2-methyl-propanone, a new a-hydroxy ketone derivative, was synthesized by Friedel-Crafts acylation and characterized by FT-IR, 1H NMR, MS spectra and single-crystal X-ray diffraction measurements. The data are as follows： monoclinic, space group P21/c, Z = 4, C12H1403, Mr = 206.24, a = 8.9430（2）, b =15.2680（4）, c = 8.2550（2） A, β = 91.9650（5）°, V = 1126.60（5）A^3, Dc = 1.216 g/cm^3, μ（MoKα） = 0.087 mm^-1, F（000） = 440, R = 0.0725 and wR = 0.1379 for 1282 observed reflections with I〉 2σ（I）. The structure was solved by direct methods and refined by full-matrix least-squares refinement on F2 methods. The benzene ring in the structure is almost coplanar with the adjacent carbonyl groups and t-carbonyl atom. Meanwhile, the long chain is approximately perpendicular to the plane. X-ray analysis reveals that the crystal structure involves two weak intramolecular C-H…O hydrogen bonds.

Synthesis, Dimeric Crystal Structure, and Biological Activities of N-(4-Methyl-6-oxo-1,6-dihydro-pyrimidin-2-yl)-N′-(2-trifluoromethyl-phenyl)-guanidine

The title compound, N-（4-methyl-6-oxo-1,6-dihydro-pyrimidin-2-yl）-N＇-（2-tritluoromethyl-phenyl）-guanidine, was synthesized and its structure was confirmed by using IR, MS,^1H NMR, and elemental analysis. The single crystal structure of the title compound was determined by X-ray diffraction. The preliminary biological test showed that the synthesized compound has a weak herbicidal activity.

Synthesis, Crystal Structure and Biological Activity of 2-Chloro-N-{2-fluoro-5-[N-(phenylsulfonyl) phenyl-sulfonamido]phenyl}benzamide

2-Chloro-N-{2-fluoro-5-[N-（phenylsulfonyl）phenylsulfonamido]phenyl}benzamide was synthesized and its crystal structure was also determined by X-ray single-crystal diffraction. The title compound（C25H18ClFN2O5S2） belongs to monoclinic, space group P21/n with a=0.7377（3） nm, b=1.2036（5） nm, c=2.6846（11） nm, β=90.895（9）°, V=2.3833（16） nm3, Mr=544.98, Z=4, Dc=1.519 g/cm3, μ=0.385 mm–1, F（000）=1120, R1=0.0632, and wR2=0.1438. Its crystal structure belongs to a novel class that has not been reported yet, and its preliminary herbicidal activity was also tested. Its inhibition rate to seedling growth of barnyard grass reaches 15.1% at 100 μg/mL.