Synthesis and X-ray Crystal Structure of a New Molecular Clip

The synthesis and X-ray crystal structure of a new molecular clip 2 was reported. It （C24H24N4O2, Mr = 400.47） crystallizes in the space group C2/c with a = 15.587（2）, b = 8.5805（12）, c = 15.259（2） A, β = 102.448（3）°, V= 1992.9 （5）A63, Z = 4, Dc = 1.335 g/cm63,μ = 0.087 mm^-1 and F（000） = 848. It remains monomeric in the crystal and a tape-like structure is formed in the crystal structure of molecular clip. The most unusual structural feature of 2 is the boat conformation of its cyclohexyl ring imposed by the ring fusion at C（9）-C（9a）.

CRYSTAL STRUCTURE AND X-RAY POWDER DIFFRACTION DATA FOR RE COMPOUND HoNiSb

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X-ray and DFT Crystal Structure Determination and Conformational Analysis of a Pyrethroid Compound

The structure of （E）-N-[（E）-3-[（lR,2R）-2-（3,4-dibromo-phenyl）-l-fluro-cyclopropyl]- allylidene]-2-0-tolyl-acetamide （C21HIsONFBrz, Mr = 479.18） has been determined by X-ray single- crystal diffraction and theoretical calculations to establish the configuration, stereochemistry and a stable conformation of the molecule. The compound crystallizes in the monoclinic space group P21/c, a = 28.3452（10）, b = 4.9311（10）, c = 14.257（2） A, fl = 102.7654（10）, V = 1943.5（5） A3 and Z = 4. The structure has been refined to the final R = 0.05 for the observed structure factors with 1 〉 30（/）. Theoretical calculations in the ground state have been carried out for the compound studied using the Hartree-Fock （HF） and density functional theory （DFT） （B3LYP） with 6-31G（d,p） basis sets. The results show that the studied compound prefers the keto form. The compound involves intra- and intermolecular hydrogen bonding of C-H.-.O and C-H-..F types, which further stabilize the structure and display a trans configuration for the C=N and C=C double bonds. The calculated results show that the predicted geometry can well reproduce the structural parameters.

Synthesis and X-ray Crystal Structure of a Methylene-bridged Glycoluril Dimer

The synthesis and X-ray crystal structure of a methylene-bridged glycoluril dimer 2 was reported.The methylene-bridged glycoluril dimer 2（C38H36Br4N8O12,Mr=1116.35） crystallizes in space group P1 with a=10.5802（6）,b=16.8469（9）,c=24.7673（14） ,α=98.00,β=96.263（1）,γ=101.606（1）o,V=4239.3（4）3,Z=4,Dc=1.749 g/cm3,μ=3.869 mm-1 and F（000）=2224.It crystallizes in an S-shaped conformation that displays two ethoxycarbonyl groups on each face of the molecule.

THE FIRST BINUCLEAR MOLYBDENUM AND TUNGSTEN COMPLEXES WITH DOUBLY-BRIDGING PYRIDINE-2-THIOLATO LIGANDS.X-RAY CRYSTAL STRUCTURE OF THE COMPLEX[Mo_2(CO)_4(μ-pyS)_2(PPh_3)_2].2C_7H_8

The title complex was obtained by reactions of [Mo(CO)_3(MeCN)_3] with [CuBr(pySH)(PPh_3)_2]or directly with pySH and PPh_3. The latter method can be used to synthesize the corresponding tungsten complex [W_2(CO)_4(μ-pyS)_2(PPh_3)_2].The molecular structure of the title compound was determined by X-ray diffraction method.

Phase Behavior and Crystal Structure of Perovskite-Type Rare Earth Complex Oxides

Several compounds of rare earth complex oxides containing manganese and titanium were synthesized in Ar, and their crystal structures were analyzed by powder X-ray diffraction data and Rietveld method. Structures of A0.67Ln0.33 Mn0.33Ti0.6703（A = Ca or Sr and Ln = rare earth） were found to have orthorhombic symmetry with the space group Pnrna, and their interatomic distances and bond angles were obtained. This space group was also derived from electron microscopic study. Electrical conductivity of Cao.67Ln0.33Mn0.33Ti0.6703 for several rare earth elements showed a semiconducting property with the activation energy of 0.4 eV. Some of these compounds of the strontium system show the antiferromagnetic properties below 10 K.

Extraction and Absolute Crystal Structure of Stachyose

The title compound stachyose （C24H42021）, a biologicaly active tetrasaccharide, was characterized by X-ray diffraction analysis. It crystallizes in the orthorhombic system, space group P21212 with C24H42021, a = 23.8760（3）, b = 12.71028（I2）, c = 10.81279（11） A, V = 3281.36（6） A3, Z = 4, Dc= 1.511 g/cm3, Mr = 746.58, F（000） = 1576, and μ = 1.230 mm^-1. The final R = 0.0666 and wR = 0.1797 for 6298 observed reflections （I 〉 2σ（I））. The molecular crystal structure of stachyose shows absolute stereochemistry of fl-D-fructofuranosyl a-D-galactopyranosyl- （1→6）-a-D-galactopyranosyl-（1→6）-a-D-glucopyranoside. The molecule is composed of two a-D-galactoses, one a-D-glucose, and one r-D-fructose and sequentially linked as a-Gal （1 →6） a-Gal （1→6） a-Glc （1→2） fl-Fru. The title compound is stacked into a 3D layer structure through hydrogen bonds. NMR spectra data are also assigned. In the crystal packing, X-ray analysis indicates that there are two intramolecular and eleven intermolecular hydrogen bonds in this compound.

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, 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 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））.

Crystal structure and properties of terbium o-methylbenzoate complex with 1,10-phenanthroline [Tb(o-CH_3C_6H_4COO)_3(C_(12)H_8N_2)]_2

A terbium o-methylbenzoate complex with 1,10-phenanthroline, Tb(o-MBA)_3phen(where o-MBA = o-methylbenzoate and phen = 1,10-phenanthroline) was prepared from ethanol solutionand its crystal structure was determined by X-ray diffraction. The crystal of the complexTb(o-MBA)_3phen belongs to triclinic crystal system and P1 (#2) space group. The crystal data are asfollows: a = 1.4371(4) nm, b = 1.7387(2) nm, c = 1.3109(2) nm, α = 96.37(1)°, β = 107.21(2)°,γ= 82.78(2)°, Ⅴ= 3.094(1) nm^3, Z= 2, M_r = 1489.12, D_c= 1.598 g·cm^(-3), μ = 2.330 mm^(-1)and F(000) = 1488.00. The final R and R_w are 0.038 and 0.047 for 8668 [Ⅰ > 2σ(Ⅰ)] uniquereflections, respectively. In the complex each Tb^(3+) ion is eight-coordinated by one1,10-phenanthroline molecule, one bidentate carboxylate group and four bridging carboxylate groups.The carboxylate groups are bonded to the terbium ion in two modes: the chelating bidentate and thebridging bidentate. Excitation and luminescence data observed at room temperature show that thetitle complex emits strong green fluorescence under ultraviolet light. The results of thermalanalysis indicate that the complex Tb(o-MBA)_3phen is quite stable to heat.

Synthesis,Crystal Structure and Thermal Analysis of N-(2,3-Dimethyl-phenyl)-N'-(methoxyl formyl)thiourea

N-（2,3-Dimethyl-phenyl）-N＇-（methoxyl formyl）thiourea was synthesized by the reacting of 2,3-dimethylaniline,potassium thiocyanate（KSCN） and methyl chloroformate（ClCOOCH 3）.Single crystal was obtained by slowly evaporation solvent at room temperature.The structure was characterized by elemental analysis,IR and X-ray crystalography.The compound crystallized：a triclinic system with space group Pī,a=0.83440（12） nm,b=0.89113（13） nm,c=0.93015（13） nm,α=76.548（2） o,β=63.906（2） o,γ=82.538（2） o,V=0.60379（15） nm 3,Z=2,D c =1.311 mg/m 3,F（000）=252,μ=0.256 mm-1,R 1 =0.0379,wR 2 =0.0919.The specific heat capacity of the title compound was determined by a Micro-DSC method,and the specific heat capacity was 1.25 J·g-1 ·K-1 at 298.15 K.Thermodynamic functions,relative to those at the standard temperature of 298.15 K,were calculated via thermodynamic relationship.The thermal behavior of the title compound under a non-isothermal condition was studied by differential scanning calorimetry/thermogravimetric（DSC/TG） method.There was an obvious endothermic peak in the DSC curve,the peak temperature was 479.43 K.The compound mass loss was 89.94% observed from the TG curve.

Synthesis and Crystal Structure of 2,6,8,12-Tetraacetyl- 2,4,6,8,10,12-hexaazatetracyclo[5.5.0.0^(5,9).0^(3,11)]dodecane

The title compound, 2,6,8,12-tetraacetyl-2,4,6,8,10,12-hexaazatetracyclo[5.5.0.05,9.03,11] dodecane (TAIW, C14H20N6O4, Mr = 336.36), has been synthesized by hydrogenolysis debenzylation of tetraacetyldibenzylhexaazaisowurtzitane (TADB) and its crystal structure was determined to be monoclinic, space group C2/c with a = 28.193(6), b = 12.139(2), c = 17.678(4) ?, β = 97.44(3)o, V = 5999(2) ?3, Z = 16, Dc = 1.490 g/cm3, F(000) = 2848, μ(MoKα) = 0.112 mm-1, R = 0.0631 and wR = 0.1586. X-ray investigations indicate that the molecule has different isomers and there exist intermolecular C–H…O hydrogen bonds in the crystal structure. The results of elemental analysis, IR and NMR spectroscopy are included.

Hydrothermal Synthesis and Crystal Structure of a Novel Selenite-chloride:[Cd_4(SeO_3)_2Cl_4(H_2O)]_n with a Three-dimensional Framework

A novel three-dimensional（3-D） compound [Cd4（SeO3）2Cl4（H2O）]n（1） was prepared from a hydrothermal reaction and structurally characterized.Compound 1 crystallizes in the space group Fmmm of the orthorhombic system with eight formula units in a cell：a = 15.5165（4）,b = 17.5090（9）,c = 7.3318（5） ,V = 1991.9（2） 3,Cd4Cl4H2O7Se2,Mr = 863.38,Dc = 5.758 g/cm3,S = 1.075,μ（MoKα） = 16.820 mm-1,F（000） = 3088,R = 0.0427 and wR = 0.1220.Compound 1 features a 3-D structure with the cadmium atoms having two different coordination environments,i.e.,six-and eight-coordination geometries.Two different chain-like structures of cadmium-oxo polyhedra are interconnect to each other to give a 2-D layer of [Cd4（SeO3）2（H2O）]n4n＋.Between the [Cd4（SeO3）2（H2O）]n4n＋ layers is a novel chloride layer.A 3-D framework is constructed from these [Cd4（SeO3）2（H2O）]n4n＋ layers linked by the chloride layers.

Effect of the partial substitution of Mg by Al on the crystal structure and hydrogenation behavior of La_2Mg_(17)

The effect of the partial substitution of Mg by A1 on the crystal structure of La2Mg17 has been investigated. It was found that the LaEMgl7 phase disappears after the partial substitution of Mg by Al. The LaE（Mgo.gAl0.1）17 alloy contains La（Mg,AI）12 and La（Mg,Al）2. Further increasing the Al content, the La2（Mg0.8Al0.2）17 alloy consists of La（Mg,Al）12, La（Mg,Al）2, and Mg. The La（Mg0.93Al0.07）12 phase in the La2（Mg0.9Al0.1）17 alloy crystallizes with the ThMn12-type structure in space group 14/mmm （No. 139）. The lattice parameters were determined to be a = 1.03246（7） nm and c = 0.59410（6） nm. In the ThMn12-type structure, AI atoms occupy 8f site but the A1 content is limited. Moreover, the hydrogenation character- istics have also been compared. La2Mgl7 decomposes into LaH3 and MgH2 under hydrogen, but the La（Mgo.93Alo.o7）12 phase can be hydrogenated into LaH3, MgH2, and La3Al11 at 473 K.

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,Crystal Structure,and Biological Activity of Naphthalen-2-yl4-methyl-1,2,3-thiadiazole-5-carboxylate

The title compound naphthalen-2-yl-4-methyl-1,2,3-thiadiazole-5-carboxylate （C 14 H 10 N 2 O 2 S,M r=270.31） was synthesized by the reaction of 4-methyl-1,2,3-thiadiazole-5-carbonyl chloride with 2-naphthol,and its structure was characterized by IR,1 H NMR,high-resolution mass spectrometry and single-crystal X-ray diffraction.The crystal belongs to orthorhombic,space group Pbcn with a=23.475（5）,b=9.6640（19）,c=10.814（2）,β=90.00°,Z=8,V=2453.2（9） 3,M r=270.30,D c=1.464 g/cm 3,μ=0.262 mm-1,F（000）=1120,R=0.0444 and wR=0.1099.X-ray analysis revealed that the thiadiazole and naphthalene rings were non-planar,while the thiadiazole ring and the ester group were essentially planar,and two intermolecular hydrogen bonds C（6） H（6）···O（1） and C（14） H（14）···O（1） were observed.The preliminary biological test showed that the title compound had antifungal and antivirus activities against tobacco mosaic virus.

Extraction and Crystal Structure of β-Sitosterol

The title compound β-sitosterol（C29H50O）, an active phytosterol in many medicinal and edible plants, was characterized by X-ray diffraction analysis and extensive nuclear magnetic resonance（NMR） data. It crystallizes in monoclinic system, space group P21 with C29H50O·1/2H2O, a = 9.4226（7）, b = 7.4824（9）, c = 36.889（3） , V = 2597.0（4） 3, Z = 4, Dx = 1.084 g/cm3, Mr = 423.70, F（000） = 948, and μ = 0.064 mm-1. The final R = 0.0886 and wR = 0.2234 for 10157 observed reflections（I 〉 2σ（I））. The molecular crystal structure of β-sitosterol shows relative stereochemistry of 24R-ethylcholest-5-en-3β-ol. The molecule is composed of one steroid nucleus（3 six-membered rings and 1 five-membered ring） and one sidechain of 10 carbons. There are two C29H50O molecules and one H2O molecule in a symmetrical unit, and the title compound is stacked into a special laminated structure through hydrogen bonds and van der Waal forces. The special laminated structure was first reported.

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 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））.