Synthesis and Crystal Structure of 2-（1-Naphthalenylamino）-4-thiazolidinone

The compound 2-(1-naphthalenylamino)-4-thiazolidinone was synthesized by the reaction of 1-(naphthalene-1-yl)thiourea with ethyl chloroacetate in an ionic liquid, and its structure was characterized by IR, 1H NMR and single-crystal X-ray diffraction. The crystal of the title compound belongs to monoclinic, space group P21 /c with a=10.0081(3), b=14.5312(4), c=7.8739(2) , β=99.425(3)°, Z=4, V=1129.64(5)3 , Dc=1.425 g/cm3 , μ=0.269 mm-1 , F(000)=504, the final R=0.0519 and wR=0.1507. X-ray analysis indicated that the five-membered ring is essentially planar in this molecule, and intermolecular hydrogen bonds N(1)-H(1)…N(2), C(3)-H(3)…O(1), C(4)-H(4)…O(1) and C(12)-H(12a)…O(1) were observed. π-π Stacking interactions contribute to the stability of the structure. DSC-TG analysis showed that the title compound experienced a phase change at 190 ℃ and began to decompose above 240 ℃.     

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 （5-Hydroxy-6-methoxybenzofuran- 3-yl）-（4-methoxyphenyl）methanone

Compound 1 (5-hydroxy-6-methoxybenzofuran-3-yl)(4-methoxyphenyl)methanone, C17H14O5 , as a potential anti-breast cancer agent has been synthesized under microwave irradiation, which was further converted to (5,6-dihydroxybenzofuran-3-yl)(4-methoxyphenyl)methanone (2). The compounds were characterized by MS and NMR spectra. Meanwhile, the crystal of 1 was obtained and determined by X-ray single-crystal diffraction. Crystal data: monoclinic system, space group P21/n, a=8.908(6), b=10.505(7), c=15.452(11), β=105.043(9)°, V=1396.4(16)3 , Z=4, F(000)=624, Dc=1.419 g/cm3 , μ=0.105 mm1, R=0.0513 and wR=0.1246 for 14459 independent reflections (Rint=0.0647) and 2488 observed ones (I>2σ(I)). Intermolecular O-H···O and π-π stacking interactions contributed to the stability of the structure.     

Synthesis,Crystal Structure and Spectroscopic Properties of Zn(Ⅱ) with N-carbamylglutamate Ligand

Zn C6H8N2O5.H2O(NCGZn) has been synthesized, and its functional groups present in the title compound were confirmed by elemental analysis, TG and IR spectral studies. Meanwhile, the crystal of NCGZn was obtained by slow evaporation of a saturated aqueous solution at room temperature and confirmed by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P21 with a = 5.03220(1), b = 13.3747(4), c = 12.9944(4) , β = 92.987(2)o, V = 873.39(4) 3, Z = 2, C12H20N4O12Zn2, Mr = 543.10, Dc = 2.065 g/cm3, F(000) = 552, μ(Mo Ka) = 2.826 mm-1, R = 0.0422 and w R = 0.1142. In NCGZn, Zn(1) and the symmetry formed Zn(1) ions are connected by five atoms from four NCG-2H anions and a water molecule. A NCG ligand has two carboxylate groups, one connecting a Zn ion, and the other bridgiong two Zn ions. The NCG ligand bridges four Zn ions through the amino group and two carboxylate groups with a water molecule to yield a 3D coordination polymer structure with hydrogen bonds.     

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

ＮｅｕｔｒｏｎＤｉｆｆｒａｃｔｉｏｎＳｔｕｄｙｏｎＳｔｒｕｃｔｕｒｅｏｆα－ＬｉＩＯ_３ＳｉｎｇｌｅＣｒｙｓｔａｌｕｎｄｅｒＤＣＶｏｌｔａｇｅＣｈｅｎｇＹｕ－Ｆｅｎ；ＹａｎｇＺｈｅｎ；ＣｈｅｎｇＺｈｉ－Ｘｕ；ＧｕｏＬｉ－Ｐｉｎｇ（ＣｈｉｎａＩｎｓｔｉ?..     

Synthesis, Structure and Transesterification of the Derivatives of β-Alkoxycarbonylethyltin Trichlorides with Diethyldithiocarbamate

o-Alkoxycarbonylethyltintrichlorides,RoCOCH2CH,SnCl,l,anovelmpeofmono-organotincompoundscontainingestergroup,havereceivedconsiderableattentionsinceHuttonetalreportedtheirSynthesis"'.Theirspectr8ldareshowedthatthecentCrtinatomwaspenta-coordinatedwithintramolecularestCrcarbonyloxygentotincoordinationandtheintramolecularcoordinationcanbebrokenbyextemalbidentatedonor,suchas2,2'-bipyridyI,l,1o-phenanthroline,etc.'-'.TheaddqctSoflwithneutraldonor,forexample,dimethylsulfoxide,hexamethylphosphor…     

Isolation and Crystal Structure of 3β-acetoxy-20 （29）-lupen-28-aldehyde from the Bark of Platanus Acerifolia Willd

The title compound,3β-acetoxy-20(29)-lupen-28-aldehyde,is a pentacyclic triterpene which was first isolated from the acetyl acetate fraction of Platanus acerifolia Willd bark and characterized by 1 H-NMR and 13 C-NMR.Besides,the crystal of the compound was acquired,and the relative configuration of 3β-acetoxy-20(29)-lupen-28-aldehyde was determined by single-crystal X-ray diffraction analysis for the first time.It crystallizes in the monoclinic system,space group C2 with a=14.428(3),b=6.6620(13),c=30.399(6),β=103.73(3)°,Z=4,C32 H50 O3,M r=482.72,Dc =1.130 g/cm 3,V=2838.5(10)3,μ(MoKa)=0.070 mm-1,F(000)= 1064,the final R=0.0657 and wR=0.1855 for 2839 independent reflections (R int=0.0802)and 1963 observed ones (I>2(I)).Intramolecular van der waals force contributes to the stability of the 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 a β-Lactam Derivative of 2,4-Diaryl-1,5-Benzothiazepine

１ＩＮＴＲＯＤＵＣＴＩＯＮ１,５ ｂｅｎｚｏｔｈｉａｚｅｐｉｎｅｓｐｏｓｅｓｐｏｔｅｎｔｉａｌｂｉｏｌｏｇｉｃａｌａｃｔｉｖｉｔｉｅｓ〔１〕．ＣｙｃｌｏａｄｄｉｔｉｏｎｒｅａｃｔｉｏｎｓａｔｔｈｅｉｒＣ＝Ｎｄｏｕｂｌｅｂｏｎｄｈａｖｅａｒｏｕｓｅｄｃ...     

Synthesis and Crystal Structure of Bis(cyclopentadienyl) Ytterbium Complex Supported by β-Diketiminate

1 INTRODUCTION Recent efforts in the design and synthesis of new ligand systems for lanthanide chemistry have been aimed at extending organolanthanide chemistry in the application of nitrogen-containing bidentate an- cillary ligands, such as β-diketiminates, guanidinates and amidinates, etc. A major impetus for such studi- es can be traced to the well known applications of lanthanide complexes in homogeneous catalysis[1, 2]. Recently, we have been interested in understanding the chemist…     

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.     

Syntheses and Crystal Structures of Pyridyl Substituted Dibenzo[b,e]-[1,4]diazepin-1-one Derivatives

A new series °f 11-pyridyl substituted dibenz°-diazepin-1-°ne derivatives 1 was synthesized by a tw° step cycl°c°ndensati°n reacti°n. All the c°mp°unds were characterized by IR,MS, and 1H NMR. And crystals °f 1a and 1b were °btained and determined by X-ray single-crystal diffracti°n. Crystal data °f 1a: C48H52N6O7, m°n°clinic system, space gr°up C2/c, a = 28.39(4), b =9.275(12), c = 16.84(2) A, β = 104.98(3)°, V = 4284(10) A3, Z = 4, F(000) = 1752, Dc = 1.279 g/cm3,R = 0.0603, and wR = 0.1314. Crystal data °f 1b: C24H21N3 O, m°n°clinic system, space gr°up P21/c,a = 11.625(5), b = 19.055(9), c = 8.741(4) A, β = 95.547(6)°, V = 1927.2(15) A3, Z = 4, F(000) =776, Dc = 1.266 g/cm3, R = 0.0494, and wR = 0.1287.     

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 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.     

Ba2SbGaS5: Solid-state Synthesis, Crystal and Electronic Structures, and Property Characterization

Single crystal of Ba2SbGaS5 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), V = 971.4(6)3 , Z = 4, Dc = 4.284 g/cm3 , = 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∞SbGaS54- anionic chain constructed from the GaS4 tetrahedra and the SbS5 polyhedra via sharing edge alternately. The paralleled 1∞SbGaS54- anionic 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 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 Cobalt（Ⅱ） Complex

A metal-organic coordination polymer [Co2(cbba)4(bix)2]n(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,and single-crystal X-ray diffraction.Pink crystals crystallize in the monoclinic system,space group P21/n with a = 21.148(4),b = 15.728(3),c = 23.879(4) ,β = 102.148(3)°,V = 7764(2)3,C316H232Cl15Co8N32O48,Mr = 6248.53,Dc = 1.336 g/cm3,F(000) = 3207,Z = 1,μ(MoKα) = 0.621 mm-1,the final R = 0.0567 and wR = 0.1280 for 8510 observed reflections(I > 2σ(I)).The structure of 1 exhibits a one-dimensional chain-like structure.     

Synthesis and Crystal Structure of Glycin·3,5-Dihydroxybenzoic Acid

1 INTRODUCTION In the last two decades, the extended field of non-linear optical (NLO) applications (frequency conver-sion, optical parametric amplification and oscillationetc) has stimulated search for highly nonlinear opticalmaterials[1~3]. Especially, organic NLO materials arerapidly investigated due to their large nonlinear sus-ceptibility, inherent synthetic flexibility, high opticaldamage thresholds and intrinsic tailorability[4~6]. It isknown that the solution growth technique a…     

Synthesis and Crystal Structure of (Z)-N-(2-(diethylamino)ethyl)-7-(5-fluoro-2-oxoindolin-3-ylidene)-2-methyl-4,5,6,7-tetrahydro-1H-indole-3-carboxamide Methanol Solvate

The crystal structure of a new compound (Z)-N-(2-(diethylamino)ethyl)-7-(5- fluoro-2-oxoindolin-3-ylidene)-2-methyl-4,5,6,7-tetrahydro-1H-indole-3-carboxamidemethanol solvate (C24H29FN4O2CH4O, Mr = 456.55) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 14.560(3), b = 7.3200(2), c = 22.233(4) , β = 101.78(3)°, V = 2319.7(8) 3 , Z = 4, Dc = 1.307 g/cm 3 , F(000) = 976, μ = 0.092 mm -1 , MoKa radiation (λ = 0.71073), R = 0.0604 and wR = 0.1644 for 4262 observed reflections with I > 2 (I). X-ray diffraction analysis reveals that the indole and pyrrole are almost coplanar. Intramolecular C-H···O and N-H···O hydrogen bonds together with π-π interactions are found in the structure.     

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.