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 a Degraded Dehydroabietylamine Thiophene Imine

A degraded dehydroabietylamine thiophene imine （C24H30NS, Mr = 364.55） has been synthesized from dehydroabietic acid, and its structure was characterized by IR, IH NMR spectroscopy and single-crystal X-ray diffraction. White crystals of the title compound crystallize in the monoclinic system, space group P21 with a = 5.9490（12）, b = 16.337（3）, c = 10.780（2）A, β = 92.21（3）°, V = 1046.9（3）A^3, Z = 2, Dc = 1.156 g/cm^3, λ= 0.71073A,μ = 0.162 mm^-1, F（000） = 394, the final R = 0.0443 and wR = 0.0805 for 1325 observed reflections with I 〉 2σ（I）. The imine group was directly attached to the chiral carbon atom of tricyclo hydrophenthenrane structure with a trans configuration. The dihedral angle between two aromatic rings is 88.3°.     

Synthesis,Crystal Structure and Antibacterial Activity of （2E,3E）-N1,N2-Bis（2,3,4-trimethoxy-6-methylbenzylidene）ethane-1,2-diamine

The title compound （2E,3E）-N1,N2-bis（2,3,4-trimethoxy-6-methylbenzylidene）- ethane-l,2-diamine （C24H32N2O6, Mr = 444.52） was synthesized and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P2/c, with a = 8.5480（10）, b = 9.3710（12）, c = 15.280（2）A, β = 90.780（2）°, V= 1223.9（3）A3, Z = 2, Dc= 1.206 g/cm3, 2 = 0.71073A,μ（MoKa） = 0.087 mm^-1, F（000） = 476, the final R = 0.0680 and wR = 0.1450 for 2144 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals that the molecule adopts an E configuration about the central C=N functional bond. The phenyl rings of two 2,3,4-trimethoxy-6-methylbenzaldehyde groups are symmetrically parallel. The molecules are linked through C-H…O hydrogen bonding interactions. The title compound possesses moderate antibacterial activity.     

Hydrothermal Synthesis and Crystal Structure of a Novel Binuclear Cd（ Ⅱ ） Coordination Polymer Based on 1,2-Benzenedicarboxylate and Imidazole

The hydrothermal reaction of Cd（OAc）2.H2O with 1,2-benzenedicarboxylate （1,2-BDC）, imidazole and H2O resulted in the formation of a binuclear polymeric Cd（ Ⅱ ） complex {[Cd2（1,2-BDC）2（Im）4].（H2O）}n which was then characterized by elemental analyses and single-crystal X-ray diffraction analysis. The crystal is of monoclinic system, space group P21/c with a = 14.6455（3）, b = 9.3530（2）, c = 23.7838（5）A, β= 106.6290（10）°, Cl12H104CdgN32O36, Mr = 3373.47, V = 3121.64（11）A^3, Dc = 1.795 g/cm^3, F（000） = 1672,μ= 1.428 cm^-1 and Z = 1. The final R = 0.0316 and wR = 0.0687 for 5045 reflections with I 〉 2σ（I）. In the title complex, the two Cd（ Ⅱ） ions are in different coordination environments with distorted octahedral and pengonal bipyramidal geometries, respectively. Two Cd polyhedra are linked together through one μ2-η^1：η^1 and one μ2-η^1：η^1 carboxylate groups from different 1,2-BDC ligands, giving rise to a binuclear Cd（ Ⅱ ） cluster, and such clusters are connected by bridged 1,2-BDC ligands to form a 2-D structure along the c axis. The inter- and intermolecular hydrogen bonds further connect the 2-D structures into a 3-D supramolecular network.     

Synthesis and Crystal Structure of 2,6-Bis（benzimidazo（1,2-c）- quinazolin-6-yl）pyridine Tetrahydrate

The title compound, 2,6-bis（benzimidazo（1,2-c）quinazolin-6-yl）pyridine tetrahydrate, was synthesized by simple condensation of 2-（2-sminophenyl） benzimidazole with pyfidine- 2,6-dicarboxylic acid and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group C2/c with a = 22.226（8）, b = 16.730（7）, c = 16.820（5）A, β = 115.796（13）°, V = 5631（4）A^3, C33H27NTO4, Mr = 585.62, Z = 8, Dc = 1.381 g/cm^3, λ（MoKα） = 0.71073 A, F（000） = 2448 and μ = 0.09 mm^-1. The structure was refined to the final R = 0.0730 and wR = 0.1573 for 6346 independent reflections （Rint = 0.0801） and 3384 observed reflections （I 〉 2σ（I））. In the crystal, the molecules are linked through intermolecular O-H…O and O-H…N hydrogen bonds. Intermolecular π-π interactions （with distances of about 3.45 A） are pronounced in the crystal structure.     

Synthesis,Crystal Structure and Biological Activities of N-（4-Cyanopyrazole-3-yl）- α-（3,5-difluorophenyl）- O,O-diisopropyl- α-aminophosphonate

The title compound has been synthesized by the addition reaction of N-（4-cyanopyrazole-3-yl）-3,5-difluorophenyl-imine and diisopropyl phosphate. Its structure was confirmed by means of IR, ^1H NMR and elemental analysis. The single-crystal structure of the title compound was determined by X-ray crystallography. The compound crystallizes in monoclinic, space group C2/c with a = 18.9959（14）, b = 9.2212（7）, c = 22.1108（16）A^°, β= 90.1540（10）°, V = 3873.0（5） A^°^3, Dc = 1.366 g/cm^3, Z = 8, μ = 0.185, F（000） = 1664, and the final R = 0.0503 and wR = 0.1539 for 2996 observed reflections （I 〉 2σ（I））. The results demonstrate that the dihedral angle between the pyrazole and benzene rings is 105.5°, and there is a full delocalized pyrazole system with sp^2 hydridization of N（3）. The crystal structure is stabilized by two intermolecular hydrogen bonds of N（1）-H（1）…O（3） and N（3）-H（3A）…N（4）. The preliminary biological test shows that the title compound has a moderate antifungal activity.     

Metallotricycle of Lanthanide Supported by a Bridging Diamide: Syntheses and Molecular Structures of {Li(THF)3[LnCl(μ2-trans-1,2-(NSiMe3)2C6H10)(μ2-Cl)]}2•2THF (Ln＝Yb, Nd)

The reactions of dilithium salt of trans-1,2-bis（trimethylsilylamino）cyclohexane with anhydrous lanthanide trichlorides LnCl3 （Ln = Yb, Nd） in THF afforded the dianionic binuclear tricycles of lanthanide chlorides {Li（THF）3[LnCl（μ2-trans-1,2-（NSiMe3）2C6H10）（μ2-Cl）]}2·2THF （Ln=Yb 1, Nd 2） in moderate yields. Both of the bridged complexes were characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction. Crystal structural analysis shows that the two complexes are the analogues which have a tricyclic framework built by two bridged lanthanide metals, four nitrogens and four carbons from two diamide ligands. Each lanthanide metal coordinates to three nitrogen atoms and two chlorines to form a distorted trigonal bipyramid and connects with a lithium by a bridging chlorine.     

Crystal Structure, Photoluminescence and Theoretical Studies of Diethyl 4,5-di（thienyl）- 3,6-bis（trimethylsilyl）phthalate

The crystal structure of the title compound, diethyl 4,5-di（thienyl）-3,6-bis（trime- thylsilyl）phthalate （C26H3404S2Si2, Mr = 530.83）, has been determined by single-crystal X-ray diffraction. The crystal belongs to the orthorhombic system, space group Pccn with a = 43.008（5）, b = 10.9000（12）, c = 11.9357（14） A, V= 5595.3（11） A3, Z = 8, F（000） = 2256, Dc= 1.260 mg/m3, p = 0.305 mm-1, T = 113（2） K, S = 1.090, R = 0.0413 and wR = 0.0969 for 5952 observed reflections with 1 〉 2o（/）. The benzene ring system is planar and makes dihedral angles of 63.7（2） and 72.5（4） with the two thienyl rings A （C（23）-C（26）, S（2）） and B （C（19）-C（22）, S（1））, respectively. The UV-vis absorption and fluorescence of the title compound were discussed. The molecular structure of the title compound has been optimized using DFT method at the B3LYP/6-31G（d） level. The computational results showed that the optimized geometer parameters are consistent well with the experiment data. The vertical ionization potential, vertical electron affinity and frontier orbitals were also discussed.     

Synthesis and Structural Characterization of 1,4-Di（2-methoxyphenyl）-2,5-piperazinedione

A new derivative of 2,5-piperazinedione, 1,4-di（2-methoxyphenyl）-2,5-piperazinedione （I）, was synthesized by the cyclocondensation reaction of N-2-methoxyphenyl chloroacetamide, and its structure was characterized by elemental analysis, IR, ^1H NMR and single crystal X-ray diffraction method. The crystal belongs to monoclinic system, space group P21/c with unit cell dimensions a=0.56934（10） nm, b=1.3880（2） nm, c=1.00329（17） nm, β= 90.376（3）°, V= 0.7928（2） nm^3, Z=2, Dc = 1.367 g·cm^-3,μ = 0.98 cm^-1, R and wR being 0.0606 and 0.1564 respectively for 1549 unique reflections with 1247 observed reflections [I〉2σ（I）]. The molecule has a crystallographically imposed symmetry center. The three rings in the molecule are each coplanar with their attached groups, excluding methyl H atoms and the H atoms attached to the piperazinedione ring, while the whole molecule is not planar, with dihedral angles of 74.7（1）° between the piperazinedione and each of the two aromatic rings. The crystal structure is stabilized by van der Waals and dipole-dipole forces.     

Synthesis,Crystal Structure and Antibacterial Activity of （E）-N1,N4-Bis（2,3,4-trimethoxy-6- methylbenzylidene）butane- 1,4-diamine

The title compound （E）-N1,N4-bis（2,3,4-trimethoxy-6-methylbenzylidene） butane- 1,4- diamine （C26H36N2O6, Mr = 472.57） was synthesized and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to triclinic, space group C2/c with a = 36.102（4）, b = 5.6620（11）, c = 13.015（2）A,β = 105.491 （2）°, V = 2563.7（7）A3, Z = 4, Dc = 1.224 g/cm3, 2 = 0.71073 A,μ（MoKα） = 0.087 mm^-1, F（000） = 1016, the final R = 0.0456 and wR = 0.1257 for 2255 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals that the molecule adopts an E configuration about the central C=N functional bond. The phenyl rings of two 2,3,4-trimethoxy-6-methylbenzaldehyde groups are parallel by symmetry. The molecules are linked through π-π and C-H…π stacking interactions and C-H…O hydrogen bonding interactions. The title compound possesses moderate antibacterial activity.     

Synthesis and Crystal Structure of Cluster [C6H4-1,2-(CO2CH2C2H-μ)2][Co2(CO)6]2

The reaction of dipropargyl phthalate C6H4-1,2-(CO2CH2C2H-μ)2 1 with octacarbonyldicobalt 2 resulted in the formation of red complex [C6H4-1,2-(CO2CH2C2H-μ)2][Co2(CO)6]2 3, in which each Co2(CO)6 group coordinates to one of the two C≡C bonds of 1. Molecular structure of complex 3 was determined by single crystal X-ray analyses. The crystal belongs to the monoclinic system, space group P21/a with the following crystallographic parameters: a=8.521(2), b=29.143(6), c=12.918(7)(A), β= 100.12(3)°, V=3158(2)(A)3, Z=4, Mr=814.09, Dc=1.712 g.cm-3, F(000)=1608, μ(Mo-Kα)=21.37 cm-1 and final R=0.044 for 3151 observations.     

Synthesis and Crystal Structure of (1R,2S,3S,4S)-(6-O-Acetyl-1,2-O-isoproplidene-3,5-dideoxy-α-D-glucofuranoso)-1,3,5-trihydro-2,3-oxathiaindene-2,2-dioxide

(1R,2S,3S,4S)-(6-O-Acetyl-1,2-O-isoproplidene-3,5-dideoxy-α-D-glucofuranoso)-1,3,5-trihydro-2,3-oxathiaindene-2,2-dioxide(C11H16O8S,Mr=308.30) was synthesized and structurally characterized by NMR,MS and single-crystal X-ray diffraction.It belongs to the triclinic system,space group P1 with a=7.0836(14),b=10.832(2),c=14.895(3),α=96.01(3),β=98.85(3),γ=108.59(3)o,V=1055.8(4)3,Z=3,Dc=1.455g/cm3,F(000)=486,μ=0.264mm-1,the final R=0.0360 and wR=0.0712.It is a tricyclic sultone derivative composed of three five-membered rings.     

Synthesis and Crystal Structure of 1,2-Bis-（p-nitrophenylsulfonamido）-4,5-dinitrobenzene

The title compound, 1,2-bis-(p-nitro-phenylsulfonamido)-4,5-dinitrobenzene, was synthesized and characterized by elemental analysis, IR and 1H NMR. A pale yellow prism crystal of C23H26N8O13S2 (Mr = 686.64) was obtained in DMF solution and determined by single-crystal X-ray diffraction method. It crystallizes in triclinic system, space group P1 with a = 10.346(4), b = 12.210(5), c = 12.976(5) , α = 108.220(8), β = 99.482(4), γ = 95.490(4)°, V = 1516.7(10) 3, Z = 2, Dc = 1.504 g/cm3, F(000) = 712, μ = 0.254, Mr = 686.64, the final R = 0.0561 and wR = 0.1487. One sulfonamido group of the title compound is deprotoned and forms N(3)=C(13). The crystal involves N,N-dimethylamine from the decomposition of DMF and the proton is transferred to N,N- dimethylamine. It is a strong proof for the characterization of deprotoned recognition compound by X-ray single-crystal structure.     

基于双咪唑配体的一维银配位聚合物的合成、晶体结构和表征

通过水热法合成了1个一维配位聚合物[Ag(1,2-bix)].HL,并对该化合物进行了元素分析、红外和单晶X-射线表征(1,2-bix=1,2-(二亚甲基苯)二咪唑配体,HL=反式-4,4′-二羧基偶氮苯阴离子)。该化合物属于三斜晶系,空间群P1,晶胞参数a=0.937 80(5)nm,b=1.119 91(16)nm,c=1.356 36(10)nm,α=102.923(8)°,β=91.751(5)°,γ=110.792(10)°,V=1.288 5(2)nm3,Z=2,C28H23AgN6O4,Mr=615.39,Dc=1.586 g.cm-3,F(000)=624,μ(Mo Kα)=0.829 mm-1,R=0.040 7,wR=0.102 0。在该化合物中,双咪唑配体连接着中心的Ag(Ⅰ)原子形成了一维链状结构。二羧酸配体之间通过O-H…O键形成另一种一维链状结构,两种类型的链以相互垂直的方式延伸。此外,我们还仔细研究了该化合物的荧光性质。     

Synthesis and Crystal Structure of 2,5-Dimorpholinyl-3,4-di(p-chlorophenyl)thiophene

1 INTRODUCTION a-thiobenzoylthioformamides were syn- thesized in 1980[1,2]; however, there is no report concerning the properties and reaction activities of these compounds[3]. According to literature, three-valenced phosphorus reagent is easy to react with thiirane[4] and thiocarbonyl compounds[5] to form C=C double bond. Recently, we have reported the reaction of a-thiobenzoylthioformmorpholine with trimethyl phosphite in dry diethyl ether at room temperature[6], but the product wa…     

Syntheses, Structures, and Some Properties of Three Vanadium Selenites

Three novel vanadium selenites with the formulae [（VO2）（1,10-phenanthtoline）（SeO3H）]2 1, [（VO2）（2,2′-bipyridine）]2（SeO3） 2 and [（VO）（H2O）（SeO3）2]2（HaEDD） 3 （EDD = N1,N1′-（ethane-1,2-diyl）diethane-1,2-diamine） were hydrothermally synthesized, and characterized with elemental analysis, FT-IR spectrum, Raman spectrum, TG-DTA analysis, EPR spectra, and single-crystal X-ray diffraction analysis. Compound I belongs to the triclinic system, space group P1^- with a = 7.7527（5）, b = 9.5345（10）, c = 9.8192（8） A^°, α = 92.712（3）, β = 105.540（3）, γ = 108.154（4）°, V = 657.66（1） A^°^3, Mr = 782.22, Z = 1, F（000） = 384,μ（MoKa） = 3.544 mm^-1, R = 0.0432 and wR = 0.1142; Compound 2 is of orthorhombic system, space group F212121 with a = 7.6574（15）, b = 14.916（3）, c = 19.085（4） A, V = 2179.8（8） Aa, Mr = 605.21, Z = 4, F（000） = 1200, μ（MoKa） = 2.579 mm^-1, R = 0.0338 and wR = 0.0658; Compound 3 belongs to the triclinic system, space group P1^- with a = 9.247（2）, b = 9.659（2）, c = 7.2651（19） A^°, α = 98.171（7）, β = 103.709（5）, γ = 114.712（13）°, V = 550.9（2） A^°^3, Mr = 828.03, Z = 1, F（000） = 400, μ（MoKa） = 7.537 mm^-1, R = 0.0641 and wR = 0.2118. Compound 1 is constructed from alternating corner-shared [VO4N2] octahedra and SeO3H units, forming a dimeric vanadium unit. These assemblies are further linked into an infinite chain via hydrogen bonds along the a axis. In the structure of 2, two distinct V centers form centrosymmetric [V2O6N4] clusters through edge-sharing, and the SeO3 unit serves as a capping unit to fix the oxovanadate cluster. In the structure of 3, each [VO6] octahedron shares four oxygen atoms with adjacent Se atoms, while every SeO3 unit shares two oxygen atoms with neighboring V atoms. This connectivity of alternating VO6 and SeO3 units results in a joint-like chain. Based on the TGA analysis, these three compounds are thermally stable under 200℃ .     

Crystal and Molecular Structure of 5，6，7，8，9，10－Hexahydro－3－（4－methylphenylamino）－2－thioxoquinoxaline

ＣｒｙｓｔａｌａｎｄＭｏｌｅｃｕｌａｒＳｔｒｕｃｔｕｒｅｏｆ５，６，７，８，９，１０－Ｈｅｘａｈｙｄｒｏ－３－（４－ｍｅｔｈｙｌｐｈｅｎｙｌａｍｉｎｏ）－２－ｔｈｉｏｘｏｑｕｉｎｏｘａｌｉｎｅＳｕｎＤａ－Ｑｉｎｇ；ＬａｎｇＪｉａｎ－Ｐｉｎｇ；ＬｕＺｈ...     

Crystal Structure of 1，2：5，6－Di－O－isopropylidene－α－D－glucofuranosyl N，N－bis（2－chloroethyl） Phosphordiamidate

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ１，２：５，６－Ｄｉ－Ｏ－ｉｓｏｐｒｏｐｙｌｉｄｅｎｅ－α－Ｄ－ｇｌｕｃｏｆｕｒａｎｏｓｙｌＮ，Ｎ－ｂｉｓ（２－ｃｈｌｏｒｏｅｔｈｙｌ）ＰｈｏｓｐｈｏｒｄｉａｍｉｄａｔｅＣｈｅｎＲｕ－Ｙｕ；ＣｈｅｎＸｉａｏ－Ｒｕ（...     

Metal-oxygen-metal arrays in lamellar hybrid materials: cobalt and manganese 4-cyclohexene-1,2-dicarboxylates

We have obtained three layered hybrid materials from the hydrothermal reaction of 4-cyclohexene-1,2-dicarboxylic acid with Co and Mn salts: Co(C(8)H(8)O(4))[1], Mn(H(2)O)(C(8)H(8)O(4))[2], and Mn(4)(H(2)O)(C(8)H(8)O(4))(4).0.3(H(2)O)[3]. The structures for all materials were solved by single-crystal XRD ([1]P1, a=4.805(2) A, b=6.650(3) A, c=12.960(6) A, alpha=98.285(7) degrees, beta=98.986(7) degrees, gamma=95.689(7) degrees, V= 401.6(3) A(3), R(1)= 0.0438; [2] P2(1)/c, a=11.151(2) A, b=11.330(2) A, c=7.6560(15) A, beta=108.813(3) degrees , V=915.6(3) A(3), R(1)=0.0412; [3] P1, a= 11.412(3) A, b=12.136(4) A, c=13.809(4) A, alpha=104.703(6) degrees, beta=103.207(6) degrees, gamma=92.468(5) degrees, V=1790.6(9) A(3), R(1)=0.1056). While all three structures are two-dimensional overall, the metal-oxygen-metal dimensionality within the layers varies from isolated metal atoms in the case of [1] to 1D ribbons of vertex sharing MnO(6) octahedra [2] and 2D arrays of edge- and vertex-sharing polyhedra in [3].