Synthesis and Crystal Structure of 7-Acetamido-5-chloro-8-（p-methyl- oxybenzenesulfonyloxy）-2-styrylquinoline

The title compound 7-acetamido-5-chloro-8-(p-methyloxybenzenesulfonyloxy)-2- styrylquinoline 4 (C26H21ClN2O5S, Mr = 508.96) has been synthesized and characterized by 1H- NMR, IR, ESI-MS and single-crystal X-ray diffraction techniques. The crystal belongs to orthorhombic, space group Pca21, with a = 7.920(3), b = 10.672(5), c = 28.008(12) , V = 2367.3(17) 3, Z = 4, Dc = 1.425 g/cm3, μ = 0.290 mm-1, F(000) = 1056, R = 0.0323 and wR = 0.0692 for 3895 unique reflections with 3127 observed ones (I > 2σ(I)). X-ray analysis reveals that the styrylquinoline subunit adopts a coplanar conformation, where the benzene ring and quinoline are in trans configuration.     

Synthesis,Crystal Structure,and Antitumor Activity of 1-（4-Methoxybenzylidene）-2-（1-phenyl-6-trifluoromethyl- 1H-pyrazolo [3,4-d] pyrimidin-4-yl）hydrazine Monohydrate

The novel title compound 1-(4-methoxybenzylidene)-2-(1-phenyl-6-trifluoromethyl-1H-pyrazolo[3,4-d]pyrimidin-4-yl)hydrazine monohydrate(C20H15F3N6O·H2O, Mr = 430.40) has been synthesized by a four-step procedure including the cyclization, chlorination, hydrazinolysis and condensation reaction, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to orthorhombic, space group Pbca with a = 8.3779(13), b = 17.607(3), c = 26.774(4) , V = 3949.2(11) 3, Z = 8, Dc = 1.448 g/cm3, μ = 0.117 mm–1, F(000) = 1776, the final R = 0.0553 and wR = 0.1516 for 2354 observed reflections with I 2■(I). X-ray diffraction analysis reveals that the title compound is almost coplanar except for the trifluoromethyl and phenyl moieties. In the crystal packing, the molecules are linked by intermolecular O(1W)–H(1WA)···N(2), O(1W)–H(1WA)···N(4) and N(5)–H(5A)···O(1W) hydrogen bonds via water molecules and stacked through π-π stacking interactions. The preliminary bioassay suggested that the title compound exhibits relatively good antitumor activity against HepG2 and BCG-823.     

Structures of 1-（3,4-Dihydroxyphenyl）-2-（3,4-dimethoxyphenyl） ethanone and Its Hydrate Complex

The title compounds, C16H16O5 (I) and C16H16O5·H2O (II), were structurally characterized by single-crystal X-ray diffraction. Compound I crystallizes in monoclinic space group P21/c with a = 10.5574(10), b = 8.3576(9), c = 16.5528(16) , β = 91.762(3)°, Z = 4, R = 0.0524 and wR = 0.1084. The molecules are jointed into a chain by intermolecular O-H···O and C-H···O hydrogen bonds, which form layers parallel to (001). The chains run along the [110] and [110] directions alternatively layer by layer, and are assembled into a network by intermolecular O-H···O (carboxyl) hydrogen bonds. On the other hand, the hydrate complex (II) crystallizes in the triclinic space group P1 with a = 5.1451(2), b = 10.4583(4), c = 14.8267(5) , α = 70.900(2), β = 82.478(2), γ = 81.359(2)°, Z = 2, R = 0.0393 and wR = 0.0983. The molecules are linked into infinite two-dimensional ribbons by O-H···O (carbonyl) and solvent-bridged O-H···O hydrogen bonds.     

Synthesis and Crystal Structure of a New Tetracopper Complex [Cu(H_2O)_3Cu(HCDTA)]_2(ClO_4)_2·H_2O

A new tetracopper complex [Cu(H2O)3Cu(HCDTA)]2(ClO4)2·H2O (CDTA = transcyclohexane-1,2-diamine-N,N,N′,N′-tetraacetate) has been prepared and characterized by singlecrystal X-ray diffraction analysis. The crystal adopts space group C2/c with a = 16.990(10), b = 9.150(5), c = 29.318(17) , β = 104.289(9)°, V = 4417(4) 3, Z = 4, C28H52Cl2Cu4N4O31, Mr = 1265.80, Dc = 1.904 g/cm3, μ = 2.130 mm-1, F(000) = 2584, T = 293(2) K, the final R = 0.0328 and wR = 0.0809 for 4938 observed reflections (I 2σ(I)). The tetracopper units are interconnected by weak covalent bonds into a layered structure.     

Extraction and Absolute Crystal Structure of Stachyose

The title compound stachyose(C24H42O21),a biologicaly active tetrasaccharide,was characterized by X-ray diffraction analysis.It crystallizes in the orthorhombic system,space group P21212 with C24H42O21,a = 23.8760(3),b = 12.71028(12),c = 10.81279(11) ,V = 3281.36(6) 3,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 β-D-fructofuranosyl α-D-galactopyranosyl-(1→6)-α-D-galactopyranosyl-(1→6)-α-D-glucopyranoside.The molecule is composed of two α-D-galactoses,one α-D-glucose,and one β-D-fructose and sequentially linked as α-Gal(1→6) α-Gal(1→6) α-Glc(1→2) β-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.     

Syntheses,Crystal Structures and Properties of Three New Complexes [Ni（C9N2O2H7）2（CH3OH）2],[Zn（C9N2O2H7）2（H2O）2] and [Cd（C9N2O2H7）2（CH3OH）2]

Three novel metal-organic complexes with formulas [Ni(C9N2O2H7)2(CH3OH)2](1),[Zn(C9N2O2H7)2(H2O)2](2) and [Cd(C9N2O2H7)2(CH3OH)2](3) were synthesized by the reactions of Ni,Zn and Cd salts with ethyl 2-benzimidazolylacetate under hydrothermal conditions or layering technique,and characterized by single-crystal X-ray diffraction analysis,IR spec-troscopy,solid-state luminescent properties and thermogravimetric(TG) analysis.The crystal data for these three complexes are as follows:for 1,monoclinic,space group P21/c,a = 9.384(3),b = 9.634(3),c = 11.292(3) ,β = 95.787(5)°,V = 1015.7(5) 3,Z = 2,F(000) = 492,Dc = 1.547 Kg/m3,μ = 1.002 mm-1,the final R = 0.0451 and wR = 0.0900 for 1833 observed reflections with Ⅰ 2σ(Ⅰ);for 2,orthorhombic,space group Pbca,a = 10.031(4),b = 10.379(4),c = 17.525(7),V = 1824.6(12) 3,Z = 4,F(000) = 928,Dc = 1.645 Kg/m3,μ = 1.392 mm-1,the final R = 0.0452 and wR = 0.0996 for 1661 observed reflections with Ⅰ 2σ(Ⅰ);for 3,monoclinic,space group P21/c,a = 9.9114(13),b =10.4852(15),c = 10.4120(14) ,β = 108.453(5)°,V = 1026.4(2) 3,Z = 2,F(000) = 532,Dc = 1.705 Kg/m3,μ = 1.110 mm-1,the final R = 0.0322 and wR = 0.0805 for 1822 observed reflections with Ⅰ 2σ(Ⅰ).In the three complexes,the ethyl 2-benzimidazolylacetate shows the same chelating mode,and the adjacent units are interlinked into a two-dimensional layer through hydrogen-bonds(O-H···O,N-H···O).     

Synthesis and Structural Characterization of One New Polyoxotungstate Connected via Potassium Cations with a Three-dimensional Framework: H6Na2K4(H2W12O42)Cl2·14H2O

One new polyoxotungstate complex H6Na2K4(H2W12O42)Cl2·14H2O 1 has been prepared in the beaker solution and characterized by elemental analysis and IR spectroscopy. Crystal data: H36Cl2K4W12Na2O56, Mr = 3411.77, monoclinic, space group P21/c, a = 11.5734(16), b = 14.3136(19), c = 15.459(2)(A), β = 105.601(2)°, V = 2466.5(6)(A)3, Z = 2, Dc = 4.594 g/cm3, F(000) = 3008, μ = 28.447 mm-1, R = 0.0574 and wR = 0.1239 (Ⅰ＞ 2σ(Ⅰ)). Single-crystal X-ray diffraction analysis results reveal that a three-dimensional architecture in the title compound is constructed from the H2W12O4210- units linked by potassium.     

Synthesis and Crystal Structure of a Cobalt（Ⅱ） Coordination Polymer with Benzene-1,3,5-triacetate and 1,2-Di（pyridin-4-yl）ethene

A novel coordination polymer, [Co3(bta)2(dpe)3(H2O)2]·2H2O (1, H3bta = benzene-1,3,5-triacetic acid, and dpe = 1,2-di(pyridin-4-yl)ethene), has been hydrothermally prepared and characterized by IR spectroscopy, elemental analysis and single-crystal X-ray diffraction. The crystal is of triclinic system, space group P , with a = 9.5687(15), b = 11.2470(17), c = 13.686(2) , α = 78.262(3), β = 89.271(4), γ = 81.292(3)°, V = 1425.2(4) 3, C60H56N6O16Co3, Mr = 1293.90, Dc = 1.508 g/cm3, F(000) = 667, μ = 0.940 mm-1 and Z = 1. The final R = 0.0707 and wR = 0.1413 for 4950 observed reflections (I > 2σ(I)). In the title complex, the bta ligand acts as a four-dentate bridging ligand to link up cobalt atoms into lamellar frameworks which are further interlinked by the dpe ligands to generate a trinodal (3,4,6)-connected (4.62)2(42.68.83.102)(64.82) net.     

Synthesis, Crystal Structural Characterization and Electrochemical Properties of a 1D Tape-like Polymer of Cobalt Adamantanedicarboxylate： [Co_2（adc）_2（py）_4（H_2O）]_n

The new complex, [Co2(adc)2(py)4(H2O)}n 1 (adc = 1,3-adamantanedicarboxylate, py = pyridine), has been hydrothermally synthesized as polymeric solid, and characterized by X-ray diffraction, elemental analysis, IR spectra and thermogravimetric analysis. Complex 1 crystallizes in monoclinic, space group C2/c with a = 18.932(4), b = 19.779(4), c = 12.352(3) , β = 112.03(3)o, V = 4288(2) 3, Z = 4, GOF = 0.998, R = 0.0518 and wR = 0.1074. X-ray single-crystal analysis reveals that 1 presents a 3D simple parallel rod-like supramolecular array constructed by 1D tape-like polymeric motif through aromatic π-π stacking interaction. Electrochemical investigation shows that 1 exhibits appreciable electrocatalytic activity for the reduction reaction of nitrite.     

Synthesis and Crystal Structure of a Mixed （Phthalocyaninato）（porphyrinato） Yttrium Double-decker Complex

The title compound,a mixed(phthalocyaninato)(porphyrinato) yttrium double-decker complex 1,has been synthesized and structurally characterized by X-ray single-crystal diffraction method.Crystal data:monoclinic,space group C2/c,Z = 8,C79H52Cl10N12O4Y,Mr = 1676.74,a = 38.217(3),b = 18.9867(13),c = 26.200(3) ,β = 128.0190(10)°,V = 14977(2) 3,Dc = 1.487 g/cm3,μ(MoKα) = 1.196 mm-1,F(000) = 6808,R = 0.0745 and wR = 0.2208 for observed reflections with I > 2σ(I).X-ray analysis reveals that the coordination polyhedron adopts a slightly distorted square-antiprismatic structure around the metal center.Both phthalocyanine and porphyrin ligands are saucer-shaped,with the skew angle of the two ligand planes approximately 45°.     

Eta 1 and eta 2 Coordination of 1-amino-closo-dodecaborate

The reaction of the sodium salt of 1-amino-closo-dodecaborate [Na]2[NH2-B12H11] ([Na]2[1]) with [Au(PPh3)Cl] and [Ni(THF)2(Br)2] led to eta 1(N) coordination of 1in [Na][Au(PPh3)(NH2-B12H11)] (2) and [Na]6[Ni(NH2-B12H11)4] (3), respectively. Furthermore, eta 2(N,BH) coordination of was found in [MePPh3][Rh(PPh3)2(NH2-B12H11)] (4), which was synthesized by the reaction of [MePPh3][Na][1] with [Rh(PPh3)3Cl]. All compounds were characterized by single crystal X-ray diffraction and heteronuclear NMR spectroscopy.     

A Novel 3D Extended Network Cobalt Paradodecatungstate:Synthesis,Characterization and Crystal Structure of [Co(H2O)5]2[Co(H2O)4]3[H2W12O42]·11H2O

A cobalt paradodecatungstate [Co(H2O)5]2[Co(H2O)4]3[H2W12O42]·11H2O has been successfully synthesized and structurally characterized by X-ray crystallography. Structure analysis indicates that the title compound is of monoclinic, space group P21/n, with a = 13.449(3), b =19.585(4), c = 13.990(3) (A),β = 113.79(3)°, V = 3371.8(12) (A)3, Z= 2, R= 0.0519 and wR= 0.1242.The title compound exhibits a novel 3D extended network structure constructed by interconnecting the paradodecatungstate polyanion [H2W12O42]10- clusters and cobalt11 coordination ions.     

A Novel 3D Extended Network Cobalt Paradodecatungstate:Synthesis,Characterization and Crystal Structure of [Co(H_2O)_5]_2[Co(H_2O)_4]_3[H_2W_(12)O_(42)]·11H_2O

1 INTRODUCTION Polyoxometalates are the unique metal-oxygen clusters composed of transition metals in groups V and VI (Mo, W, V, Nb, Ta) in a high oxidation state showing a large structural varieties as well as inte- resting physical and chemical properties in diverse fields including catalysis, analytical chemistry, nanotechnology, chemical sensing, biochemical and geochemical processes, medicine and materials science[1～5]. Recently, there has been increasing interest in the synthesis…     

[Cu(en)_2]~(2+)修饰的二维仲钨酸化合物:[{Na_3(H_2O)_(10)}_2H_2{Cu(en)_2(H_2W_(12)O_(42))}]·16H_2O(英文)

利用水热合成法制备了一种基于[Cu(en)2]2+修饰的仲钨酸化合物:[{Na3(H2O)10}2H2{Cu(en)2(H2W12O42)}].16H2O(en=乙二胺)(1),借助元素分析、X射线单晶衍射分析I、R、UV、热分析和X射线光电子能谱对这种化合物进行了结构和性质研究.化合物(1)属于三斜晶系,P-1空间群.晶胞参数为:a=1.183 2(5)nm,b=1.296 0(6)nm,c=1.416 9(6)nm,α=63.348 0(10)°,β=82.844 0(10)°,γ=68.907 0(10)°,V=1.810 0(14)nm3,Z=1,R1[I2σ(I)]=0.024 7,wR2[I2σ(I)]=0.058 2.化合物(1)通过仲钨酸阴离子,铜离子和[Na3(H2O)10]3+三核簇形成了新型的二维层状结构.     

Syntheses and chemistry of hypervalent cyclo-R4Sb4, cyclo-(RSbE)n[R = 2-(Me2NCH2)C6H4, E = O, S] and precursors

The cyclostibane R(4)Sb(4)(1)(R = 2-(Me(2)NCH(2))C(6)H(4)) was synthesized by reduction of RSbCl(2) with Mg in THF or with Na in liquid NH(3). The reaction of 1 with [W(CO)(5)(THF)] gives the stibinidene complex RSb[W(CO)(5)](2)(2). RSbCl(2) and (RSbCl)(2)E [E = O (6), E = S (8)] react with KOH or Na(2)S in toluene/water to give the heterocycles (RSbE)(n)[E = O, n= 3 (3); E = S, n= 2 (4)]. The chalcogeno-bridged compounds of the type (RSbCl)(2)E [E = O (6), E = S (8)] were synthesized by reaction of RSbCl(2) with KOH or Na(2)S in toluene/water, but also by reaction of RSbCl(2) with the heterocycles (RSbE)(n). The compounds (RSbI)(2)O (7) and (RSbBr)(2)S (9) were prepared via halogen-exchange reactions between (RSbCl)(2)E and NaI (E = O) or KBr (E = S) or by reactions between RSbI(2) and KOH or RSbBr(2) and Na(2)S. The reaction of cyclo-(RSbS)(2) with W(CO)(5)(THF) in THF results in trapping of the cis isomer in cyclo-(RSbS)(2)[W(CO)(5)](5). The solution behaviour of the compounds was investigated by (1)H and (13)C NMR spectroscopy. The molecular structures of compounds 1-7 and 9 were determined by single-crystal X-ray diffraction.     

A New Coordinated Transition-metal Linked Network Compound Constructed by Octamolybdate Chain

1 INTRODUCTION The polyoxometalates have aroused extensive in-terest due to their alluring topologies and potentialapplications in various fields (e.g. catalysis, biology,medicine and materials science)[1]. A variety of po-lyoxometalate anions and related fragments withoxygen-rich compositions can serve as inorganic li-gands to coordinate secondary transition metal ions(so-called heterometals, such as Cu2 , Ni2 , Co2 andMn2 )[2]. Thus, larger discrete species and infinitelyextending ar…     

Synthesis, crystal structure, and solution stability of Keggin-type heteropolytungstates (NH4)6NiII0.5[alpha-FeIIIO4W11O30NiIIO5(OH2)].nH2O, (NH4)7Zn0.5[alpha-ZnO4W11O30ZnO5(OH2)].nH2O, and (NH4)7NiII0.5[alpha-ZnO4W11O30NiIIO5(OH2)].nH2O (n approximately 18)

Reaction of acidified (pH approximately 7) sodium tungstate solutions with transition metal cations (Fe(3+), Ni(2+), Zn(2+), Co(2+)) leads to the formation of transition-metal-disubstituted Keggin-type heteropolytungstates with 3d-metal ions distributed over three different positions. A detailed investigation of the synthesis conditions confirmed that the complexes could equally be obtained using aqueous solutions of either Na(2)WO(4).2H(2)O (sodium monotungstate) at pH approximately 7, Na(6)[W(7)O(24)]. approximately 14H(2)O (sodium paratungstate A), or Na(10)[H(2)W(12)O(42)].27H(2)O (sodium paratungstate B) as starting materials. Three complexes, (NH(4))(6)Ni(II)(0.5)[alpha-Fe(III)O(4)W(11)O(30)Ni(II)O(5)(OH(2))].18H(2)O, (NH(4))(7)Zn(0.5)[alpha-ZnO(4)W(11)O(30) ZnO(5)(OH(2))].18H(2)O, and (NH(4))(7)Ni(II)(0.5)[alpha-ZnO(4)W(11)O(30)Ni(II)O(5)(OH(2))].18H(2)O were isolated in crystalline form. X-ray single-crystal structure analysis revealed that the solid-state structures of the three compounds consist of four main structural fragments, namely [MO(4)W(11)O(30)M'O(5)(OH(2))](n-) (Keggin-type, alpha-isomer) heteropolytungstates, hexaquo metal cations, [M'(OH(2))(6)](2+), ammonium-water cluster ions, [(NH(4)(+))(8)(OH(2))(12)], and additional ammonium cations and water molecules. The 3d metals occupy the central (tetrahedral, M) and the peripheral (octahedral, M') positions of the Keggin anion, as well as cationic sites (M') outside of the polyoxotungstate framework. UV-vis spectroscopy, solution ((1)H, (183)W) and solid-state ((1)H) NMR, and also chemical analysis data provided evidence that the 3d-metal-disubstituted Keggin anions do not exist in solution but are being formed only during the crystallization process. Investigations in the solid state and in solution were completed by ESR, IR, and Raman measurements.     

A novel organic-inorganic hybrid based on an 8-electron-reduced Keggin polymolybdate capped by tetrahedral, trigonal bipyramidal, and octahedral zinc: synthesis and crystal structure of (CH3NH3)(H2bipy)[Zn4(bipy)3(H2O)2MoV8MoVI4O36)(PO4)].4H2O

Hydrothermal reaction of H(3)PO(3), CH(3)NH(2), zinc(II) acetate, 4,4'-bipyridine (bipy), and (NH(4))(6)Mo(7)O(24).4H(2)O at 180 degrees C led to a novel organic-inorganic layered hybrid, [CH(3)NH(3)][H(2)bipy][Zn(4)(bipy)(3)(H(2)O)(2)Mo(V)(8)Mo(VI)O(36)(PO(4))].4H(2)O (1). Its structure was established by single-crystal X-ray diffraction. It crystallizes in the monoclinic space group P2(1)/c with cell parameters of a = 17.3032(2), b = 17.8113(3), and c = 23.4597 (4) A, beta = 106.410(1) degrees, V = 6935.6(2) A(3), and Z = 4. The structure of compound 1 features a novel 2D layer built from the 8e-reduced tetracapped Keggin [Zn(4)Mo(12)O(36)(PO(4))](3)(-) anions, which are further interconnected by bridging bipy ligands. The four zinc(II) ions are in tetrahedral, trigonal bipyramidal, and octahedral coordination geometries, respectively.     

A Porous Organic-inorganic Hybrid Compound Constructed from Polyoxovanadium Borate Anions,Dinuclear Na Sites and Metal-organic Units

A polyoxovanadium borate [Na(H2O)]2[Na(H2O)2]2[Cu(en)2][V12B18O54(OH)6]·(H3O)2·(H2O)18 1(en = ethylenediamine) has been hydrothermally synthesized and characterized by IR,two-dimensional infrared(2D IR) correlation spectroscopy with magnetic and thermal perturba-tion,thermal IR spectroscopy,thermal gravimetric analysis and single-crystal X-ray diffraction.It crystallizes in triclinic,space group P1 with a = 12.981(3),b = 13.044(3),c = 14.208(3) ,α = 63.98(3),β = 77.17(3),γ = 14.208(3)°,V = 2001.0(8) 3,Z = 1,Mr = 2518.05,Dc = 2.090 g/cm-1,F(000) = 1255.0,Mu(mm-1) = 1.756,λ(MoKα) = 0.71073 ,R = 0.0625 and wR = 0.1952.In 1,the [V12B18O54(OH)6]8-units are connected by [Cu(en)2]2+,binuclear Na(1) and Na(2) to form a three-dimensional porous framework.