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.     

Structural Studies and Photoluminescence of a Novel Mercury（Ⅱ） Complex Based on a Tris[4-（1-pyrazolyl）-phenyl]amine

A novel iodine-bridged mercury（Ⅱ） complex [Hg（L）（μ-I）（I）]2 was isolated by a reaction between HgI2 and the organic ligand tris[4-（1-pyrazolyl）phenyl]amine L, and the complex and ligand were both characterized by FT-IR spectroscopy, ^1H NMR and elemental analysis. The complex crystallizes in monoclinic space group P21/c with a = 9.579（5）, b = 27.331 （5）, c = 11.268（5） А, β= 105.624（5）°, Z = 2, Dc = 2.099 g·cm^-3 and μ= 7.620 mm^-1. The title complex C54H42Hg2I4N14 is a diplex bridged dinuclear complex consisting of two Hg（Ⅱ） ions, two ligands, two bridging I-anions, and two terminal I-anions. Universal hydrogen bonds in the complex with the partners of neighboring molecule have generated a supramolecular arrangement. Solid-state emission of the ligand and its complex have been investigated at room temperature.     

Synthesis and Crystal Structure of a One-dimensional Ladder-like Complex [Cu2（L）（dca）2]n （dca = [N（CN）2]^-, L = 1,4-Bis（3-furanyl）-2,3-diaza-1,3-butadiene）

A new Cu（I）-dicyanamide with formula [Cu2（L）（dca）2]n （dca = dicyanamide anion, L = 1,4-bis（3-furanyl）-2,3-diaza-1,3-butadiene） has been synthesized and structurally characterized. The complex crystallizes in the monoclinic system, space group P21/n with a = 9.271（2）, b = 7.7355（16）, c = 11.967（3）A,β = 102.693（3）°, V= 837.3（3）A^3, Z = 4, Mr = 223.68, Dc = 1.775 g/cm^3,μ（MoKa） = 2.567 mm^-1, F（000） = 444, R = 0.0782 and wR = 0.2582 for 951 observed reflections （I 〉 2σ（I））. Single-crystal X-ray analysis reveals that the copper atom is three-coordinated by two nitrogen atoms from two dicyanamide anions and another one from the ligand, and each copper atom is connected by two [N（CN）2] anions to form an infinite double-stranded bridge fashion leading to 1D ladder-like motifs.     

Synthesis and Crystal Structure of a Novel Hexanuclear Copper-indium Thiolate Complex [（InCl）2（OMe）（μ-OMe）2（μ3-OMe）（μ-SPrn）2（CuPPh3）]2

A novel hexanuclear copper-indium thiolate complex, [（InCl）2（OMe）（μ-OMe）2（μ- OMe）（μ-SPrn）2（CuPPh3）]2 1, was synthesized from the reaction of NaSPrn, InCl3 and [Cu（Me- CN）a][PF6] in the presence of Ph3P and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P211n with a = 11.3533（8）, b = 15.4939（11）, c = 20.5189（14） A, β = 98.577（2）°, V = 3569.0（4） A3, Z = 2, C56H82Cl4Cu2In4O8P2S4, Mr = 1801.56, Dc = 1.676 g/cm3,μ（MoKa） = 2.213 mm^-1, F（000） = 1796, S = 0.985, the final R = 0.0559 and wR = 0.1099 for 8878 observed reflections with I 〉 2σ（I） and 367 variables. Complex 1 consists of two CuPPh3 fragments which symmetrically side-attach to the tetranuclear core of [InaCl4（OMe）2（μ-OMe）a（μ- OMe）2（μ-SPrn）4] by coordinating with sulfur atoms of propane-thio moieties. The average In-Ot （terminal）, In-μ-O and In-μ3-O bond distances are 2.305（4）, 2.144（4） and 2.294（4） A, respectively.     

Synthesis and Structure Characterization of a Manganese（II） Complex With Eight Coordination Geometry： [Mn（OeCMe）e（phen）2]

The title compound [Mn（O2CMe）2（phen）2] （phen = 1,10-phenanthroline） 1 has been synthesized and structurally determined by single-crystal X-ray diffraction. The crystal is of orthor- hombic, space group Pbcn, with a = 12.554（4）, b = 10.168（3）, c = 17.704（5）A, V= 2259.7（12）A^3 Z = 4, C28H22MnN4O4, Mr= 533.44, Dc= 1.568 g]cm^3, F（000） = 1100, Rint = 0.0242, T= 293（2） K and p = 0.631 mm^-1. The final R = 0.0687 and wR = 0.1960 for 2046 observed reflections with I 〉 20（/）. The structure of the complex consists of one Mn（II） core coordinated by two bidentate-bound CH3COO^- groups and two η^2-phen groups forming an eight-coordinate geometrical configuration.     

Synthesis and Crystal Structure of [VO2（C17H11N3O2） ] [VO （C4H13N3）（C6H5N3O） ]（C2H5OH）

The reaction of VO（acac）2 with 2-hydroxyl-1-naphthaldehyde isonicotinyl hydrazone and amines （ethylenediamine or diethylenetriamine） in CH3OH yields crystals of novel vanadium compounds characterized by IR, NMR spectroscopic methods and X-ray single-crystal structure determination. Two different vanadium units exist in the crystal cell of [VO2（C17H11N3O2）][VO- （C4H13N3）（C6H5N3O）]（C2H5OH） which crystallizes in the triclinic system, space group P1 with a = 8.0104（17）, b = 13.898（3）, c = 14.955（3）A, α = 89.103（4）, β = 79.551（4）, γ = 78.352（4）°, V = 1603.3（6）A^3, Mr = 723.54, Dc = 1.499 g/cm^3, Z = 2, λ（MoKα） = 0.71073 ]A,μ= 0.644 mm^-1, F（000） = 748, the final R = 0.0547 and wR = 0.0997 for 8920 observed reflections with I 〉 2σ（I）. According to structure analysis, two different molecules are arranged in the lattice and the two vanadium atoms adopt octahedral and square pyramidal coordination geometries, respectively. The interactions between DNA and vanadium complexes have been investigated by UV-Vis absorption spectro- photometry.     

Solid and Solution Structural Studies of Dimeric and Tetrameric Molybdenum（VI） Malate Complexes

Reactions of potassium molybdate with racemic malic acid （H3mal = C4H6O5） result in the isolation of two mesomeric molybdenum malate complexes K8[（MoO2）2O（R-mal）2][（MoO2）2O（Smal）2]-4H2O 1 and （Him）2K6[（MoO2）4O3（R-mal）2][（MoOE）4O3（S-mal）2]-8H2O 2. Complex 1 belongs to the monoclinic system, space group C2/c with a = 14.8637（3）, b = 6.9544（1）, c = 19.6783（5）A, β = 100.081（2）°, V = 2002.70（7） A^3, Mr = 1452.88, Z = 2, F（000） = 1416, T = 173 K, Dc = 2.409 g/cm3, fl（MoKa＇） = 2.167, R = 0.0283 and wR = 0.0733.2 is of triclinic system, space group P1^- with a = 8.7707（2）, b = 9.3310（3）, c = 17.9093（7）A, α= 83.781（3）, β = 85.626（2）, y= 84.822（2）°, V = 1447.84（8）A^3, Mr = 2160.68, Z = 1, F（000） = 1048, T = 173 K, Dc = 2.478 g/cm^3,μ（MoKα） = 2.230, R = 0.0234 and wR = 0.0584.1 is the first isolated dinuclear molybdenum（VI） malato complex in 1：1 molar ratio. The molybdenum atoms in the two complexes are six-coordinated in an approximately octahedral geometry. Two malates coordinate tridentately with the Mo atom via their α-alkoxy, α-carboxy and α-carboxy groups in 1 and 2. β-Carboxy group in 2 further links with the other two Mo atoms to give a tetrameric unit. The solution ^1H and ^13C NMR spectra indicate that dimeric malate molybdenum in 1 dissociates partly in solution and exists in an equilibrium with tetrameric species, while 2 is stable and retains its tetrameric structure without any dissociation.     

Synthesis and Crystal Structure of [Cu3（dmpzm）4（μ-1, 3-dca）2（dca）4]·2H2O （dmpzm = 1,1＇-Methylenebis- （3,5-dimethyl-1H-pyrazole）, dca = dicyanamide）

The title compound, [Cu3（dmpzm）4（μ-1,3-dca）2（dca）4]·2H2O （dmpzm = 1,1＇-methylenebis（3,5-dimethyl-lH-pyrazole）, dca = dicyanamide） 1·2H2O, was synthesized via the reaction of CuCl2·2H2O with dmpzm and Na（dca）, and characterized by elemental analysis and IR spectra. 1·2H2O crystallizes in the monoclinic system, space group C2/m with a = 13.578（3）, b = 16.769（3）, c = 14.769（3） A, β = 104.10（3）° V = 3261.4（11） A^3, Z = 2, Dc = 1.466 g/cm^3, T = 153（2） K, C56H68N34O2Cu3, Mr = 1440.09, F（000） = 1490,μ（MoKa） = 1.040 mm^-1, S = 1.150, R = 0.0553 and wR = 0.1123 for 2744 observed reflections with I 〉 2σ（I）. The central copper atom is chelated by two dmpzm ligands and coordinated by two bridging dca anions, forming a slightly distorted octahedral geometry. The two external copper atoms adopt a square-pyramidal coordination geometry, coordinated by one chelating dmpzm ligand and one bridging and two terminal dca anions. Two intermolecular hydrogen bonding interactions result in the formation of a 2D （4,4） hydrogen-bonded network.     

Synthesis and Crystal Structure of a 2D Coordination Polymer： [Nd2（PDB）2（CH3COO）2（H2O）3]

A novel coordination polymer [Nd2（PDB）2（CH3COO）2（H2O）3] （H2PDB = pyridine3,4-dicarboxylic acid） has been synthesized by the reaction of Nd（CH3COO）3 with pyridine3,4-dicarboxylic acid under hydrothermal conditions. Elemental analysis, IR spectra and X-ray crystal structure analysis were carried out to determine the composition and crystal structure of the title complex which belongs to the triclinic system, space group P^-1 with a = 6.9409（14）, b = 7.5497（15）, c = 22.530（5）A, α = 84.79（3）, β = 88.15（3）, γ= 75.55（3）^o, C18H18N2O15Nd2, Mr = 790.82, Z = 2, V = 1138.5（4） A^3, Dc = 2.307 g/cm^3,μ = 4.593 mm^-1, -6≤h≤8, -5≤k ≤8, -26≤l≤ 26, F（000） = 760, Rint = 0.0298, R= 0.0314 and wR= 0.0695 （I〉 2σ（I））. Nd（1） and Nd（2） are linked into zigzag chains by carboxylate groups of acetate with interesting μ3-η^2：η^2 fashion. The zigzag chains are bridged by PDB to form a 2D framework, and a 3D supramolecular network is further constructed via π-π stacking.     

A New Complex [Ni（L）2]·2H2O Containing an Interesting Six-membered Water Ring （HL = 2-Iminomethyl-6-methoxy-phenol）

A new complex, [Ni（L）2]·2（H2O） I （HL = 2-iminomethyl-6-methoxyphenol）, has been synthesized and structurally determined. The crystal belongs to the trigonal system, space group R3- with a = 1.9341 （3）, b = 1.9341 （3）, C = 1.2048（2） nm, V = 3.9029（11） nm^3, Mr = 395.05, Z = 9, Dc = 1.513 g·cm^-3, F（000） = 1854,μ= 1.153 mm^-1 and S = 1.014. Each Ni^Ⅱ atom is four-coordinated by two N and two O atoms from two different L anions to give a slightly distorted square-plane geometry. The complex forms a 3-D network structure through N-H...O and O-H...O hydrogen bonds containing an interesting six-membered water ring.     

Synthesis and Crystal Structure of Two iso-closo 11-Vertex p-Bromobenzoate Ruthenoborane Clusters： [（PPh3）（p-BrC6H4CO2）2RUB10H8 and [（PPh3）2Ru（p-BrC6H4CO2）-（PPh3）RuB10H9]

The title clusters [（PPh3）（p-BrC6H4CO2）2RuB10H8] （1） and [（PPh3）2Ru（PPh3）（p-BrC6H4CO2）RuB10H9] （2） have been prepared and characterized by elemental analysis, FT-IR, ^1H, ^13C NMR spectra and single-crystal X-ray diffraction analysis. The clusters crystallize in monoclinic system, space group C2/c, with a =2.569（4） nm, b= 1.546（2） nm, c= 1.927（3） nm ,8=95.11（2）°, Z=8, V=7.622（21） nm^3, Dc=1.533 Mg/m^3, F（000）=3472, S= 1.009, R= 0.0418, wR=0.0775 and triclinic system, space group P-l, with a=1.3142（3） nm, b= 1.3761（3） nm, c=1.8503（4） nm, a =90.445（4）°,β=105.950（4）°, γ108.980（4）°, Z=2, V=3.0251（12） nm^3, Dc = 1.434 Mg/m^3, F（000）= 1316, S=1.007, R=0.0464, wR=0.1175, respectively for 1 and 2. In the structures, both of the dusters are based on a closo-type C2v 1： 2 ： 4 ： 2 ： 2 RUB10 stack with the metal occupying the unique six-connected apical position. In cluster 1, the metal center has three exo-polyhedral ligands： one triphenylphosphine and two dative oxygen atoms of p-bromobenzoates. The other oxygen atoms of two p-bromobenzoate are additionally bonded to B（2） and B（3） atoms respectively, resulting in two exo-cyclic five-membered Ru-O-C-O-B rings and engendering a symmetrical conformation. The cluster 2 is a bimetallic species in which the second ruthenium is bound to the {RUB10} center via one Ru-Ru bond and two {RuHμB} bridges resulting in one closo distorted exo-polyhedral Ru（1）-Ru（2）-B（3）-B（6） tetrahedron.     

Synthesis and Crystal Structure of a Cr（Ⅲ） Dimer [Cr2（8-hqn）2Cl4（H2O）2]·2（CH3）2CO （8-hqn = 8-Hydroxyoxyquinolate）

The title complex [Cr2（8-hqn）2Cl4（H2O）2]·2（CH3）2CO （8-hqn = 8-hydroxyoxyquinolate） has been synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in the triclinic system, space group P^-1 with a = 8.719（1）, b = 9.226（1）, c = 9.717（1） A^°, α = 71.916（2）, β= 78.072（2）, γ = 76.014（2）°, V= 713.72（15） A^°^3, Z= 1, Dc= 1.597g/cm^3, F（000） = 350 and μ（MoKa） = 1.177 mm^-1, the final R = 0.0490 and wR = 0.1055 for 1616 observed reflections with I 〉 2σ（I）. It is a dimer constructed by two monomeric units [Cr（8-hqn）Cl2（H2O）] bridged by phenoxide-like oxygen atom from 8-hydroxyoxyquinolate, where the two six-coordinated Cr（Ⅲ）atoms exhibit an octahedral coordination geometry.     

Crystal Structure of a Novel Cadmium Coordination Polymer [Cd15（OH）4（SO4）4（L1）6（L2）12]n （HL1 = 1,2,3-1H-Triazole,HLe = 5-Methyl-lH-tetrazole

A novel cadmium coordination polymer [Cdls（OH）4（SO4）4（L1）6（L2）12]n （HL1 = 1,2,3-1H-triazole, HL2 = 5-methyl-lH-tetrazole） has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The compound crystallizes in cubicI-43d space group with a = 21.5247（4）, V = 9972.7（3） A3, Z = 4, Dc = 2.360 g/cm3, Mr = 3543.68, μ（MoKα） = 3.298 mm^-1, F（000） = 6696, the final R = 0.0340 and wR = 0.0992 for 1909 observed reflections （I 〉 2σ（I））. The compound contains two crystallographicatly independent Cd coordination centers linked up through one L1 and two L2 bridges. The structure displays an inorganic-organic hybrid cadmium coordination polymer.     

Synthesis and Crystal Structure of a Distorted 2D （6,3） Layer Complex, [Cd（H2mbdpz）（N3）2]n （H2mbdpz = 4,4′-Methylenebis（3,5-dimethylpyrazole）） Containing both End-on and End-to-end Azide Bridges

The complex [Cd（H2mbdpz）（N3）2]n 1 （H2mbdpz = 4,4′-methylenebis（3,5-dimethylpyrazole）） has been hydrothermally synthesized and characterized by single-crystal X-ray diffraction analysis. It crystallizes in the monoclinic system, space groups C2/c with a = 22.154（5）, b = 7.4835（15）, c = 21.044（8）A^°,β= 115.51（3）°, V= 3148.7（17）A^°3, Z= 8, C11H16CdN10, Mr = 400.75, Dc = 1.691 g/cm^3,μ = 1.401 mm^-1, F（000） = 1599, T= 293（2） K, the final R = 0.0228 and wR = 0.0581 for 3604 observed reflections with I 〉 2σ（I）. The structural determination revealed that the coordination environment of Cd（Ⅱ） atom is a distorted octahedron consisting of two nitrogen donors of two H2mbdpz ligands and four nitrogen donors from four azide ligands. The azide moieties act as bridges in two modes： end-on （μ1,1-） and end-to-end （μ1,3-）, and H2mbdpz also serves as a bridge with a bis-monodentate coordination. Both bridging ligands link the Cd（Ⅱ） atoms to form a distorted two-dimensional （6,3） layer.     

Synthesis,Crystal Structure and Photoluminescent Properties of a New Dinuclear Copper（Ⅰ） Complex [Cu2（μ2-dppm）2（MeCN）2（μ2-MeCN）]（ClO4）2·MeCN

The title compound [Cu2（μ2-dppm）2（MeCN）2（μ2-MeCN）]（ClO4）2·MeCN （dppm = bis（diphenylphosphino）methane） has been prepared and characterized. It crystallizes in the monoclinic system,space group P21/n,with a = 11.904（6）,b = 20.755（11）,c = 24.744（13）A,β = 98.226（12）°,C58H56Cl2Cu2N4O8P4,Mr = 1258.93,V = 6051（5） A^3,Z = 4,Dc = 1.382 g/cm^3,μ = 9.52 mm^-1,F（000） = 2592,R = 0.0533 and wR = 0.1295 for 6175 observed reflections with I 〉 2σ（I）. Each Cu（I） center is tetrahedrally coordinated by two phosphine atoms from two bridging dppm ligands,one nitrogen atom from a terminally coordinated acetonitrile molecule,and another nitrogen atom from a μ2-acetonitrile molecule. The two Cu（I） centers are bridged by two dppm ligands as well as a unique acetonitrile molecule. The full molecule exhibits a ＇chair-like＇ configuration. This dinuclear complex exhibits intense or middle photoluminescence at room temperature in the solid state or actonitrile solution at 486 nm.     

A New Two-dimensional Cd（Ⅱ） Coordination Polymer Constructed by Pyridine-2,5-dicarbohydrazide

A new two-dimensional Cd（Ⅱ） coordination polymer, [Cd（2,5-pdch）（H2O）]n·2n（ClO4）·nH2O （2,5-pdch = pyridine-2,5-dicarbohydrazide）, was prepared and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction analysis. The crystal belongs to monoclinic, space group P21/c with a = 10.905（2）, b = 11.602（1）, c = 15.034（2） A, β = 117.794 （10°, V = 1682.8（4A3, Z = 4, C7H13CdCl2NsO12, Mr = 542.52, Dc = 2.141 g/cm^3,/μ = 1.691 mm^-1, F（000） = 1072, 2（MoKa） = 0.71073A, the final R = 0.0608 and wR = 0.1329 for 2972 observed reflections with I 〉 2σ（I）. Single-crystal X-ray diffraction analysis reveals that the Cd（Ⅱ） atom displays a distorted pentagonal-bipyramidal geometry coordinated by three N atoms and three O atoms from three different 2,5-pdch ligands, and one water molecule. Interestingly, each two Cd（Ⅱ） atoms are bridged by two carbohydrazide groups of the 2,5-pdch ligands to form a dimeric unit, and such dimeric units are further connected by the 2,5-pdch ligand to generate a two-dimensional （4,4）-network.     

Synthesis,Crystal Structure and Biological Activity of a Novel Complex： Co（L）2（CH3OH）2Cl2 （L = 3-（1,2,4-Triazole-yl）-6-chloro-pyridazine）

The title compound, Co（L）2（CH3OH）2Cl2 （L = 3-（1,2,4-triazole-yl）-6-chloro-pyridazine） 1, has been synthesized and its crystal structure has been determined by X-ray analysis. Complex 1 crystallizes in the triclinic system, space group P1 with a = 6.018（3）, b = 9.832（5）, c = 9.921（5）A, a = 78.270（8）, β = 74.550（8）, γ = 83.807（8）°, V = 553.1（5）A^3, Z = 1, C14H16Cl4CoN10O2, Mr = 557.10, Dc = 1.673 g/cm^3, F（000） = 281,μ（MoKα） = 1.293 mm^-1, the final R = 0.0453 and wR = 0.1181 for 1539 observed reflections with I 〉 2σ（I）. The Co（II） ion is in a distorted centrosymmetric six-coordinate octahedral environment with two Ntriazole, two Omethanol and two Cl atoms. Via hydrogen bonds the configuration of 1 has been extended into 1D chains which are developed to 2D layers via π-π sticking action, and these layers are further extended into a 3D network by hydrogen bonds. The antibacterial activity of the title compound has been detected, and the results show that the ligands and cobalt（II） complex exhibit certain fungicidal activity against several bacteria. Furthermore, the spectral properties of the title compound have been also studied and discussed.     

Synthesis and Structure of a POMs-based 3D Zeolike Ionic Crystal, {[Co（dpdo）2（H2O）2（CH3CN）]2（SiMo12O40）（H2O）2}n

A POMs-based 3D zeolike ionic crystal 1, {[Co（dpdo）2（CH3CN）（H2O）2]2（SiMo12O40）- （HEO）2}n （dpdo = 4,4＇-bipyridine-N,N＇-dioxide）, was constructed via self-assembly by embedding Keggintype [SiMo12O40]^4- polyanions within the intercrystalline voids as pillars and structurally characterized. The crystal structure was determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1 with a = 11.430（3）, b = 12.242（3）, c = 14.279（3）A, α = 106.196（4）,β = 94.316（4）, γ = 98.294（3）°, V = 1884.5（7）A^3 Z = 1, C44H50N10O54CoEMo12Si, Mr = 2880.17, Dc = 2.538 g/cm^3, p = 2.484 mm^-1,F（000） = 1388, the final R = 0.0383 and wR = 0.1096 for 7753 observed reflections with I 〉 2σ（I）. Flack factor is 0.22（3）. Compound 1 is a pillar-layered framework with the [SiMo12O40]^4- anions linearly located on the square voids between the 2D bilayers which are formed by the dpdo ligands and cobalt（II） ions.     

Synthesis,Crystal Structure and Antimicrobial Property of 4-Bromo- 2- [（3-methypyridin-2-ylimino）methyl]phenol

The title Schiff base compound 4-bromo-2-[（3-methylpyridin-2-ylimino）methyl]phenol was prepared and structurally characterized by elemental analysis, IR spectrum, and single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P2 1/n, with a = 4.4870（9）, b = 19.953（4）, c = 13.860（3）A, β = 93.13（3）°, V = 1239.0（4）A3 Z = 4, Dc = 1.561 g/cm3, C13H11BrN2O2 , Mr = 291.15, p = 3.302 mm-1 and F（000） = 584. The final refinement gave R = 0.0608 and wR = 0.1377 for 1329 observed reflections with I 〉 2σ（I）. X-ray diffraction reveals that the non-hydrogen atoms in the compound are nearly coplanar, with the mean deviation of 0.0197A from the plane. The molecule adopts an E configuration about the central C=N functional bond. The compound possesses moderate antimicrobial property.     

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.