Synthesis, Characterization, Crystal Structure and Antibacterial Activities of a Nickel（Ⅱ） Complex with 2＇-（2-Thienylidene）-hydroxybenzoylhydrazide

In the ethanol solvent, a nickel(Ⅱ) complex Ni(C12H10N2O2S)2 upon reaction of 2'-(2-thienylidene)-hydroxybenzoylhydrazide with nickel acetate was synthesized, and its structure was characterized by IR, UV, elemental analysis and X-ray diffraction analysis. The crystal belongs to monoclinic system, space group C2/c with a = 22.052(3), b = 5.9681(6), c = 18.522(2) (A), β = 110.679(4)° , V = 2280.6(4) (A)3, Z = 4, Mr = 551.27, μ = 1.606 mm-1, Dc = 1.075 g/cm3, F(000) = 1136 and Rint = 0.0556. The nickel(Ⅱ) atom in the compound is four-coordinated with two nitrogen atoms from amide and two oxygen atoms from keto group. The biological activities have been measured, show- ing the compound exhibits better anti-bacterial activity than the ligand.     

Synthesis and Crystal Structure of a Ni（Ⅱ） Complex of 2＇-[4-N,N＇-（Dimethylaminobenzyl- idene）]-3,5-dihydroxybenzoylhydrazide and Its Spectral Properties

A new nickel（II） complex [NiL2]（DMF）4 （HL = 2＇-[4-N,N＇-（dimethylamino- benzylidene）]-3,5-dihydroxybenzoylhydrazide） has been synthesized and its structure was characterized by IR,UV-Vis,1H NMR and elemental analysis. The fluorescence emission mechanism of the complex was discussed by fluorimetric spectra. The single-crystal structure was determined by X-ray diffraction analysis. The crystal belongs to the triclinic system,space group P1 with a = 0.9918（4）,b = 1.1297（4）,c = 1.1331（4） nm,α = 76.860（7）,β = 75.105（6）,γ = 89.022（7）°,V = 1.1936（8） nm^3,Z = 1,μ = 0.472 mm^-1,Dc = 1.319 g/cm^3,F（000） = 502 and Rint = 0.0913. In the title compound,the nickel（II） atom is four-coordinated with two nitrogen atoms from amide and two oxygen atoms from keto group. The complex is centrosymmetric with nickel located at the center.     

Synthesis and Crystal Structure of a Copper(Ⅱ) Compound with 4-Hydroxybenzoic Acid and Isonicotinamide:[Cu(4-hba)_2(inta)(H_2O)]·H_2O

A new copper(Ⅱ) compound has been prepared and fully characterized by elemen-tal analysis,IR,TG and single-crystal X-ray diffraction.The compound [Cu(4-hba)2(inta)(H2O)]·H2O (4-hba=4-hydroxybenzoic acid,inta=isonicotinamide) 1 crystallizes in the monoclinic system,space group P21/c with a=7.590(5),b=11.027(5),c=23.761(5),β=102.5740(10)o,V=1974.1(16) 3,Mr=991.84,Z=2,Dc=1.669 g/cm3,F(000)=1020,μ=1.166 mm-1,R=0.0353 and wR=0.0604 for 3166 observed reflections (I 2σ(I)).In compound 1,the copper cation is penta-coordinated with two carboxylate oxygen atoms from two different 4-hba ligands,two oxygen atoms from two coordinated water molecules and one nitrogen atom from inta ligand,showing a slightly distorted square-pyramidal geometry.     

CRYSTAL AND MOLECULAR STRUCTURE OF MOLYBDENUM COM-PLEX MoO_2Cl_2(C_4H_3OCOOH)_2

<正> The crystal and molecular structure of the title compound was determined by single crystal X-ray diffraction method. The complex crystallizes in the mono-clinic space group P21/n with a = 10. 306 ( 3) , b = 10. 161 (2), c = 14. 798 ( 4) A . β= 108. 52(2)°, V= 1469. 4(6)A3,Z= 4. The structure was solved by direct methods. Least-squares refinement converged to a final value of R = 0. 043 and Rw= 0. 040 for 1237 reflections. The molybdenum (Ⅵ) ion is bonded to two chlorine atoms, two oxo atoms and two oxygen atoms from two monodentately and weakly coordinated carboxyl groups of molecules C4H3OCOOH, forming a octahedron. The Mo-O distances are in the range 1. 66 - 2. 39A ,the Mo-Cl distances fall in the range 2. 33-2. 34A.     

SYNTHESIS, CHARACTERIZATION AND STRUCTURE OF [Co(DBP)_2·3Py]_2·2CHCl_3

The mixed ligand complex of cobalt with dibutylphosphate (HDBP) and pyridine has been synthesized. Elemental analysis yields the result that the formula of this compound is Co(DBP)_2·3Py·CHCl_3 (Py=pyridine). The thermal analsyis, visible spectra and magnetic properties of it have been studied as well. Single crystal structural analysis shows that the crystal is triclinic with space group P and the unit cell parameters are as follows:a=14.490(10), α=90.37(4)°,b=15.721(7), β=96.04(5)°,c=20.109(12), γ=105.63(4)°.The final R factor is 0.0773. Two Co atoms are connected by two bridging DBP groups to form a dinuclear molecule [Co(DBP)_2·3Py]_2 which has a C_s, symmetry. Each cell contains two dinuclear molecules and four chloroform molecules. The cobalt is coordinated in an octahedral arrangement by three oxygen atoms and three nitrogen atoms, of which one oxygen atom comes from a monodentate DBP group, two oxygen atoms from two bridging DBP groups, and the three nitrogen atoms from the three pyridi     

A 3D Nickel(Ⅱ) Complex Constructed by Bis(2-dimethylaminoethyl) Ether: Solvothermal Synthesis,Crystal Structure and Catalytic Properties

Treatment of bis(2-dimethylaminoethyl) ether(BDMAE) with nickel acetate afforded a novel 3D nickel(Ⅱ) complex [Ni(BDMAE)(H_2O)_3·(CH_3COO)_2·(H_2O)_2] under solvothermal conditions. Its crystal structure was characterized by elemental analysis, IR spectrum, PXRD and single-crystal X-ray diffraction analysis. The complex belongs to the orthorhombic system, space group C2221 with a=8.823(2), b=13.932(3), c=17.563(4) ?, V=2158.9(8) ?~3, Z=4, C_(12)H_(36)N_2NiO_(10), Mr=427.14, Dc=1.314 g/cm~3, F(000)=920 and μ=0.944 mm~(-1). Single-crystal X-ray diffraction reveals that the mononuclear nickel(Ⅱ) ion is six-coordinated to one oxygen, two nitrogen atoms of the BDMAE ligand and three oxygen atoms of coordinated water molecules. The complex exhibits a 3D supramolecular structure through a variety of intermolecular and intramolecular hydrogen bonding interactions. In addition, the complex has been investigated for catalytic properties towards the Henry reaction of nitromethane with p-nitrobenzaldehyde, and the results indicated that the 1-p-nitrophenyl-2-nitroethanol product was obtained in excellent yield under optimum conditions with the complex as the catalyst.     

Synthesis, Crystal Structure and Electrochemical Properties of [Ni(phen)_3]·(m-nitrobenzoic acid)_2·(H_2O)

A new nickel(II) coordination complex [Ni(phen)3]·(m-nitrobenzoic acid)2·(H2O) was synthesized by self-assembly of m-nitrobenzoic acid, 1,10-phenanthroline and nickelous per- chlorate. It crystallizes in the monoclinic system, space group C2/c, with a = 2.4596(6), b = 1.2124(3), c = 1.9824(5) nm, β = 97.088(5)o, V = 5.866(3) nm3, Dc = 1.474 g/cm3, Z = 4, Mr = 1301.82, μ(MoKα) = 0.417 mm-1 F(000) = 2688, R = 0.0493 and wR = 0.1025. Structural deter- mination indicates that the nickel(II) ion is coordinated with six nitrogen atoms from three phens, giving a distorted octahedral coordination geometry. The cyclic voltametric analysis shows that the electron transfer in the electrode reaction is irreversible.     

Synthesis,Crystal Structure and Thermal Stability Properties of a Binuclear Copper(Ⅱ) Coordination Polymer {[Cu_2(4,4'-bipy)_2(o-ABA)_4(H_2O)_2][(H_2O)_2]}_n

One-dimensional chain copper(Ⅱ) coordination polymer has been synthesized and characterized in the solvent mixture of water and alcohol with o-acetamidobenzoic acid,4,4'-bipyridine and copper perchlorate.It is of tetragonal,space group P41212 with a=1.57756(10),b= 1.57756(10),c=2.1438(3)nm,V=5.3352(8) nm3,Dc=1.524 g/cm3,Z=4,F(000)=2536,R= 0.0479 and wR=0.0979.The crystal structure shows two coordination modes.The copper(1) is coordinated with two nitrogen atoms of one 4,4'-bipyridine molecule and two oxygen atoms from two o-acetamidobenzoic acid molecules,forming a distorted tetrahedral coordination geometry;the copper(2) is coordinated with two nitrogen atoms of one 4,4'-bipyridine molecule,four oxygen atoms from two o-acetamidobenzoic acid molecules and two water molecules,generating a distorted octahedral coordination geometry.The result of TG analysis shows that the title complex is stable below 180.0 ℃.     

Synthesis,Crystal Structure and Magnetic Properties of an Oxalato-bridged Dinickel(Ⅱ) Complex with Nitronyl Nitroxide Radicals

A new oxalato-bridged dinickel(Ⅱ) complex [Ni2(NIT-MeImz)4(C2O4)](Ac)2·8H2O has been synthesized and characterized structurally as well as magnetically.It crystallizes in monoclinic,space group C2/c with a=24.608(4),b=21.399(3),c=17.992(3),β=131.680(2)°,V=7076(2)3,C50H86N16Ni2O24,Mr=1412.77,Z=4,Dc=1.326 g/cm3,μ(MoKα)=0.614 mm-1,F(000)=2984,R=0.0751 and wR=0.1791 for 2956 observed reflections with Ⅰ2σ(Ⅰ).X-ray analysis reveals that the crystal structure consists of [Ni2(NIT-MeImz)4(C2O4)]2+ moiety and two Ac-anions.Each nickel(Ⅱ) ion is six-coordinated with a distorted octahedral geometry:two nitrogen atoms and two oxygen atoms from NIT-MeImz together with two other oxygen atoms from the oxalato ion.The 2-D net structure is formed and arranged through intermolecular H-bonding interactions.Magnetic measurements show antiferromagnetic interactions for this complex.     

STUDY ON SYNTHESIS, STRUCTURE AND COMPLEXATION CHARACTERISTIC OF UO_2Cl_4(DCH 18C6·H_3O)_2*

The title compound was synthesized by extracting nranylchloride in HC1 system using dicyclohexyl-18-crown-6 as extraction agent. The absorption peaks 1090 cm~(-1) and 912 cm~(-1) in IR spectrum result from frequence red-shift of anti-symmetric stretch vibration of C—O—C of crown ring and [OUO] group, respectively.X-ray diffraction analysis results in its crystallographic parameters: triclinic system, space group P; a=10.183(3), b=10.606(3), c=12.850(6), α=72.09(3), β=85.97(4), γ=86.14(2)°, V=1315.7, z=1. The structure was solved by heavy atom method. Structure refinements converged to final R=0.062, R_w=0.061. U atom is situated on the symmetry center and coordinated by four chlorine atoms and two oxygen atoms to form a square bipyramid coordination polyhedron. The H_3O~+ group is embedded in the crown ring and connected with three crown oxygen atoms via hydrogen bonds.     

Synthesis and Crystal Structure of a New Dinuclear Manganese(Ⅱ) Manganese(Ⅲ) Complex of a Macrocyclic Ligand

A mixed-valence dinuclear manganese complex, [MnⅡMnⅢL](ClO4)·1/2MeOH, where L is a macrocyclic ligand derived from the cyclocondensation of sodium 2,6-diformyl-4-methylphenolate with N,N-bis(2-aminoethyl)-2-hydroxybenzyl amine, was obtained and its structure was determined by X-ray diffraction. The orange crystal is a monoclinic system with space group P21/c and lattice parameters a=1.1617(4), b=1.4005(3), c=1.4641(3) nm, β=113.03(2)°, and Z=2. The crystal structure shows that each pendant-arm is bonded in a bidentate fashion to the adjacent metal atom and that both the arms are on the same side of the macrocycle. The two Mn atoms are bridged by two μ2-phenoxy oxygen atoms of the tetra-imine macrocycle, and each Mn atom, locating in a trigonal prismatic coordination environment(N3O3), is six-coordinated by the two imine nitrogen atoms, one tertiary nitrogen atom and a pendant phenol moiety apart from the two oxygen atoms.     

Hydrothermal Synthesis, Crystal Structure and Electrochemical Properties of Complex Cu（α-Furacrylic acid）2（phen）

The title complex (C26H18CuN2O6,Mr=517.96) has been synthesized by the reac-tion of α-furanacrylic acid with 1,10-phenanthroline (phen) in the solvent mixture of water and methanol. Crystal data: monoclinic,space group C2/c with a =2.2927(4),b=1.01248(18),c=1.05061(18) nm,β=111.188(3)o,V=2.274(7) nm3,Dc=1.513 g/cm3,Z=4,F(000)=1060,μ= 1.007mm?1,R=0.0320 and wR=0.0781. The crystal structural analysis shows that the copper atom is coordinated with four oxygen atoms from two α-furacrylic acids and two nitrogen atoms from 1,10-phenanthroline,giving a distorted octahedral coordination geometry. The result of electroche-mical analysis shows that the electron transfer in the electrode reaction is quasi-reversible.     

Synthesis,Crystal Structure and Fluorescent and Thermal Stability Properties of the Zinc(Ⅱ) Complex [Zn(C_(15)H_(11)O_3)_2(C_(12)H_8N_2)_2]·5H_2O

A new complex has been synthesized with o-methylbenzoyl-benzoic acid(HL) and 1,10-phenanthroline(phen) in the mixture of water and ethanol. It crystallizes in monoclinic, space group C2/c with a = 13.6328(18), b = 17.7876(18), c = 19.998(2), β = 104.720(4)o, C54H48N4O11Zn, Mr = 994.33, V = 4690.2(9)3, Dc = 1.408 g/cm3, Z = 4, F(000) = 2072, μ(MoKα) = 0.59 mm-1, R = 0.0736 and wR = 0.2029. The crystal structure shows that the zinc ions are coordinated with two oxygen atoms from two HL molecules and four nitrogen atoms from two phen molecules, forming distorted octahedral coordination geometry. The fluorescent and thermal stability properties of the complex are studied. The result shows that it has one fluorescent emission band at around 412 nm. In addition, the complex is stable under 210 ℃.     

两个N-己酰基水杨酰肼合镍(Ⅱ)配合物的合成、结构及抗菌活性的研究

The two trinuclear nickel（Ⅱ） complexes, Ni3（C13H15N2O3）2（C5H5N）4 （1） and Ni3（C13H15N2O3）2（C5H5N）2- （C3H7NO）2 （2）, were prepared by the reaction of Ni（OAc）2·4H2O with N-hexanoylsalicylhydrazide. The crystal structures of complexes were determined by X-ray diffraction analysis. Complex 1 takes triclinic symmetry with space group P-1 and cell dimensions of a=0.92377（2） nm, b= 1.08786（6） nm, c= 1.29391（3） nm, α=76.395（4）°, β=78.418（3）°, γ=67.378（4）°, V= 1.15772（7） nm^3, Z= 1,μ= 12.63 cm^-1. Complex 2 belongs to triclinic system and P2（1） space group and the crystallographic data： a= 1.4889（2） nm, b= 1.0389（1） nm, c= 1.4994（2） nm, β= 96.174（4）°, V=2.3058（5） nm^3, Z=2,μ= 12.70 cm^-1. The structures of the two molecules are similar. The three nickel atoms in each molecule of the two title complexes arrange in a strictly linear structure. The central nickel atom of the molecule adopts octahedral configuration, while the two nickel atoms on the two sides adopt square-planar configuration in each molecule. But the central nickel atoms of the two complexes have different axial ligands, which cause a slight difference in the bond distances of the octahedron. The antibacterial activity of compound 1 against seven common bacteria was investigated.     

Solvothermal Synthesis,Crystal Structure and Antimicrobial Activity of a Novel Imide Nickel Complex [Ni（CH_3CONCOCH_3）_2·2（H_2O）]

A novel imide nickel complex [Ni(CH3CONCOCH3)2·2(H2O)] was synthesized by the solvothermal reaction of nickel acetate tetrahydrate and acetonitrile.What amazed us is that acetonitrile had changed into acetyl imide in enol form during the formation process of the title complex.The complex was characterized by elemental analysis,IR spectrum and X-ray single-crystal diffraction analysis.It crystallizes in the orthorhombic system,space group Pbca with a = 7.4503(7),b = 13.1089(12),c = 14.1303(14),V = 1380.0(2)3,Dc = 1.420 g/cm3,Mr = 294.94,Z = 4,F(000) = 616,μ = 1.422 mm-1,the final R = 0.0487 and wR = 0.1482.The four-coordinated nickel(II) center is surrounded by 4O atoms from two imide ligands and has a distorted square planar geometry.The complex is connected to form a supramolecule with an infinite three-dimensional network through intramolecular and intermolecular hydrogen bonds.Antimicrobial activity was investigated by agar diffusion method,and the result showed that the complex was active against coli bacillus,staphylococcus aureus and bacillus subtilis.The thermal stability of the title complex was also studied by TG-DTA method.     

氢键构筑的二维网状结构镍配合物[Ni(en)2(dpas)2]的合成、晶体结构及电化学性质

A new 2D Hydrogen-bonded network complex [Ni(en)2(dpas)2] (Nadpas=sodium diphenylamine sulphonic acid salt,en=ethanediamine) has been synthesized in aqueous solution,and characterized by elemental analysis,IR. The crystal structure was determined by single-crystal X-ray diffraction. The complex crystallizes in space group P21/c,with cell parameters a=0.605 6(5)nm,b=1.448 1(5) nm,c=1.711 9(5)nm,β=93.257(5)°,and V=1.498 9(14) nm3,Dc=1.497 g·cm-3,Z=2,F (000)=708,R=0.027 7,wR=0.072 5. The crystal structure shows that the nickel atom is coordinated with four nitrogen atoms from the two en and two oxygen atoms from two dpas to form a mononuclear complex. Furthermore,the adjacent complex units are extended into a 2D supramolecular network through hydrogen bonds.     

CRYSTAL STRUCTURES OF COPPER (Ⅱ) AND COBALT (Ⅲ) COM- PLEXES OF o-HYDROXYBENZYLGLYCINATE (HBG)

<正> The structures of two complexes C(CuOC6H4CH2NHCH2COO)2 (H2 O)]·H2P(1) and [Co(NH3)6[Co(OC6H4CH2NHCH2COO)2]2[C1]·10H2O (2) were determined by X-ray analyses. Compound (1) crystallizes in the orthorhombic space group P212121 with a=11. 357(1),b= 24. 304(2),c=7.317(4) A,Z= 4;While compound (2) in the monoclinic space group A2/a(C2/c) with a=23. 486(9) ,b=26. 605(6) ,c= 10. 542(1) A,γ= 128. 42(4)°,Z= 4. In compound (1),two Cu(Ⅱ) ions are bonded together by the phenolic oxygen atoms of two tridentate chelating ligands and each of them is separately coordinated by the carboxyl oxygen,amino nitrogen of each chelate ligand and by the fifth oxygen atom as well (from aqua or the carbonyl group in adjacent molecule). Thus the coordination of each Cu(Ⅱ) is a square pyramid with distances of 1. 93- 1. 97A to the four corner atoms and 2. 30 and 2. 32 A to the apex atoms. The whole molecule has an approximately planar configuratioir with the two pyramid apexes pointing towards one side. Compound (2) consists of     

Synthesis and Crystal Structure of [Mn（DPMT）2Cl2（H2O）2]

The title compound [Mn(DPMT)2Cl2(H2O)2] (DPMT = 1-[[2-(2,4-dichlorophenyl)- 1,3-dioxolan-2-yl]methyl]-1H-1,2,4-triazole) was synthesized by the reaction of MnCl2·4H2O and DPMT in ethanol solution and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c with a = 23.913(4), b = 7.8883(13), c = 8.6291(14) , β = 95.816(3)o, V = 1619.4(5) 3, Z = 2, C24H26Cl6MnN6O6, Mr = 762.15, Dc = 1.563 g/cm3, μ = 0.950 mm-1, S = 1.045, F(000) = 774, R = 0.0462 and wR = 0.0981. The molecular structure is a centrosymmetric conformation, and two ligands are symmetrically located on both sides of the Mn atom. The manganese atom is surrounded by two nitrogen atoms from ligands, two chlorine atoms and two oxygen atoms from water molecules to form a slightly distorted octahedral geometry.     

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.     

SYNTHESIS AND CRYSTAL STRUCTURE OF A MOLYBDENUM-COPPER-SULFUR CLUSTER COMPLEX WITH DITHIOBENZOATE LIGAND [Bu_4N]_2[MoCu_2S_4(C_6H_5CS_2)_2]

<正> The title compound has been synthesized by the reaction of (Bu4N)2MoS4, CuCl and (C6H5CS2)(Bu4N) in DMF and recrystallized from DMF/ Et2O. The red black crystal belongs to the triclinic space group P1 with a = 12. 021 (6), b = 17.045(8), c=17. 136(7)(?) , α=110.05(3), β=108.64(4), γ=103.87 (4)°, V = 2873(3)(?)3, Dc=1. 321gcm-3, Z = 2. The structure was refined to R = 0. 065 for .4783 reflections. The anion of the title compound can be described as a MoS42- tetrahedron coordinated by two [Cu(C6H5CS2)] units with the three metal atoms lying on a line. The coordination number of each Cu atom is three.