Syntheses,Crystal Structures and Antibacterial Activities of Schiff Base Ligand and Its Nickel(Ⅱ) Complex

A complex [NiL2] was synthesized, in which L, or to be exact, a Schiff base ligand(HL), was derived from the condensation of 1-phenyl-3-methyl-4-phenylacetyl-5-pyrazolone(PMPAP) with L-phenylalanine methyl ester. They were characterized by IR and single-crystal X-ray diffraction. Green block crystals of both ligand and its complex were grown at room temperature. The ligand, which consists of two individual fragments, crystalizes in the P1 space group(a = 5.6268(5), b = 10.6892(11) and c = 19.4869(18) ). The complex crystalizes in the P21 space group(a = 21.4076(18), b = 9.4792(8) and c = 25.287(2) ), which consists of a nickel six-coordinated compound. Every fragment is a distorted octahedron with four oxygen and two nitrogen atoms. The Schiff base ligand(HL) and its complex have been tested in vitro to evaluate their antibacterial activity against bacteria Escherichia Coli and Bacillus subtilis. It is found that the complex has higher activity than the corresponding free Schiff base ligand(HL) against the same bacterial.     

6-甲基-4-羟基-喹啉酸盐羟基钒(Ⅴ)(英)

The central V atom in bis[6-methyl-4-hydroxy-3-quinolinecarboxylate] mono(oxo)mono-hydroxy-vanadium(Ⅴ) (1), synthesized by the hydrothermal treatment of ethyl 6-methyl-4-hydroxy-3-quinolinecarboxylate and V₂O₅, has a distorted octahedral coordination geometry formed by six oxygen atoms from two oxygen atom of two hydroxy groups and two oxygen atoms of two carboxylate groups as well as one oxo group and hydroxy group. CCDC: 285592.     

PMBP缩1-萘胺合钴(Ⅱ)配合物的合成和晶体结构

Using 4-[(1-naphthylamino)phenylmethylene]-5-methyl-2-phenyl-2H-pyrazol-3(4H) one (L), its Co(Ⅱ) complex was synthesized and characterized by IR and UV in which the ligand as a -1 valence bidentate with Co(Ⅱ) form 2∶1 complex. X-ray structure analysis indicates that the Co(Ⅱ) ion is coordinated with oxygen atoms of pyrazolinon, nitrogen atoms of imine and oxygen atoms of DMF molecules to form a distorted six-coordination octahedron. π-π reciprocity and aromatic stack interaction are observed. There are no intra- and inter- hydrogen bond in the crystal and the complexes are held together by electronic and Van der Waals forces.     

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 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.     

Solvothermal Synthesis,Crystal Structure and Electrochemical Property of Complex [Co(p-MBA)_2(2,2′-bipy)(H_2O)]·(H_2O)

One novel complex [Co(p-MBA)2(2,2′-bipy)(H2O)]·(H2O) has been synthesized by the reaction of p-methylbenzoic acid with 2,2′-bipyridine in the solvent mixture of water and methanol. It crystallizes in triclinic,space group P1 with a=0.70479(14),b=1.1211(2),c=1.6718(3) nm,α=103.806(3),β=90.795(3),γ=104.207(3)o,V=1.2399(4) nm3,Mr=512.41,Dc=1.373 g/cm3,Z=2,F(000)=532,μ=0.733 mm-1,R= 0.0432 and wR=0.0957. The crystal structural analysis shows that the cobalt atom is coordinated with three oxygen atoms from two p-methylbenzoic acids and one water molecule and two nitrogen atoms from one 2,2′-bipyridine,forming a distorted square-pyramidal coordination geometry. The cyclic voltammetry behavior of the complex is also reported.     

Synthesis and Characterization of a New Symmetric Dinucleating Ligand and Its Dizinc(Ⅱ)Complex with Alkoxo and Carboxylate Bridges

<正>A novel dinuclear zinc(Ⅱ)complex[Zn_2L(μ-OAc)](PF_6)_2(CH_3OH)has been synthesized from a new symmetrical compartmental ligand HL in which the pendant arms,bearing pyridyl groups,are bridged by 1,3-diaminopropan-2-ol.X-ray crystal structure shows that the two zinc atoms reside within the adjacent ligand compartments and are bridged by the endogenous alkoxo-O from ligand and one exogenous carboxylate from acetate with a syn-syn mode.The coordination geometry of two zinc atoms is a distorted trigonal bipyramid with the pyridyl-N atoms and bridging alkoxo-O atom providing the equatorial donor set.Such coordination geometry observed in this complex is similar to that found in the dinuclear unit of phospholipase C.     

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 ℃.     

Hydrothermal Synthesis and Crystal Structure of a Lead(Ⅱ) Polymer with a Two-dimensional Network Structure:[Pb_2(PDB)_2(phen)]_n·nH_2O

A new metal-organic complex [Pb2(PDB)2(phen)]n·nH2O (H2PDB=pyridine-3,4-dicarboxylic acid,phen=1,10-phenanthroline) 1 has been hydrothermally synthesized and structurally characterized by elemental analysis,IR spectrum,TG and single-crystal X-ray diffraction.The compound crystallizes in triclinic,space group P1 with a=7.2472(5),b=10.6966(8),c=16.2376(12),α=98.2960(10),β=91.6430(10),γ=97.4810(10)o,V=1233.53(16)3,C26H16O9N4Pb2,Mr=942.81,Dc=2.538 g/cm3,μ(MoKα)=13.697 mm-1,F(000)=872,Z=2,the final R=0.0247 and wR=0.0654 for 3886 observed reflections (I 2σ(I)).In the crystal structure,the Pb(1) atom is six-coordinated with four carboxylate oxygen atoms from three different PDB ligands and two nitrogen atoms from phen ligand,showing a distorted octahedral geometry;the Pb(2) atom is four-coordinated with four carboxylate oxygen atoms from four different PDB ligands,showing a distorted tetrahedral geometry.It exhibits a three-dimensional supramolecular network structure formed by hydrogen bonds and π-π interactions.     

A novel mixed-coordination cobalt(Ⅲ)complex:synthesis and structure of Co(Ⅲ)(mpp)(Hmpp)(n-Bu_3P)_2

Complex Co(Ⅲ)(mpp)(Hmpp) (n-Bu_3P)_2(1,H_mpp=2-mereapto-3-pyridinol) wasobtained from the reaction of COCl_2 with H_2mpp,n-Bu_3P and Na metal in EtOH.The Co atomin a distorted octahedral geometry is coordinated with donor atoms N,O,P and S.The twoH_2mpp ligands form two different ehelato ringa with the Co(Ⅲ) ion:one 5-membered and thoother ono 4-membered,while the two n-Bu_3P ligands are in the axial positions with the angleP(1)-Co-P(2) of 176.1°.     

Hydrothermal Synthesis, Crystal Structure and Electrochemical Properties of the Complex Cu(o-Methylbenzoic acid)_2(2,2′-bipy)·(H_2O)

The title complex (C26H24CuN2O5, Mr = 508.01) has been synthesized by o-me- thylbenzoic acid, 2,2′-bipyridine (bipy) and copper perchlorate in the mixed solvent of water and methanol. It crystallizes in orthorhombic, space group P212121 with a = 0.70814(10), b = 1.6953(3), c = 1.9539(3) nm, V = 2.3457(6) nm3, Dc = 1.439 g/cm3, Z = 4, μ = 0.971 mm-1, F(000) = 1052, R = 0.0432 and wR = 0.0860. The structural determination shows that the copper atom is coordinated by three oxygen atoms from two o-methylbenzoic acids and one water molecule together with two nitrogen atoms from 2,2′-bipyridine, giving a distorted square-pyramidal coordination geometry. The cyclic voltammetric behavior of the complex is also discussed.     

Synthesis and Crystal Structure of a Manganese(Ⅱ) Complex with 2-(4'-Chlorine-benzoyl)-benzoic Acid and 1,10-Phenanthroline

A new metal-organic complex Mn2(cbba)4(phen)2 (Hcbba = 2-(4'-chlorine-benzoyl)-benzoic acid, phen = 1,10-phenanthroline) 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses and IR spectroscopy. The compound crystallizes in orthorhombic, space group Pbcn with a = 12.154(5), b = 18.166(7), c =31.197(13) (A°), V = 6887(5) (A°)3, C80H48C14Mn2N4O12, Mr= 1508.90, Dc = 1.455 g/cm3, μ(MoKa) =0.591 mm-1, F(000) = 3080, Z = 4, the final R = 0.0408 and wR = 0.0873 for 4033 observed reflections (I > 2σ(I)). In the crystal structure, the manganese atom is six-coordinated with four carboxylate oxygen atoms from three different cbba ligands and two nitrogen atoms from phen ligands, showing a distorted octahedral geometry. Furthermore, it exhibits a 3D supramolecular network through π-π interactions.     

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.     

Synthesis and Crystal Structure of a Novel Tetranuclear Zinc（Ⅱ） Coordination Polymer [Zn4（o-bda）4（p-pbim）4]n

A novel tetranuclear zinc（H） coordination polymer [Zn4（o-bda）a（p-pbim）4]n 1 （p-pbim = 4-pyridylbenzimidazole, o-bda2 = o-phenylenediacetic acid dianion） has been synthesized by a hydrothermal method and characterized by elemental analysis, IR and X-ray singlecrystal diffraction. The title complex crystallizes in monoclinic, space group of P21/n with α = 14.231（1）, b = 16.257（1）, c = 16.794（1） ]k, β = 100.26（1）°, V = 3823.1（2）A3, Z = 8, Dc = 1.573 g/cm^3,β = 1.321 mm^-1, F（000） = 1856, R = 0.0420 and wR = 0.111. The Zn（1） atom assumes a distorted trigonal bipyramidal geometry, involving three carboxyl O atoms from two different o-bda ligands and two N atoms from two p-pbim ligands. The Zn（2） atom is coordinated by two oxygens from two distinct bda2- anions and two nitrogen atoms from two p-pbim ligands to form a distorted tetrahedral geometry. The Zn（Ⅱ） atoms are alternately interlinked by o-bda ligands in bis-monodentate or chelating-bidentate and monodentate modes into one-dimensional undulate chains along axis c with the adjacent Zn…Zn distances of 8.32 and 8.47 A. Such neighboring chains are further extended into a 1D bi-chain structure with two different subrings A and B, which are 32- and 14-membered rings through interchain p-pbim ligands. There exists a 2D supramolecular network linked by intermolecular hydrogen-bonding interactions between the uncoordinated carboxylate 0（4） atom or coordinated carboxylate 0（7） atom and the uncoordinated imidazolyl N（2） and N（5） atoms with the O...N distances to be 2.695 and 2.807A.     

N,N′-苄基-1,2二胺合铜的合成和晶体结构及与DNA的相互作用(英文)

A ligand,(N,N′-dibenzylethane-1,2-diamine)(L),and its complex with copper acetate was synthesized and characterized by some spectral analyses.The copper ! ion is six-coordinated and exhibites octahedral coordination geometry,the coordination atoms are four nitrogen atoms from two(L) ligands and two carboxyl oxygen atoms from two acetic acid groups,respectively.After studying the interaction of the complex with calf thymus DNA through UV and fluorescence spectra,we can find that there is a strong binding and a large affinity berween the complex and calf thymus DNA.CCDC: 649416.     

Hydrothermal Synthesis and Crystal Structure of a New Manganese（Ⅱ） Complex with 2,4-Pyridine-dicarboxylic Acid and 2,2′-Bipyridine Ligands

A new metal-organic complex [Mn2（PDC）2（bipy）2（H2O）2] （H2PDC = 2,4-pyridine-dicarboxylic acid, bipy = 2,2′-bipyridine） 1 has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, TG and single-crystal X-ray diffraction. The compound crystallizes in triclinic, space group P ^-1 with a = 7.376（3）, b = 9.990（4）, c = 11.950（5） A^°, α= 75.217（5）, β = 78.052（5）, γ = 70.655（5）°, V = 796.0（5）A^°3, C34HE6Mn2N6O10, Mr = 788.49, De = 1.645 g/cm^3,μ（MoKa） = 0.866 mm^-1, F（000） = 235, Z = 1, the final R = 0.0425 and wR = 0.0700 for 1971 observed reflections （I 〉 2σ（I））. In the crystal structure, the manganese atom is six-coordinated by two carboxylate oxygen atoms from two different PDC ligands, one aqua ligand, and three nitrogen atoms from 2,2′-bipy and PDC ligands, giving a distorted octahedral geometry. It exhibits a three-dimensional supramolecular network defined by O-H…O hydrogen-bonding interactions.     

Hydrothermal Synthesis and Crystal Structure of a New Manganese(Ⅱ) Complex with 2,4-Pyridine-dicarboxylic Acid and 2,2'-Bipyridine Ligands

A new metal-organic complex [Mn_2(PDC)_2(bipy)_2(H_2O)_2] (H_2PDC=2,4-pyridinedicarboxylic acid,bipy=2,2'-bipyridine) 1 has been hydrothermally synthesized and structurally characterized by elemental analysis,IR spectrum,TG and single-crystal X-ray diffraction. The compound crystallizes in triclinic,space group P~(-)1 with α=7.376(3),b=9.990(4),c=11.950(5)(A),α=75.217(5),β=78.052(5),γ=70.655(5)°,V=796.0(5)(A)~3,C_(34)H_(26)Mn_2N_(6O)O_(10),M_r=788.49,D_c= 1.645 g/cm~3,μ(MoKa) = 0.866 mm~(-1),F(000)=235,Z=1,the final R=0.0425 and wR=0.0700 for 1971 observed reflections (Ⅰ > 2σ(Ⅰ)). In the crystal structure,the manganese atom is six-coordinated by two carboxylate oxygen atoms from two different PDC ligands,one aqua ligand,and three nitrogen atoms from 2,2'-bipy and PDC ligands,giving a distorted octahedral geometry. It exhibits a three-dimensional supramolecular network defined by O-H…O hydrogen-bonding interactions.     

Solid state reactions of nitrogenous heterocyclic compounds(Ⅰ)——Solid state reactions of 3-methyl-l-phenyl-5-pyrazolone with carbonyl compounds

The solid state reaction of 3-methyl-1-phenyl-5-pyrazolone (MPP) with aromatic aldehydes and ke-tones benzil derivatives and imides,and the solid state Michael addition reaction of MPP with 4-arylidene-3-methyl-1-phenyl-5-pyrnzolone 2 were investigated.Some new solid state reactions between the reactants were found,from which a series of new compounds were obtained The structures of the products were identified by IR,1H NMR,MS,elemental analyses and also by X-ray crystal analysis,and the reaction mechanism of MPP with aromatic aldehydes and ketones was proposed     

Synthesis and Crystal Structure of a Novel 2-Fold Interpenetrating Three-dimensional Coordination Polymer,{[Co_3（byip）_2（bix）_3（H_2O）_2]·H_2O}_n

The title coordination polymer including two crystallographically independent Co2+ ions is hydrothermally synthesized, in which the Co(1) 2+ ion is four-coordinated by two carboxylate oxygen atoms from two different 5-(benzoic acid-4-yldiazenyl)isophthalate (byip3-) anions and two nitrogen atoms from two distinct 1,4-bis(imidazol-1-ylmethyl) benzene (bix) ligands displaying a tetrahedral geometry. The Co(2) 2+ ion is six-coordinated by two water molecules at the apical positions, and two carboxylate oxygen atoms and two nitrogen atoms at the equatorial positions, affording a slightly distorted octahedron. Two Co(1)2+ and two Co(2)2+ ions are linked together by four byip3- anions forming a 44-membered motif and these motifs are further arranged into a three-dimensional framework through bix ligands along the a axis with a larger channel (ca. 22.70×11.01). Each individual network interpenetrates with the other identical network in a parallel fashion to generate a 2-fold interpenetrating array with the {62.84}{63}2{64.82}2 topology.     

具有梯形结构钴(Ⅱ)配位聚合物的合成及晶体结构

Co(NO₃)₂, N-carbazolyacetic acid and 4,4′-bipyridyl can give rise to a novel coordination polymer [CO₂(Cabo)₂(NO₃)₂(4,4′-bipy)₂]_n using a fritted U-tube. Single crystal X-ray diffraction displays in the complex, each Co(Ⅱ) is six-coordinated by two N atoms from different 4,4′-bipyridyl ligands, two O atoms of the bridge from two N-carbazolyacetic acid and two O atoms of one nitrate anion to form a distorted octahedral. Two O atoms of the carboxyl group act as bridge to link two Co(Ⅱ) atoms. The resulting structure is a ladder polymer. CCDC: 211713.