Synthesis and Crystal Structure of a Chiral Manganese(Ⅲ) Schiff Base Complex

A chiral salency complex,[Mn(Salency)(H2O)2](PF6)·2H2O 1(Salency =(R,R)-N,N'-bis(salicylidene)-1,2-cyclohexanediamine),has been prepared by the reaction of Mn(CH3COO)3·2H2O with Salency and NH4PF6,and was established by X-ray diffraction techniques.The complex crystallizes in triclinic,space group P1 with a=9.299(8),b=10.012(8),c=13.461(11),α=92.037(15),β=92.974(12),γ=93.530(18)°,V=1248.3(18)3,C20H28F6MnN2O6P,Mr = 592.35,Z=2,Dc=1.038 g/cm3,F(000)=608,μ=0.676 mm-1,the final R=0.0651 and wR=0.1880 for 5260 observed reflections with I 2σ(I).     

Synthesis and Crystal Structure of a Novel Dinuclear Copper（Ⅱ） Complex Containing Benzimidazole Schiff Base Ligand

A novel dinuclear copper(Ⅱ) complex [CuL(NO3)]2·2MeOH was obtained by the coordination reaction of Cu(NO3)2·3H2O with ligand HL (HL=N-(methyl-2-benzimidazol- methylidene)-2-hydroxyaniline). The single-crystal X-ray analysis has revealed that the complex crystallizes in triclinic, space group P with a=9.535(3), b=10.009(3), c=10.666(4) , α=104.303(4), β=100.105(4), γ=115.917(4)o, V=839.0(5) 3, C16H16CuN4O5, Mr=407.87, Z=2, Dc=1.614 g/cm3, F(000)=418, μ=1.338 mm-1, R=0.0543 and wR=0.0980. The basic dinuclear copper(Ⅱ) complex units [CuL(NO3)]2 are formed by NO3- as co-bridging ligands and L as NNO tridentate chelate coordinating to the copper ions. The ladder-like one-dimensional chain motifs are formed by O…H-O and O…H-N hydrogen bonds from methanol molecules connecting the dinuclear copper(Ⅱ) units.     

Synthesis and Crystal Structure of a Bimetallic Cyanide-bridged Complex Derived from Manganese(Ⅲ) Schiff-base Complex and Pentacyanidonitrosylferrate(Ⅱ) Building Blocks

A new cyanide-bridged bimetallic assembly [Mn(3-meosalpn)(H2O)]2[Fe(CN)5NO](1) was obtained by the reaction of [Fe(CN)5NO]2-with [Mn(3-meosalpn)]+,and characterized by elemental analysis,IR and single-crystal X-ray structure analysis.The complex crystallizes in the monoclinic system,space group P21/c with a = 12.992(5),b = 13.274(6),c = 14.644(6) ,β = 115.198(4)o,V = 2285.2(16)3,Z = 2,C43H44FeMn2N10O11,Mr = 1042.61,Dc = 1.515 g/cm3,F(000) = 1072,μ = 0.928 mm-1,S = 1.052,the final R = 0.0347 and wR = 0.0957 for 17377 observed reflections(Ⅰ 2σ(Ⅰ)).X-ray single-crystal diffraction analysis reveals that 1 has a trinuclear molecular structure,in which the two [Mn(3-meosalpn)(H2O)]+ cations are linked by the central [Fe(CN)5NO]2-anion via two trans CN-groups.Furthermore,the two [Mn(3-meo-salpn)(H2O)]+ cations and [Fe(CN)5NO]2-anion are connected into a one-dimensional zigzag chain through hydrogen bonding interactions.     

Synthesis,Crystal Structure and Cytotoxic Activity of a Zinc（Ⅱ） Complex of the Schiff Base Derived from S-benzyldithiocarbazate

A novel zinc(Ⅱ) complex of empirical formula,ZnL2(L=anionic forms of S-benzyl-β-N-(2,4-dichlorobenzylidene) hydrazine carbodithioate),has been synthesized and characterized by elemental analysis,IR spectra and single-crystal X-ray diffraction.The crystal belongs to the triclinic system,space group P with a = 9.3168(9),b = 13.0353(13),c = 14.7702(15) ,α = 71.2860(10),= 87.5140(10),γ = 79.4480(10)o,V = 1670.0(3) 3,Z = 2,Mr = 773.93,Dc = 1.539 g/cm3,μ = 1.334 mm-1,F(000) = 784,the final R = 0.0403 and wR = 0.0800 for 4060 observed reflections with I>2(I).In the crystal structure,the zinc(Ⅱ) complex has a distorted tetrahedral geometry in which the zinc ion is coordinated by the nitrogen and sulfur atoms from two Schiff base ligands,respectively.The preliminary bioassay indicates that the Schiff base and its zinc complex exhibit inhibitory activity against the human gastric cancer cell lines(MKN45) and hepatoma cell lines(HepG2).     

Synthesis and Crystal Structure of a Novel Fe(Ⅲ) Schiff Base Complex

A novel Fe(Ⅲ) Schiff base complex,FeⅢ(HL) {H4L = 1,1,1,1-tetrakis[(salicylaldimino)methyl]methane},has been prepared and characterized by elemental analyses,IR spectrum,and single-crystal X-ray diffraction analysis.The crystal belongs to the monoclinic system,space group P21/n with a = 12.569(3),b = 12.955(3),c = 17.647(4) ,β = 91.896(9)°,V = 2871.9(1) 3,Z = 4,Dc = 1.391 g/cm3,F(000) = 1252.0,Mr = 601.45,R = 0.0383 and wR = 0.1025.The structural analysis reveals that the Fe(Ⅲ) ions are six-coordinated by imine nitrogen atoms and phenolic oxygen atoms form three pendant arms of Schiff base ligands,and one of the salicylaldimine chelating units remains uncoordinated.Discrete complex molecules were further assembled into 1D supramolecular aggregations by C-H…O hydrogen bonding and C-H…π interactions.     

Synthesis,Crystal Structure and Property of a Binuclear Copper Complex [Cu_2L_2(pht)_2]_2·H_2O

A new binuclear copper complex, [Cu2L2(pht)2]2·H2O(Hpht = 5,5-diphenylhydantoin, i.e. phenytoin; L = 2-diethylaminoethanol), has been synthesized by the solvothermal method, and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group C2/c with a = 31.918(3), b = 12.9222(15), c = 19.868(2) , β = 98.762(2)o, V = 8098.8(16) 3, Dc = 1.429 Mg/m3, Z = 4, F(000) = 3640, μ = 1.107 mm-1, R = 0.0560 and wR = 0.1276(I 2(I)). Each copper(Ⅱ) in a molecule is coordinated with N and O atoms from ligand L and N atom from ligand Hpht in a tetradentate manner. Moreover, two copper(Ⅱ) centers are bridged by two O atoms of hydroxyl groups from two L ligands to form a slightly distorted binuclear {Cu2O2} diamond configuration. In addition, the interaction of this complex with calf thymus DNA(CT-DNA) was investigated by UV-vis spectrum and viscometry, and the complex may bind to DNA through intercalation.     

Synthesis and Crystal Structure of a Salicylaldehyde Ethylene Diamine Schiff Base Manganese (Ⅲ) Complex

1 INTRODUCTION Manganese is one of several first-row transition metal elements that have been found to play an important role in most biological systems. Perhaps the best known is in the process of photosynthesis during which water is oxidized to yield dioxygen, and it is generally believed that the process is related to a tetranuclear manganese cluster[1]. Other aspects of biological chemistry of manganese, such as three mononuclear manganese enzymes: manganese superoxide dismutase, per…     

Synthesis and Characterization of Two Mononuclear Mn~Ⅲ Compounds with Mixed Schiff Base Ligands

Two mononuclear Mn compounds of Mn III (salen)(L 1) and Mn III (salen)(L 2) (H 2 salen=N,N-ethylenebis-(salicylideneaminato),L 1=4-(2-hydroxybenzylideneamino)benzoic acid and L 2=4-(2-hydroxybenzylideneamino)-2-hydroxybenzoic acid) have been prepared and characterized by X-ray crystallography.Both compounds crystallize in the monoclinic system,space group P2 1 /c with a=14.351(4),b=14.955(3),c=11.869(3) and β=91.529(3)° for 1;and those for 2:a=14.439(9),b=15.217(9),c=11.660(7) and β=91.648(1)°.The compounds have similar structures,in which the Mn III center adopts a distorted square-pyramidal geometry with the basal plane constructed by two N and two O atoms from the salen ligand and the apical position occupied by the carboxylate O atom from L 1 or L 2 ligand.The voltammetric behavior of the compounds is examined,which shows quasi-reversible one-electron reduction of Mn(Ⅲ) to Mn(Ⅱ).The reduction potentials of both compounds fall between-0.33 V [E 0 (O 2 /O 2 ·)] and 0.65 V [E 0 (1 O 2 /O 2 ·)],which suggest that 1 and 2 could be potential mimics of Mn-SOD.     

Synthesis and Crystal Structure ofa Bipy Bridged Binuclear Cu^Ⅱ Complex Containing Aminomethanesulfonic Acid [Cu2（Sams）2（Bipy）（H2O）2]·（H2O）

The title complex [Cu2（Sams）2（H2O）2（bipy）]·（H2O） 1 （H2Sams = N-（2-hydroxybenzy） aminomethanesulfonic acid, bipy = 4,4′-bipyridine） has been synthesized by the reaction of Cu- （CH3COO）2·H2O, nESams and 4,4′-bipyridine in aqueous methanol. It was characterized by IR, elemental analysis, thermogravimetric analysis （TGA） and X-ray diffraction analysis. Complex 1 crystallizes in monoclinic, space group P21/n with a= 10.9533（17）, b = 8.3408（13）, c = 16.714（3） A^°, β = 101.295（4）°, V = 1494.3（4） A^°3 and Z = 2. The asymmetric unit is comprised of a tridentate Schiff base Sams^2- anionic ligand, a 4,4′-bipyddine and two coordinated water molecules, thus forming a binuclear copper（Ⅱ） complex. The coordination environment at Cu^Ⅱ center is described as a slightly distorted square pyramidal geometry. Via intermolecular hydrogen bonds C（10）-H（10）…O（3） and C（13）- H（13）…O（3）, an infinite supramolecular chain is yielded. A number of intermolecular hydrogen bonds greatly contribute to the stabilization of the solid-state structure for 1.     

Synthesis, Crystal Structure and Pyrolysis of a Heterobimetallic Peroxo-titanium（IV） Nitrilotriacetate Complex

A new heterobimetallic nitrilotriacetatoperoxotitanate complex with the formula of [Mn(H2O)5]2[Ti(O2)2O(nta)2]·7H2O (1, C6H6O6N = H3nta) has been isolated in pure crystals. It was characterized by elemental analyses, IR, thermal analysis (TGA) and single-crystal X-ray diffraction. Complex 1 crystallizes in monoclinic, space group C2/c with a = 15.088(3), b = 13.311(3), c = 17.741(4) , β = 100.92(3)°, Z = 4, V = 3498.6(12) 3, Mr = 968.19, Dc = 1.838 g/cm3, μ = 1.266 mm-1, F(000) = 1992, R = 0.0337 and wR = 0.0819. Single-crystal X-ray analysis reveals that the titanium atom is N,O,O',O'-chelated by the nitrilotriacetate and O,O'-chelated by the peroxo group, and is coordinated to the bridging O atom in an overall pentagonal-bipyramidal geometry. The manganese ions in the compound are both 6-coordinated by five water molecules and one bridged carboxylato oxygen atom. A decameric water cluster consisting of a cyclic water hexamer in a boat fashion is also found in complex 1. The TGA and XRD results prove that 1 undergoes facile thermal decomposition to form the mixture of Mn2O3 and TiO2 at 600～800 ℃, and pure MnTiO3 at 900 ℃.     

Hydrothermal Synthesis and Crystal Structure of a One-dimensional Manganese（Ⅱ） Compound Bridged by 2,6-Dichlorobenzoic Acid and Water

1 INTRODUCTION In recent years, coordination polymeric frame- works have attracted great attention not only due to their potential applications in the areas of magnetism, nonlinear optics, electronics, catalysis, and molecu- lar recognition and sorption but also to their intri- guing structure topologies[1～8]. The coordination polymers can be specially designed by careful selec- tion of the metal ions with definite coordination geometry, the structure of the connecting ligands, the nature…     

Synthesis,Structure and Magnetic Property of a Binuclear Nickel(Ⅱ) Complex

A new binuclear complex [Ni2(2,2'-bpy)2(C8H3NO6)2(H2O)4] 1 (2,2'-bpy = 2,2'- bipyridine, C8H3NO6 = 4-nitrophthalate) has been synthesized by a hydrothermal reaction and characterized by X-ray single-crystal diffraction analysis. The complex crystallizes in triclinic, space group P1 with a = 7.206(2), b = 10.337(4), c = 12.480(4) , α = 89.887(11), β = 77.033(9), γ = 78.349(6)o, V = 886.3(5) 3, Z = 1, C36H30Ni2N6O16, Mr = 920.08, Dc = 1.724 g cm-3, F(000) = 472, μ = 1.152 mm-1, the final R = 0.0458 and wR = 0.1163 for 3372 observed reflections with I 2σ(Ⅰ). The two Ni(Ⅱ) ions are bridged by two 4-nitrophthalates both in a bis-monodentate mode. Magnetic measurements reveal that the intramolecular exchange couplings in the dimer are ferromagnetic with 2J/k = 2.32 K, D =-1.44 K and g = 2.18.     

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

IntroductionIn recentyears many efforts have been devotedto the preparation and characterization of pendant-arm macrocyclic complexes due to the fact that theligating groups attaching to the macrocyclic skele-ton can offer additional donor groups to maintainthe coordination sphere of metal centers in themacrocycles[1,2 ] .In this way,functionalised pen-dant- arm macrocyclic complexes have been de-signed and prepared so as to mimic the structureand properties of certain metalloenzymes and met-a…     

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.     

Synthesis,Crystal Structure and Magnetic Property of a Novel Cu(Ⅱ)-Fluconazole-azide Complex

The title compound formulated as Cu2(C13H11N6OF2)(N3)3CH3OH was synthesized and structurally characterized by elemental analysis,IR and single-crystal X-ray diffraction.In the structure of the complex,the deprotonated fluconazole and azide anion link two copper centers to construct a binuclear SBU and the azide anion exhibits a μ1,1-coordination mode.Each triazole group of fluconazole links two SBUs and the compound exhibits a chain-like architecture with strong antiferromagnetism.     

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.     

Synthesis and Crystal Structure of a Mixed-ligand Manganese（Ⅱ） Complex Containing Abundant Hydrogen-bonding Interactions

A new mixed-ligand Mn(II)complex,namely [Mn(bipy)2(Huca)]·5H2O(1,bipy = 2,2'-bipyridine,and H3uca = uracil-5-carboxylic acid)has been prepared and characterized by single-crystal X-ray diffraction,FT-IR spectroscopy and thermogravimetric analysis.It crystallizes in monoclinic,space group C2/c with a = 23.597(8),b = 16.434(5),c = 15.531(6),β = 112.785(6)o,C25H28MnN6O9,Mr = 611.47,V = 5553(3)3,Z = 8,μ = 0.538,Dc = 1.463 g/cm3,F(000)= 2536,R = 0.0441 and wR = 0.1230 for all 5227 observed reflections(I > 2σ(I)).The manganese(II)center is surrounded by three bidentate chelating ligands,and it displays a severely distorted octahedral geometry,with cis angles ranging from 72.14(6)to 109.78(6)o.Extensive intermolecular hydrogen bonds link the [Mn(bipy)2(Huca)] monomers and lattice water molecules to yield a three-dimensional supramolecular framework.TGA shows complete removal of all lattice water molecules above 270 ℃.