Syntheses, Crystal Structures and Antibacterial Activities of Cobalt(Ⅱ) and Manganese(Ⅱ) Complexes with Schiff Base Ligand Derived from Tryptamine

Two new mononuclear complexes, namely [Co（L）2]（1） and [Mn（L）2]（2）（HL = N-（3-methylsalicylidene）tryptamine）, have been synthesized by the reactions of the ligand with cobalt acetate or manganese acetate in anhydrous ethanol. The crystal structures of the complexes were characterized by IR spectrum, elemental analysis, PXRD and single-crystal X-ray diffraction analysis. Complex 1 crystallizes in monoclinic, space group C2/c, with a = 23.146（2）, b = 9.4864（10）, c = 13.9261（15）A, β = 102.898（2）°, V = 2980.6（5） ？3, Z = 4, Dc = 1.367 g/cm3, F（000） = 1284 and μ = 0.616 mm^-1. Complex 2 crystallizes in monoclinic, space group P21/n, with a = 14.807（11）, b = 13.118（10）, c = 16.663（13） A, β = 111.237（14）°, V = 3017（4） A^3, Z = 4, Dc = 1.342 g/cm^3, F（000） = 1276 and μ = 0.477 mm-1. The units of complex 1 are linked by intermolecular N–H…π hydrogen bonds into infinite 1D chains, which are further extended into a 3D supramolecular structure by a series of π···π stacking interactions. The units of complex 2 are linked by intermolecular N–H…π hydrogen bonds and C–H…π hydrogen bonds into an infinite 3D supramolecular structure. Meanwhile, the antibacterial activities of the ligand and its complexes have been tested against four kinds of bacteria. The results show that the three compounds all have excellent antibacterial activities and that 1 and 2 possess stronger inhibiting effects against the bacteria than the Schiff base.

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） A）. The complex crystalizes in the P21 space group （a -- 21.4076（18）, b = 9.4792（8） and c = 25.287（2） A）, 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.

Syntheses, Characterizations, Crystal Structures and Antibacterial Activities of Two Zinc(II) Complexes with a Schiff Base Derived from o-Vanillin and p-Toluidine

Two new zinc（Ⅱ） complexes, [Zn2L2Ch].2[ZnL（CH3OH）Cl2] 1 and [ZnL2（NO3）2] 2, were synthesized by reacting ZnX2.nH2O （X = Cl^-, NO3^-） and a Schiff base ligand 2-[（4-methylphenylimino）methyl]-6-methoxyphenol （C15HIsNO2, L） which was obtained by the condensation of o-vanillin （2-hydroxy-3-methoxybenzaldehyde） with p-toluidine. Both 1 and 2 were characterized by single-crystal X-ray diffraction technique, elemental analysis, molar conductance, FT-IR, UV-Vis, IH-NMR spectra and thermogravimetrie analysis. The Schiff base ligand and its zinc（Ⅱ） complexes have been tested in vitro to evaluate their antibacterial activity against bacteria, viz., Escherichia Coli, Staphylococcus aureus and Bacillus Subtilis. The results show that these complexes have higher activity than the corresponding free Schiff base ligand against the same bacteria.

Syntheses, Crystal Structures and Antibacterial Activities of Two Heterocyclic Schiff Base Compounds

Two heterocyclic Schiff bases were synthesized via the condensation reactions of primary amines with carbonyl compounds. 2-[（4-pyridylmethylene）-amino] phenol （compound 1） was synthesized by the interaction of 4-pyridinecarboxaldehyde with o-aminophenol in ethanol solvent; N,N＇-bis（3-（furan-2-yl）allylidene）benzene-1,4-diamin （compound 2） was synthesized by the interaction of 3-（2-furyl）acrolein with p-phenylenediamine in ethanol medium. The compounds were characterized by elemental analysis, IR, MS and single-crystal X-ray diffraction. Compound 1 （C12H10N2O） crystallizes in the monoclinic system, space group P21/c with α = 7.0771（7）, b = 7.2820（7）, c = 19.849（2）, b = 96.3390（10）°, V = 1016.66（17） ？3, Z = 4, Mr = 198.22, Dc = 1.295 g/cm3, F（000） = 416, GOOF = 1.060, m = 0.085 mm-1, the final R = 0.0371 and wR = 0.0929 for 1497 observed reflections with I 〉 2σ（I）. Compound 2 （C20H16N2O2） crystallizes in the orthorhombic system, space group Fdd2 with α = 26.344（15）, b = 48.50（3）, c = 5.293（3）, V = 6764（7） ？3, Z = 16, Mr = 316.35, Dc = 1.243 g/cm3, F（000） = 2656, GOOF = 1.043, m = 0.081 mm-1, the final R = 0.0526 and wR = 0.1267 for 2059 observed reflections with I 〉 2σ（I）. 1 and 2 molecules are connected through hydrogen bonds to generate a 2D network and a 1D chain structure, respectively. The preliminary antibacterial activity results showed that the title compounds display excellent antibacterial activities to Escherichia coli, Staphylococcus aureus and Bacillus subtilis.

Synthesis and Crystal Structure of a New 2D O-bridged Copper(Ⅱ) Coordination Polymer Constructed from Sulfonate-derived Schiff Base

A new chain-like coordination polymer, namely, [CuL]n （1, Na2L = 2-[（2-hydroxy- benzylidene）-amino]-benzenesulfonic acid sodium salt）, has been synthesized and characterized by single-crystal X-ray diffraction, IR spectroscopy and elemental analysis. Complex 1 crystallizes in monoclinic system, space group P21/c with a = 9.2296（16）, b = 10.4754（18）, c = 12.200（2） A, β = 102.392（2）°, V = 1152.0（3）A3, CI3H9CuNOaN, Mr = 338.83, Dc = 1.953 g/cm3, Z = 4, F（000） = 684, p = 2.089 mm-1, the final R = 0.0376 and wR = 0.0956. X-ray diffraction analyses indicate that 1 displays a square-pyramidal metal center with NO4 donor sets. The sulfonate-derived Schiff base serves as a common N,O,O＇-tridentate and a unique O-bridged ligand connecting the metals. Dinuclear copper complexes serve as secondary building blocks （SBUs） to construct an unusual 2D coordination network. In the crystal, the components form a stable 3D supramolecular architecture by C-H...O interactions and to-stacking

Syntheses and Crystal Structures of Calix[4]arene Dithiocarbazate Schiff Bases

The regioselective syntheses of novel p-tert-butylcalix[4]arenes with functional aldehyde and dithiocarbazate Schiff base groups were carried out. p-tert-Butylcalix[4]arene was alkylated with o-, p-（ω-chloroalkoxy）- benzaldehydes in the system of K2CO3/KI/CH3CN to give calixarene 1,3-dialdehydes. Then the condensation reactions of active calixarene aldehydes with S-methyl and S-benzyldithiocarbazate, calixarene sulfur-containing Schiff bases were efficiently obtained in satisfied yields. The single crystal analysis of the four representative products shows that calixarene aldehydes and Schiff bases exist in cone conformation and there are interesting intermolecular hydrogen-bands and π...π interaction in the crystals.

Synthesis and Crystal Structure of a Zinc(II) Complex Salt with the Schiff Base of Picolinaldehyde N-oxide and Semicarbazone

The title zinc（Ⅱ） complex salt [Zn（H2O）6]（ClO4）2-（PNOS）4, where PNOS is derived from picolinaldehyde N-oxide with semicarbazone, has been prepared and structurally characterized by X-ray single-crystal analysis. It crystallizes in triclinic, space group PI with a = 7.529（3）, b = 10.206（4）, c = 14.678（6）A, a = 86.293（6）, β= 87.686（7）, γ= 81.382（6）°, C28H44Cl2N16O22Zn, Mr = 1093.06, V = 1112.3（8） ,A^3 Z = 1, Dc = 1.632 g/cm^3, S = 1.089, μ（MoKa） = 0.773 mm^-1, F（000） = 564, the final R = 0.0438 and wR = 0.1076 for 3888 independent reflections with Rint = 0.0224. The crystal structure possesses a [Zn（H2O）6]^2＋ cation, two ClO4^- anions and four PNOSs. In the crystal structure, Zn^2＋ cation is located at the symcenter and coordinated by six water molecules. In [Zn（H2O）6]^2＋, an elongate octahedral complex cation, the average Zn-O bond length is 2.087（2） A. There exist a lot of H bonds in the structure, linking the cation [Zn（H2O）6]^2＋, anion ClO4^- and PNOS to form a 3D network.

Synthesis and Crystal Structure of a New Three-dimensional Supramolecule of Copper(Ⅱ) Schiff Base Complex

A new three-dimensional supramolecule composed of copper-Schiff base complex, [Cu（naphdien）]Cl·H2O, where naphdien is Schiff base of 2-hydroxy-1-naphthaldehyde and diethylenetriamine, has been synthesized and determined by single-crystal X-ray diffraction. It belongs to the monoclinic system, space group P21/c, with a = 7.3490（15）, b = 7.0847（16）, c = 30.845（3）A, β= 95.33（3）°, V = 1599.0（5）A3, Z = 4, C15 H20ClCuN3O2, Mr = 373.33, De = 1.551 g/cm3, μ = 1.543 mm^-1, F（000） = 772, R = 0.0536 and wR = 0.0927 for 2788 unique reflections with 1659 observed ones （I 〉2σ（I））. In the crystal structure, mononuclear units [Cu（naphdien）]Cl·H2O are linked into a two-dimensional framework via strong hydrogen bonds, and extended into a three-dimensional supramolecular structure through π-π stacking interactions.

Synthesis and Crystal Structure of Complex of Zinc(Ⅱ) with Schiff Base {Zn[CH_3O(O)-C_6H_3CH_3=NN=C(S)NH_2](DMF)}_2

The title complex is a new binuclear Zn(Ⅱ) with chelate ligand of Schiff base containing S and N atom.The complex crystallizes in the orthorhombicspace group Pccn,with a=12.338(9),b=16.666(8),c=17.503(6),V=3599(6),Mr=723.52,Z=4,Dx=1.34 g/cm3,μ=15.22 cm-1,F(000)=1488.The structure was solved by direct methods and the final R=0.078.The crystal consists of discrete molecules with symmetric center at the center of the fourmembered ring consisting of two Zn atoms and two O atoms.

Synthesis, Structure and Antibacterial Activities of 4-BBTS Schiff Base and Its Complexes

4-Bromobenzaldehyde thiosemicarbazone Schiff base （4-BBTS） and its Cu（Ⅱ）, Zn（Ⅱ）, Co（Ⅱ） and Ni（Ⅱ） complexes were synthesized and characterized by elemental analysis, UV, IR, MS, ^1H NMR, and molar conductivity. Using disc diffusion method, the antibacterial activity tests were conducted. The results revealed that the ligand as well as all the complexes exhibits good antibacterial activities against E. Coli. and S. Aureus. Moreover, Cu（Ⅱ） complex shows the best antibacterial activity, which provides beneficial reference for studying the relationship between the structures and performances.

Synthesis and Crystal Structure of an Azide Bridged Binuclear Zinc(Ⅱ) Dimer Containing Taurine Schiff Base [Zn_2(C_8H_9N_2O_3S)_2·(N_3)_2·(H_2O)_2]_2·_2H_2O

The title complex [Zn2L2（N3）2（H2O）2]·2H2O （L = N-（2-pyridylmethylidene） taurine） has been synthesized in a methanol-water solution. The crystal belongs to monoclinic, space group P2 1/C with a = 15.8064（10）, b = 10.5015（5）, c = 17.3193（11） ,A, β= 111.314（2）°, V = 2678.2 （3） ,A ^3 C16H26N10O10S2Zn2, Mr = 713.33, Z = 4, DC = 1.769 g/cm^3, μ = 2.017 mm^-1 and F（000） = 1456. The asymmetric unit consists of two half-molecules of the complex and two water molecules. Four N and two O atoms form the coordination environment of each Zn atom, resulting in a distorted octahedral configuration. The two halves of each independent dimer are related by a crystallographic inversion centre, which lies at the centre of the ring formed by two Zn atoms and the coordinating atoms of the two azide anions. The average separation of Zn（Ⅱ）...Zn（Ⅱ） is 3.322 A. The molecules are linked by O-H...O hydrogen bonds, generating an interesting zigzag infinite chain structure in the ac plane.

Synthesis, Crystal Structure and Photoluminescence of a 2D Two-fold Interpenetrating Cd(II) Coordination Polymer Based on a Flexible Reduced Schiff Base Ligand

By the reaction of cadmium chloride with a reduced Schiff base ligand （H2L= N-（4- carboxybenzyl）-glycine）, a novel Cd（Ⅱ） compound [Cd（HL）2]·4H2O （1） has been obtained. Single-crystal X-ray diffraction analysis reveals that it crystallizes in orthorhombic, space group Pbcn with a = 13.9788（8）, b = 24.4204（14）, c = 13.9580（8） A, V= 4764.8（5） A^3, Z = 8, Mr = 600.84, Dc = 1.675 g/cm^3,/z = 0.983 mm^-1, F（000） = 2448, S = 1.084, R = 0.0806 and wR = 0.1705 （I〉 2a（1））. It displays a 2D two-fold interpenetrating structure. The Cd（Ⅱ） ions are six-coordinated. The cross-linkage of Cd（Ⅱ） ions by the bridge of HL anions results in a [Cd（HL）2] layer. Every two [Cd（HL）2]n layers are penetrated with each other, resulting in a two-fold interpenetrating double-layer structure by π-π stacking interactions and hydrogen bonds. Such double-layers are further linked by hydrogen bonds into a supramolecular structure. Photoluminescent investigation shows that compound 1 displays strong emission in the purple region.

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

The title compound, [Mn(salen)(salicyl)]?.5H2O ( H2salen = N, N?ethylenebis- (salicylideneaminato), Hsalicyl = salicylaldehyde), has been obtained from the reaction system containing (o-HOC6H4CH=NCH2)2, o-HOC6H4CHO and Mn(ClO4)2?H2O in EtOH solvent and structurally characterized. It crystallizes in the monoclinic, space group P21/c with a = 13.0548(4), b = 13.9254(4), c = 11.6630(1) ? b = 105.199(2)? V = 2046.09(9) ?, Z = 4, C23H22MnN2O5.5, Mr = 469.37, Dc = 1.524 g/cm3, F(000) = 972, m = 0.687mm-1 . R = 0.0630 and wR = 0.1142 for 1901 observed reflections with I >2(I). The Mn(Ⅲ) is coordinated by N(1), N(2), O(1) and O(2) of the Schiff base ligand and phenolate O atom of salicylaldehyde with O(3)Mn distance of 2.050(4) , forming a relatively rare five-coordinate square-pyramidal structure.

Synthesis and Crystal Structure of a Dinuclear Cu(II) Complex with Tridentate Schiff Base and Azido Bridge

A new dinuclear copper(II) complex ([Cu(C12H17N2O)(N3)]2, C24H34Cu2N10O2) has been synthesized and characterized by X-ray structure determination. It crystallizes in the monoclinic system, space group P21/c with a = 18.529(4), b = 10.933(2), c = 14.534(3) ?, β = 111.07(3)°, V = 2748(1) ?3, Z = 4, Mr = 621.69, F(000) = 1288, Dc = 1.503 g/cm3 and μ(MoKα) = 1.590 mm?1. The structure was refined to R = 0.0647 and wR = 0.1846 for 4406 observed reflections (I > 2σ(I)). The asymmetric unit comprises two halfmolecules. The complex is a centrosymmetric dimmer in which the copper atoms are penta-coordinated by three coordination atoms from the corresponding tridentate Schiff base ligand and two bridging azide anions. The Cu(II)…Cu(II) average distance is 3.350(1) ?.

Synthesis and Crystal Structure of a New Nickel(II) Complex with Unsymmetric Quadridentate Schiff Base Containing Oxime

The title complex, C18H15N3NiO3, has been prepared and characterized by X-ray diffraction analysis. It crystallizes in the monoclinic system, space group Cc with a = 10.939(2), b = 22.909(5), c = 6.907(1) ?, β = 116.75(3)°, V = 1545.7(5) ?, Z = 4, Mr = 380.04, F(000) = 784, Dc = 1.633 g/cm3 and μ(MoKα) = 1.279 mm–1. The structure was refined to R = 0.0472 and wR = 0.0893 for 2571 observed reflections with I > 2σ(I). The absolute structure Flack parameter X is 0.01(2). In this crystal structure, strong face-to-face π-π stacking interactions between adjacent molecules lead to a one-dimensional chain structure.

Synthesis and Crystal Structure of a Co(II) Complex with Schiff Base and Imidazole Ligand

The title compound, [Co（C3H4N2）2（C22H18N2O4）]·5H2O （Mr = 659.56）, has been prepared and its crystal structure was determined by X-ray diffraction method. The crystal belongs to monoclinic, space group P21/n, a = 9.6808（2）, b = 26.7204（5）, c = 12.7993（3） A, β = 100.9340（10）°, V= 3250.75（12） A^3, Z = 4, Dc = 1.348 g/cm^3,μ = 0.586 mm^-1, F（000） = 1380, S = 1.131, R = 0.0689 and wR = 0.1883 for 4782 observed reflections （Ⅰ 〉 2σ（Ⅰ））. The title crystal consists of Co（Ⅱ） complex and lattice water molecules. The Co（Ⅱ） complex assumes a distorted octahedral coordination geometry, formed by one Schiff base dianion phenylenediamine-3-methoxysali-cylaldehyde and two imidazole ligands. The π-π stacking interaction occurs between nearly parallel benzene rings of the neighboring complexes.

Syntheses and Crystal Structures of Two VO(IV) Schiff Base Complexes with Oxyammonia Ligand

Two novel VO(IV) Schiff base complexes, VO(SALHA)2[SALHA: salicyaldehyde- oxyammonia] and VO(o-VANHA)2 [o-VANHA: o-vanillin-oxyammonia], have been synthesized with salicyaldehyde or o-vanilline, hydroxylammonium chloride and vanadyl sulfate in absolute methanol, and their crystal structures were determined by single-crystal X-ray diffraction. The vanadium(IV) centers in both complexes are five-coordinate in a distorted square pyramidal geometry. VO(SALHA)2 (C14H12N2O5V, Mr = 339.20) crystallizes in the monoclinic system, space group P21/n with a = 14.716(9), b = 7.175(5), c = 14.716(9) ? b = 113.130(7), V = 1428.8(15) 3, Z = 4, Dc = 1.577 g/cm3, l = 0.71073 ? m(MoKa) = 0.720 mm-1, F(000) = 692, the final R = 0.0466 and wR = 0.0829 for 1561 observed reflections (I > 2s(I)). VO(o-VANHA)2 (C16H16N2O7V, Mr = 399.25) is of monoclinic, space group P21/n with a = 11.386(12), b = 10.405(10), c = 14.627(15) , b = 93.654(19), V = 1729(3) 3, Z = 4, Dc = 1.533 g/cm3, l = 0.71073 , m(MoKa) = 0.615 mm-1, F(000) = 820, the final R = 0.0513 and wR = 0.1129 for 1235 observed reflections (I > 2s(I)).

Syntheses, Crystal Structures and Fluorescent Properties of Two New Imidazolidino Schiff Base Compounds

Two new imidazolidino Schiff base compounds, （E）-N-（（quinoxalin-2-yl）methylene）- 2-（2-（quinoxalin-3-yl）imidazolidin-1-yl）ethanamine 1 and 2-（1-（2-（2-（quinoxalin-3-yl）imidazolidin- 1-yl）ethyl）imidazolidin-2-yl）quinoxaline 2, have been synthesized and characterized by elemental analysis, ^1H NMR, IR, MS and single-crystal X-ray diffraction. Crystallographic data for 1： C22H21N7, Mr = 383.46, monoclinic, space group P21, a = 7.0036（14）, b = 6.9151（14）, c = 19.701（4）A, β = 96.57（3）°, Z = 2, V = 947.9（3）A^3, Dc = 1.344 g/cm^3, F（000） = 404, μ = 0.085 mm^-1, Flack parameter = 0（2）, R = 0.0464 and wR = 0.1055; and those for 2： C24H26N8, Mr = 426.53, triclinic, space group PI, a = 9.6680（19）, b = 10.334（2）, c = 11.389（2）A, α= 104.12（3）, β = 102.95（3）, γ= 100.48（3）°, Z= 2, V = 1041.2（4）A3, Dc= 1.361 g/cm^3, F（000） = 452, μ = 0.086 mm^-1, R = 0.0373 and wR = 0.1155. For the two compounds, the five-membered imidazolidine rings all adopt envelope conformation. Moreover, the title compounds show one-dimensional layered and three-dimensional supramolecular chainlike structures, respectively. Fluorescent properties of the two compounds have been investigated in the solid state at room temperature. Compound 1 exhibits strong fluorescence and thus may serve as excellent candidates of green fluorescent materials.

Synthesis and Crystal Structure of a Dinuclear Cu(II) Complex [Cu(C_(12)H_(17)N_2O)(NCS)]_2 with Tridentate Schiff Base Ligand N-(Salicylidene)-3-dimethylaminopropylamine

A new dinuclear copper(II) complex (Cu(C12H17N2O)(NCS)2, C26H34Cu2N6O2S2) has been synthesized and characterized by X-ray structure determination. It crystallizes in the triclinic system, space group P1 with a = 11.289(2), b = 12.071(2), c = 12.113(2) ?, α = 72.90(3), β = 83.76(3), γ = 65.60(3)°, V = 1436.7(5) ?3, Z = 2, Mr = 653.79, F(000) = 676, Dc = 1.511 g/cm3, μ(MoKα) = 1.660 mm?1, the final R = 0.0334 and wR = 0.0856 for 5047 observed reflections (I > 2σ(I)). The asymmetric unit comprises two half-molecules. The complex is a centrosymmetric dimmer in which each copper(II) is coordinated in the equatorial plane to the N-(salicylidene)-3- dimethylaminopropylamine ligand through the deprotonated phenolic oxygen atom as well as the nitrogen atoms of imine and amine. The fourth coordination site is occupied by the nitrogen atom of NCS?, while the axial one by the symmetrically related phenoxy oxygen of the other monomeric unit. The Cu(II)…Cu(II) average distance is 3.110(1) ?.

Novel Isatin-Schiff Base Cu (II) and Ni(II) Complexes. X-ray Crystal Structure of Bis[3-(4-hexylphenylimino)-1H-indol-2(3H)-one]-dichlorocopper(II) Complex

Schiff base ligand （HL） derived from 4-hexylaniline with isatin （1H-indole-2,3-dione） and its complexes with Cu（Ⅱ）, Ni（Ⅱ） were prepared and characterized by analytical, spectroscopic （IR, UV-Vis, Mass） techniques, electrical conductivity, magnetic and thermal measurements. The crystal and molecular structure of [Cu（HL）2Cl2] was determined by a single-crystal X-ray diffraction study. The molecular structure of the title compound has an inversion center on the Cu atom.