Synthesis, Crystal Structure and Electrochemical Property of 5,10,15,20-Tetrakis(4-chlorophenyl)porphyrin

The title compound 5,10,15,20-tetrakis（4-chlorophenyl）porphyrin was synthesized and structurally characterized by X-ray single-crystal diffraction method. Crystal data： triclinic, space group P, Z=1, C50H32Cl4N4, Mr=830.60, a=6.4316（13）, b=11.322（2）, c=13.833（3） , α =91.44（3）, β=91.06（2）, γ=92.67（3）°, V=1005.7（3）3 , Dc=1.371 g/cm3 , μ（MoKα）=0.34 mm-1 , F（000）=428, R=0.0563 and wR=0.0867 for 2712 observed reflections with I 〉 2σ（I）. X-ray analysis reveals the phenyl rings and the pyrrole rings are not in the same plane. The dihedral angles between adjacent phenyl rings and pyrrole rings are 66.1 and 66.8°, respectively.

Synthesis,Crystal Structure and Electrochemical Property of the Ferrocenyl Schiff-base (E)-N’(Ferrocene Ethylidene)Picolino Hydrazide

A novel Schiff-base compound based on ferrocene C18H17OFeN3 （1） has been synthesized and characterized by X-ray diffraction. The title compound crystallizes in monoclinic, space group P21/c with a = 19.2343（17）, b = 10.5084（9）, c = 7.9373（7） A, β = 97.7740°, Z = 4, V = 1589.6（2） A^3, Dc = 1.451 g/cm^3, μ（MoKα） = 0.956 mm^-1, F（000） = 720, the final R = 0.0343 and wR = 0.0973 for 2759 observed reflections （I 〉 2σ（I））. Electrochemical measurements exhibit that compound 1 undergoes a reversible one-electron redox process.

Crystal Structure, DFT and Electrochemical Property of a Novel C3-symmetrical 1,3,5-Tri（9-ethyl-6-nitrocarbazol-3-yl） Benzene

A novel C3-symmetrical molecule, 1,3,5-tri(9-ethyl-6-nitrocarbazol-3-yl) benzene(IV), was synthesized and characterized by 1 H NMR, 13 C NMR and UV-vis spectroscopy, elemental analyses and X-ray single crystal diffraction analysis. For this complex: C48 H36 N6 O6, Mr = 792.83, triclinic system, space group P1, a = 11.568(6), b = 13.158(7), c = 17.856(10) ?, α = 95.419(9), β = 107.345(8), γ = 114.682(8)o, V = 2281(2) ?3, Z = 2, Dc = 1.154 g/cm3, λ = 0.71073 ?, F(000) = 828, S = 1.083, R = 0.0836 and wR = 0.1926 for 3304 observed reflections with I > 2ζ(I). The compound possesses good thermal stability with the decomposition temperature(Td) of 265 ℃. The absorption and emission spectra show that the compound can emit blue light in CHCl3, and the quantum yield of compound IV in EtOH was 0.66. Furthermore, the electrochemical properties of compound IV were also studied by cyclic voltammetry(CV) method, and the results correspond to the data of theoretical calculation by the Gaussian 09 software.

Synthesis, Crystal Structure and Electrochemical Properties of a One-dimensional Chain Coordination Polymer [Cu(phen)(2,4,6-TMBA)_2(H_2O)]_n

A one-dimensional chain coordination polymer [Cu（phen）（2,4,6-TMBA）2（H2O）]n has been synthesized by reacting 2,4,6-trimethyl-benzoic acid, 1,10-phenanthroline and Cu（Ⅱ） perchlorate and its structure was characterized. Crystal data for this complex： tetragonal, space group I41, a = 2.0293（3）, b = 2.0293（3）, c = 1.3758（2） nm, α =β= γ = 90°, V= 5.6657（13） nm3, Dc= 1.379 g/cm3, Z = 8, μ（MoKa） = 0.815 mm-1, Mr = 588.14, F（000） = 2456, S = 1.047, R = 0.0459 and wR = 0.1053. The crystal structure shows that two neighboring Cu（Ⅱ） ions are linked together by one bridging-chelating 2,4,6-trimethyl-benzoic group, forming a one-dimensional chain structure. Each Cu（Ⅱ） ion is coordinated with two nitrogen atoms from one 1,10-phenanthroline molecule, three oxygen atoms from three 2,4,6-trimethyl-benzoic acid molecules and one oxygen atom from one water molecule, giving a six-coordinate distorted octahedral coordination geometry. The cyclic voltammetry behavior of the complex was also investigated.

Synthesis, Crystal Structure and Electrochemical Properties of Complex [Ni(2,2’-bipy)_2(ClC_6H_4COO)(H_2O)](ClO_4)

A new nickel（Ⅱ） coordination complex [Ni（2,2＇-bipy）2（ClC6H4COO）（H2O）]（ClO4） was synthesized by self-assembly reaction of m-chlorobenzoic acid, 2,2＇-bipy and Ni（ClQ4h·6H2O. The crystal of the title compound belongs to monoclinic system, space group P2（1/n） with a = 0.77764（14）, b = 2.6572（5）, c = 1.3637（2） nm, β = 96.456（3）°, V= 2.8000（9） nm^3, D,, = 1.528 g/cm^3, Z = 4, Mr = 644.10, μ（MoKα） = 0.937 mm^-1, F（000） =1320, R = 0.0549 and wR = 0.1164. Structure analysis shows that the nickel（Ⅱ） ion is coordinated with four nitrogen atoms from two bipys as well as two oxygen atoms from m-chlorobenzoic acid and water, respectively, giving a distorted octahedral coordination geometry. The cyclic voltametric behavior of the complex is also presented.

A Novel Copper(Ⅱ) Complex of Asymmetrically N-Functionalized 1,4,7-Triazacyclononane Ligand： Syntheses, Structure, Electrochemical Property and Biological Activities

A novel copper（Ⅱ） complex derived from 1,4,7-triazacyclononane[CuL]_2（PF_6）_3×MeCN×H_2 O was synthesized and crystallographically characterized {L = 1,4-bis（2-carbamoylethyl）-7-benzimidazole-2-yl-methyl-1,4,7-triazacyclononane}. It crystallizes in triclinic, space group P1, with a = 13.2425（13）, b = 14.0807（15）, c = 17.6798（18）, α = 86.296（2）, β = 72.773（2）, γ= 68.905（2）o, V = 2934.5（5）A^3, Z = 2, D_c = 1.611 g/m^3, F（000） = 1456, M_r = 1423.09, m = 0.920 mm^-1. The final R = 0.0671 and wR = 0.1874 for 6501 observed reflections with I 〉 2σ（I）. The structural analysis shows that the complex cation（[CuL]_2^3＋） was formed by two complex cations, namely（[CuL^3]^2＋） and [CuL_（-H）~3]~＋） through a hydrogen bond. In each complex cation, the Cu（Ⅱ） lies in a distorted square pyramidal geometry. The redox behavior was studied by cyclic voltammetry（CV） in aqueous solution which indicates a reversible one electron redox reaction. The result of UV absorption, ethidium bromide（EB） fluorescence spectra indicated that the complex binds to CT-DNA in an intercalative mode. Superoxide dismutase（SOD） activity of the complex was determined by photoreduction of NBT, and the value of IC_（50） is 5.22 μmol·L^-1.

Synthesis, Crystal Structure and Electrochemical Properties of a One-dimensional Chain Coordination Polymer [Mn(NAA)_2(4,4’-bipy)(H_2O)_4]_n

A novel one-dimensional chain coordination polymer [Mn（NAAh（4,4′-bipy）（H2O）4], has been synthesized with a-naphthaleneacetic acid, 4,4′-bipy and manganese（Ⅱ） sulfate as raw materials. Crystal data for this complex： monoclinic, space group P21/c, a = 1.1421（2）, b = 1.6337（3）, c = 0.94177（19） nm, β = 112.15（3）°, V = 1.6275（6） nm^3, De = 1.407 g/cm^3, Z = 2, μ（MoKa） = 0.467 mm^-1, F（000） = 722, S = 1.007, R= 0.0412 and wR = 0.1022. The crystal structure shows that two neighboring manganese（Ⅱ） ions are linked together by one 4,4′-bipy molecule, and the whole complex molecule forms a one-dimensional chain structure. Each manganese（Ⅱ） ion is coordinated with two oxygen atoms of two a-naphthaleneacetic acid molecules, two nitrogen atoms of two 4,4′-bipy molecules and two oxygen atoms from two water molecules, giving a distorted octahedral coordination geometry. The electrochemical properties were also analyzed.

Hydrothermal Synthesis, Crystal Structure and Electrochemical Properties of Complex Mn_2(phen)_2(p-CBA)_4(H_2O)

One novel complex Mn2（phen）2（p-CBA）4（H2O） has been hydrothermally synthesized from p-chlorobenzoic acid （p-CBA）, 1,10-phenanthroline （phen） and anhydrous manganese（Ⅱ） sulfate and then characterized. Crystal data for this complex： monoclinic, space group C2/c, with a = 2.3416（3）, b = 1.5604（2）, c =1.5605（2） nm, β = 121.048（2）°, V = 4.8849（12） nm^3, Dc = 1.510 g/cm^3, Mr = 555.26, Z = 8, μ = 0.798 mm^-1, F（000） = 2256, GOOF = 1.032, the final R = 0.0393 and wR = 0.0816. The crystal structure shows that two neighboring manganese（Ⅱ） ions are linked together by two bridge-chelating p-chlorobenzoic groups and one bridging water molecule, forming a cage structure with the Mn–Mn bond distance of 0.3512 nm. Each manganese（Ⅱ ） ion is coordinated by two nitrogen atoms of one 1,10-phenanthroline molecule and four oxygen atoms from three p-chlorobenzoic acid anions and one water molecule, giving a distorted octahedral coordination geometry. The cyclic voltammetric behavior of the complex was also investigated.

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

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

Synthesis, Crystal Structure and Electrochemical Properties of a Novel Phenothiazine Derivative

A new compound 1,1?-bis(3-pyridyl)-propylene(3,7-diformyl-N-ethylpheno- thiazinyl)ketone (C30H23N3O2S, Mr = 489.4) has been synthesized, and its crystal structure was determined by single-crystal X-ray diffraction method. The crystal is of orthorhombic, space group Ima2 with a = 27.491(5), b = 11.942(2), c = 7.389(2) ?, V = 2425.8(7) ?3, Z = 8, Dc = 1.340 g/cm3, μ = 0.167 mm-1, F(000) = 1024, the final R = 0.0363 and wR = 0.0869 for 2054 unique reflections with Rint = 0.0254. The structural determination shows that the molecule assumes a butterfly configuration with nearly planar wings. In addition, the electrochemical study indicates that there is a high electronic delocalization in the molecule.

Synthesis, Crystal Structure and Electrochemical Properties of 2-Chlorobenzaldehyde Thiosemicarbazone

The title compound crystallized in space goups P2(1)/c with Z=4, in a unit cell of dimensions, a=12.964(4), b=5.131(5), c=14.970(1)Angstrom; V=9331(1) Angstrom(3) Dc=1.429gcm(-3), mu=0.541mm(-1), R=0.045, Rw=0.059. The equilibrium constant of the ligand with CdBr2 was obtained by polarographic method. Crystal structure determination revealed that the molecule is in transconformation and non-hydrogen atoms of the molecule are in one plane except N(3) atom.

Hydrothermal Syntheses and Crystal Structures of Two Complexes with 3,5-Dinitrosalicylate and 2,2′-Bipyridine Ligands

The two title complexes, [Cd{3,5-（NO2）2sal}（2,2′-bipy）]n 1 and [Mn{3,5- （NO2）2sal}（2,2′-bipy）]n 2 （3,5-（NO2）2sal = 3,5-dinitrosalicylate, 2,2＇-bipy = 2,2′-bipyridine）, were synthesized by the hydrothermal reaction and structurally characterized. Complex 1 crystallizes in triclinic, space group P1, a = 5.581（4）, b = 12.071（8）, c = 12.88（1）A, α= 92.10（3）,β= 96.73（3）, γ = 102.02（2）°, C17H10N407Cd, Mr = 494.69, V= 841（1）A3, Z = 2, Dc = 1.954 g/cm3, F（000） = 488, μ= 1.353 mm^-1, R = 0.0248 and wR = 0.0761. Complex 2 crystallizes in monoclinic with space group P21/c, a = 8.604（3）, b = 23.88（1）, c = 8.894（3） A, β = 102.45（1）°, C17H10N407Mn, Mr = 437.23, V= 1785（1） A3, Z=.4, Dc = 1.627 g/cm3, F（000） = 884, μ = 0.791 mm^-1, R = 0.0471 and wR = 0.1250. Complex 1 possesses an infinite 1D polymeric chain structure consisting of the repeated basic four-membered ring units （Cd2O2） and eight-membered ring units （CdOCO）2. Compound 2displays a linear 1D chain through Mn（Ⅱ） atoms and bridging carboxylate groups of 3,5-dinitrosalicylic acid ligands with the Mn…Mn separation of 4.472（2）A. The fluorescence properties and cyclic voltammetric behaviors of the complexes are also reported.

Synthesis, Crystal Structure and Properties of a Dinuclear Cobalt(Ⅱ) Complex [Co_2(α-furacrylato)_4(Phen)_2(H_2O)]·C_2H_5OH

A dinuclear cobalt（II） complex [Co2（a-furacrylato）4（Phen）2（H20）]＇C2HsOH has been synthesized with a-furacrylic acid and 1,10-phenanthroline as the ligands, and its crystal structure was determined. The crystal is of monoclinic system, space group C2/c with a = 1.07388（8）, b = 2.4300（2）, c = 1.86708（14） nm, β= 104.3830（10）°, V= 4.719.4（7） nm3, Dc = 1.503 g/cm3, Z = 2, F（000） = 2196, GOOF = 1.053, the final R = 0.0343 and wR = 0.0883. The crystal structure shows that two neighboring cobalt（II） ions are linked by the bridging coordination of two a-furacrylic acid anions and one water molecule, and their end positions are respectively coordinated with two 1,10-phenanthroline molecules and two a-furacrylic acid anions, forming a dinuclear structure. Both cobalt（II） ions adopt hexa-coordinated distorted octahedral geometry. The electrochemical and fluorescence properties of the title complex are also discussed.

Synthesis, Crystal Structure and Properties of the Cobalt(Ⅱ) Complex of Methyl-5-norbornene-2,3-dicarboxylic Acid

A new cobalt complex Co（C10H8N2）（H2O）3[C9H11O2（COO）] with methy-5-norbor- nene-2,3-dicarboxylic anhydride acid （MNA） and 2,2＇-bipyridine as ligands has been synthesized in the mixed solvents of ethanol and water. It crystallizes in monoclinic, space group P21/c with α = 13.0430（13）, b = 21.014（2）, c = 7.5151（7） ？, β = 102.319（2）o, V = 2012.4（3） A3, Dc = 1.529 g/cm3, Z = 4, F（000） = 964, GOOF = 1.051, the final R= 0.0457 and wR= 0.0974. The crystal structure shows that the cobalt ion is coordinated with four oxygen atoms from one MNA molecule and three water molecules together with two nitrogen atoms from the 2,2＇-bipyridine molecule, forming a distorted octahedral coordination geometry. The thermal stabilityand electrochemical properties have studied in this paper.

Crystal Structure,Electrochemical and Fluorescent Properties of a New Cadmium(II) Complex[Cd(C_(12)H_6O_4N_2)(Phen)_2(H_2O)]·3H_2O

A new Cd（II） complex [Cd（C12H6OaN2）（Phen）ffH2O）]＇3H2O with 2,2＂-bipyridine- 3,3＂-dicarboxylic acid as a ligand has been synthesized. Crystal data for the title complex are as follows： monoclinic, space group P2dn, a = 12.8458（5）, b = 17.9131（7）, c = 15.2960（6） A, β = 111.7430（10）°, V = 3269.3（2） A3, Dc = 1.581 g/cm3, Z = 4,/a（MoKa） = 0.731 mm-1, F（000） = 1580, the R = 0.0244 and wR = 0.0605. In the title complex, the central Cd（ll） ion is located in a distorted octahedral coordination environment. The electrochemical and fluorescent properties of the title complex were studied. The results show that the electron transfer of the title complex is irreversible in the electrode reaction and it has a broad emission peak in the range of 470-508 nm with the excitation wavelength of 488 nm.

Syntheses,Crystal Structures and Electrochemical Properties of Supramolecular Complexes [M_4L_(12)]·(HPO_4)·(PO_4)_2(L=2,2'-Dibenzimidazole,M=Co and Ni)

Two novel supramolecular complexes,[M4L12]·（HPO4）·（PO4）2（L = 2,2＇-dibenzi-midazole,M = Co and Ni） were synthesized by the hydrothermal method and characterized by elemental analysis,IR,UV,and TG-TGA,and the crystal structures were determined by single-crystal X-ray diffraction.The results showed that both of them belong to the cubic system and space group I 4 3d.Crystal parameters of C168H121Co4N48O12P3（1）：a = b = c = 2.5104（6） nm,V = 15.820（7） nm3,Mr = 3332.75,Z = 4,Dc = 1.399 Mg/m3,μ = 0.521 mm-1,F（000） = 6852,S = 1.011,the final R = 0.0248 and wR = 0.0663 for 2120 observed reflections（I 2σ（I）） and R = 0.0315 and wR = 0.0706 for all data.Crystal parameters of C168H121Ni4N48O12P3（2）：a = b = c = 2.4977（5） nm,V = 15.581（5） nm3,Mr = 3331.87,Z = 4,Dc = 1.420 Mg/m3,μ = 0.587 mm-1,F（000） = 6868,S = 1.074,the final R = 0.0443 and wR = 0.1364 for 1774 observer reflections（I 2σ（I）） and R = 0.0647 and wR = 0.1492 for all data.Each of them consisted of four M（II） cations,twelve 2,2＇-dibenzimidazole ligands,one monohydrogen phosphate anion and two phosphate anions in the single cell.The central M（II） cation,coordinated with six alkaline nitrogen atoms from three 2,2＇-dibenzimidazole ligands,displayed the expected distorted-octahedral geometry.The 3D supramolecular system was formed by the hydrogen bond N-H...O and π-π stacking interaction between neighboring single cells.Complex 1 showed two irreversible single-electron reduction processes of the central metal ion at-0.06 and-0.42 V in DMF solution.

Syntheses,Crystal Structures and Electrochemical Properties of Two Molybdophosphates

Two molybdophosphate compounds,[Ni（bim）3]2[H2P2Mo5O23]·2H2O 1 and [Zn（bpy）2]2[Zn（bpy）（H2O）]2Zn[Mo6O12（OH）3（HPO4）4]2·9H2O 2 （bim = 2,2＇-biimidazole,bpy = 2,2＇-dipyridyl）,have been synthesized under hydrothermal conditions and structurally characterized by elemental analysis,TG,and IR. The single-crystal X-ray analysis exhibits that 1 consists of one [H2P2Mo5O23]4-,two [Ni（bim）3]2＋ cations and two lattice water molecules,while 2 is constructed from one sandwich-type [ZnP4Mo6] anion modified by four Zn-bpy complexes and nine lattice water molecules. The electrochemical behaviors of compounds 1 and 2 have been studied in detail based on solid bulk modified carbon paste electrodes of compound （CPEs）.

Syntheses, Crystal Structures, and Electrochemical Properties of Three Anhydrides Based on Ferrocenecarboxylic Acid and Dehydroabietic Acid

Three title compounds(3~5) have been successfully synthesized via interactive reactions between ferrocenecarboxylic and dehydroabietic acids, which can be characterized by FT-IR, elemental analysis, ESI-MS, and NMR spectroscopy. The crystal structures of compounds 4 and 5 can be determined by single-crystal X-ray diffraction. Compound 4 is of orthorhombic system, space group P212121 with a = 7.7010(5), b = 11.7542(9), c = 28.3173(18) ?, Z = 4, V = 2563.3(3) ?~3, Mr = 512.45, Dc = 1.328 g/cm^(-1), S = 1.041, μ = 0.619 mm^(-1), F(000) = 1088, the final R = 0.0396 and wR = 0.0945 for 4394 observed reflections(I > 2σ(I)). Compound 5 crystallizes in orthorhombic system, space group P21212 as well, with parameters of a = 11.9875(15), b = 19.651(2), c = 7.2163(9) ?, Z = 2, V = 1699.9(3) ?~3, Mr = 582.83, Dc = 1.139 g/cm^(-1), S = 1.091, μ = 0.070 mm^(-1), F(000) = 636, the final R = 0.0653 and wR = 0.0719 for 1518 observed reflections(I > 2σ(I)). Additionally, electrochemical properties of compounds 3 and 4 have been investigated by the cyclic and differential pulse voltammogram techniques.

Crystal Structure and Electrochemical, Fluorescent and Magnetic Properties of a New Complex [Ag(2,2ˊ-bipy)(C_(14)H_9O_3)]·(C_(14)H_(10)O_3)

A novel silver（I） complex [Ag（2,2ˊ-bipy）（C14H9O3）]·（C14H10O3） has been synthesized with 2-benzoylbenzoic acid as the ligand. Crystal data for the title complex： monoclinic, space group Cc, a = 27.4089（13）, b = 10.2897（5）, c = 12.0024（6）A, β = 111.864（4）°, Mr = 715.49, V = 3141.5（3） A3, Dc = 1.513 g/cm^3, Z = 4, μ（Mo Kα） = 0.694 mm^-1, F（000） = 1456, the final R = 0.0473 and w R = 0.1146. In the title complex, the central Ag（I） ion is located in a triangular coordination environment. The electron transfer is quasi-reversible in the electrode reaction and it shows a strong emission peak in the range of 495-520 nm under 502 nm excitation. In addition, it displays diamagnetic property from 3 to 300 K.

Hydrothermal Synthesis,Crystal Structure and Electrochemical Properties of Complex [Cd(phen)_3]·(ClO_4)_2·(p-MBA)_2·(H_2O)_2

One new cadmium complex [Cd（phen）3]·（ClO4）2·（p-MBA）2·（H2O）2 has been hydrothermally synthesized by reacting p-methylbenzoic acid （p-MBA）, 1,10-phenanthroline （phen） and cadmium perchlorate. It crystallizes in the triclinic system, space group P1, with a = 1.2809（3）, b = 1.3431（3）, c = 1.3734（3） nm, α = 84.259（4）, β = 71.603（3）, γ = 74.424（3）°, V= 2.1594（8） nm3, Do = 1.532 g/cm3, Z = 2, F（000） = 1008, μ= 0.697 mm^-1, R = 0.0646 and wR = 0.1648. The crystal structure shows that the cadmium ion is coordinated with six nitrogen atoms from three 1,10-phenanthroline molecules, forming a distorted octahedral coordination geometry. The result of electrochemical property analysis shows that the electron transfer in the electrode reaction is irreversible.