Synthesis,Crystal Structure and Electrochemical Property of a Dinuclear Manganese（Ⅱ） Complex [Mn_2（C_（12）H_8N_2）_4（C_8H_5O_4）_2]（C_8H_4O_4）·H_2O

One dinuclear manganese(II)complex [Mn2(C12H8N2)4(C8H5O4)2](C8H4O4)·H2O has been synthesized with o-phthalic acid and 1,10-phenanthroline.The crystal structure was determined by X-ray diffraction.The crystal belongs to the triclinic system,space group P1 with a = 1.17767(3),b = 1.22292(2),c = 1.35860(3)nm,α = 110.5300(10),β = 97.6140(10),γ = 93.7300(10)o,V = 1.80307(7)nm3,Dc = 1.404 g/cm3,Z = 2,F(000)= 784,the final GOOF = 1.047,R = 0.0398 and wR = 0.1038.The crystal structure of the title complex consists of one [Mn2(C12H8N2)4(C8H5O4)2]2+ cation,one uncoordinate o-phthalate anion(C8H4O4)2-and one uncoordinate water molecule.In [Mn2(C12H8N2)4(C8H5O4)2]2+,the central Mn(II)ion is coordinated by four nitrogen atoms and two oxygen atoms to give a distorted octahedral coordination geometry.The electrochemical property of the title complex was also studied.     

CRYSTAL STRUCTURE OF [Ni((C)_6H_(11)O)_2PS_2)·(C_4H_9NH_2)_4]-(C_6H_(11)O)_2PS_2

<正> [Ni((C6H11O)2PS2)·(C4H9NH2)4](C6H11O)2PS2,Mr-=938. 05, triclinic,P1,a=13. 513(6),b=16. 040 (7), c= 12. 891(6) A , α= 95. 66 (4),β= 90. 23(4),γ= 75. 46(3)°,V = 2691 A3,Z=2,Dc= 1. 16 g·cm3.μ=6. 07cm-1,MoKa radiation, λ=0. 71069 A ,F(000) = 1020,R=0. 100 for 4595 reflections with I≥3σ(I). The title compound molecule consists of a complex cation [Ni((C6H11O)2PS2)(C4H9-NH2)4]+ and a complex anion (C6H11O)2PS2- . The Ni (Ⅱ) atom in the cation is octahedrally coordinated by four nitrogen atoms from four w-butylamine ligands and two sulfur atoms from one (C6H11O)2PS2 group.     

Crystal Structure of Copper（ Ⅱ）Complex with 3—Hydroxyl—1,5—diazaylo

Crystal structure of copper (II) complex with a new aminocarboxylate ligand, 3-hydroxyl-1, 5-diazacycloheptane-N,N-diacetate, C9H14CuN2O5.H2O, Mr=311.78 is reported. It crystallizes in orthorhombic Pna21 with a=13.340(4), b=8.127(1), c=10.583(4) , V=1147.2(7)3 , Z=4, Dc=1.805g/cm3, μ=19.287cm-1 (MoKα), F(000)=644. The final R and Rw are 0.049 and 0.065 for 888 observed reflections with I≥3σ(I). The result of X-ray structure determination shows that the Cu(Ⅱ) forms a planar complex with two oxygen atoms and two nitrogen atoms of the ligand.     

Synthesis and Crystal Structure of Bis{2-bromo- 4-chloro-6-[（2-isopropylammonioethylimino）- methyl]phenolato}bisthiocyanatozinc（Ⅱ）

A Schiff base zinc(Ⅱ) complex [Zn(C12H16BrClN2O)2(NCS)2] was prepared and characterized by elemental analysis,IR and single-crystal X-ray diffraction. The crystal belongs to the triclinic system,space group P1 with a=8.414(1),b=9.124(1),c=22.212(3),α=79.177(2),β=86.296(2),γ=89.899(2)o,V=1671.3(4)3,Z=2,Dc=1.631 g/cm3,Mr=820.79,λ(MoKα)= 0.71073,μ=3.444 mm-1,F(000)=824,R=0.0646 and wR=0.1179. A total of 7371 unique reflections were collected,of which 3904 with I > 2σ(I) were observed. The complex crystallizes with two half-molecules per asymmetric unit and each mononuclear molecule is centrosymmetric. The Zn atom lying at the inversion centre is six-coordinated in a slightly distorted octahedral geometry by two phenolate O atoms and two imine N atoms from two Schiff base ligands,as well as two N atoms from two thiocyanate anions. In the crystal structure,the combination of π-π stacking interactions and intermolecular hydrogen bonds (N–H…Br,N–H…O,N–H…N,C–H…O,C–H…S and C–H…Cl) leads to a three-dimensional network.     

Crystal Structure and Magnetic Property of a Two-dimensional Manganese Compound [Mn（PhCOO）2（4,4＇-bipyridine）]n

A new two-dimensional polymeric manganese compound [Mn(PhCOO)2(4,4'-bipyridine)]n 1 has been prepared and structurally characterized by X-ray diffraction. The complex crystallizes in space group Pbcn with a = 18.7158(2), b = 11.6919(3), c = 9.4799(2)(A), V = 2074.42(7)(A)3, Z = 4, Mr = 453.34, Dc = 1.452 g/cm3, μ = 0.670 mm-1 and F(000) = 932. The final refinement gave R = 0.0458 and wR = 0.1439 for 1358 observed reflections with Ⅰ＞ 2σ(Ⅰ). The complex consists of repeating units of Mn(PhCOO)2(4,4'-bipyridine). Each Mn center is sixcoordinated by four carboxylate O atoms of four benzoate anions and two pyridyl N atoms from bipy ligands to furnish a slightly distorted octahedral geometry. The two adjacent Mn atoms are connected by a pair of μ1,3-carboxylate groups to form infinite chains, which are further interlinked by bipy to complete a 2D grid network. The magnetic property of the polymeric complex has also been investigated.     

Synthesis, Crystal Structure and Luminescence Property of a 2D Mn（II） Coordination Polymer Based on Isoniazid

A novel 2D Mn(Ⅱ) coordination polymer [Mn(CH3COO)2(INH)]n(INH=isoniazid) has been synthesized in DMF solution with isoniazid and Mn(CH3COO)2 . The polymer was characterized by single-crystal X-ray diffraction analysis, FTIR and X-ray powder diffraction (XRPD). The crystal belongs to the monoclinic system, space group P2 1 /c with a=9.3251(18), b=16.340(3), c=8.8096(17) , β=94.747(3)°, V=1337.7(4) 3 , Z=4, μ(MoKα)=1.006 mm -1 , F(000)=636, R=0.0754 and wR=0.1375 (I > 2σ(I)). In the complex, each Mn(Ⅱ) atom is coordinated to three CH3COO- groups and two INH ligands. The Mn(Ⅱ) atoms locate in a distorted coordination octahedron and are bridged by CH3COO- ions to form a 1D S shaped chain extending along the c direction. The INH molecules act as bridges to link the Mn(Ⅱ) atoms of adjacent chains and further construct a lamellar polymer. The remaining coordination site is occupied by an O atom of the other CH3COO-. The experimental results show that the title complex has good luminescence property and could be used as potential optical materials.     

One—dimensional Zigzag Chain Coordination Polymer [Zn（μ—phth）（imi）2]∞ Bridged by o—Phthalato

The reaction of zinc carbonate with o-phthalic acid and imidazole in an aqueous-alcohol solution led to the formation of colorless crystals of [Znμ-phthimi2]∞. Single-crystal X-ray analysis has revealed that the complex crystallizes in a monoclinic system, space group Pn with a = 8.394(2), b = 9.976(3), c = 9.959(3)A, β = 104.409(4)°, V = 807.6(4)A3, Z = 2, C14H12N4O4Zn, Mr = 365.6(5), Dc = 1.504 g/cm3, μ = 1.544 mm-1, F000 = 372, the final R = 0.0466 and wR = 0.1171 for 1834 reflections with I>2σ(I). The complex displays a zigzag infinite chain structure in which each zinc(Ⅱ)center is coordinated by two oxygen atoms and two nitrogen atoms to generate a ZnN2O2 distorted tetrahedral geometry. The neighboring zinc atoms are bridged by the o-phthalate ligand. Each chain is linked by hydrogen bonds with its neighbors to form a three-dimensional coordination polymer.     

STRUCTURE OF { CEu_2 (OOCCH_2NHCOCH_2NH_3)_4 (H_2O)_4]·(C1O_4)_6·4H_2O}_n

<正> {[Eu(OOCCH2NHCOCH2NH3)2(H2O)2]·(ClO4)3·2H2O}2,Mr = 1572,P21/n,a=12. 014(4),b=8. 910(5),c=22. 749(5)A ,β=91. 73(3)°,V = 2034 A3,Z=2,Dx=2. 15g·cm-3,λ(MoKa) = 0. 71073A,R=0. 060 for 3107 unique observed reflections (I≥3σ(I)). The complex cation is of one-dimensional chain structure in which the basic unit is a dinuclear complex and the gly-gly ligands are coordinated to metal atoms in two kinds of forms. The overall structure of the dinuclear unit is dioxo and dicarboxyl-bridged.     

Preparation,Crystal Structure,Thermal Decomposition and Explosive Properties of K2（tza）2（H2O） （tza=Tetrazole-1-acetic Acid）

A new energetic compound based on the tetrazole-1-acetic acid (tza) and potassium(I) salt, K2(tza)2(H2O), was synthesized and characterized by elemental analysis and FT-IR spectrum. Its crystal structure was determined by single-crystal X-ray diffraction analysis. The results show that the crystal belongs to the orthorhombic system, space group Pna21 with a = 1.11972(17) nm, b = 0.46647(7) nm, c = 2.5158(4) nm, V = 1.3140(3) nm3, K2C6H8N8O5, Mr = 350.40 g·mol-1, Dc = 1.771 g·cm-3, μ(MoKα) = 0.759 mm-1, F(000) = 712, Z = 4, R = 0.023 and wR = 0.0527 for 2961 observed reflections (I > 2σ(I)). The K(I) cation is six-coordinated with four O atoms from three carboxylate groups, one O atom from one H2O molecule and one N atom from tetrazolyl ring, in which each tza is coordinated in a tridentate chelating bridging coordination mode. The thermal decomposition mechanism of the title complex was studied by DSC and TG-DTG techniques. Under nitrogen atmosphere at a heating rate of 10 K·min-1, the thermal decomposition of the complex contains one main exothermic process between 191.7 and 243.8 ℃ in the DSC curve. Its combustion heat was mensurated by oxygen bomb calorimetry. The non-isothermal kinetics parameters were calculated by the Kissinger's method and Ozawa-Doyle's method, respectively. The sensitivity properties of K2(tza)2(H2O) were also determined with standard methods, which was very sensitive to flame.     

Synthesis and Structure Characterization of a Tetranuclear Manganese(Ⅲ) Complex:[Mn4O2(O2CMe)6(MeOH)2(dbm)2]·2MeCOOH·2CH2Cl2

The title compound, [Mn4O2(O2CMe)6(MeOH)2(dbm)2]·2MeCOOH·2CH2Cl2 (Hdbm = dibenzoylmethane), has been synthesized and structurally determined by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P(-l), with a = 10.729(3), b = 12.269(3), c =13.085(4) (A), a = 106.367(3), β = 107.643(2), γ = 94.771(2)°, V = 1547.9(7) (A)3, Z = 1,C50H64Cl4Mn4O24, Mr= 1410.57, Dc= 1.513 g/em3, F(000) = 724, Rint = 0.0147, T = 293(2) K and μ = 1.046 mm-1. The fimal R = 0.0359 and wR = 0.0938 for 5791 observed reflections with I ＞ 2( )I).The structure of the complex consists of one [Mn4(μ3-O)2]8+ core with four coplanar Mn atoms disposed in an extended "butterfly-like" arrangement and two O atoms triply bridging each "wing",and the peripheral ligation is provided by six μ2-MeCO2-, two terminalμ2-dbm- groups at the two hydrogen bonding interactions are found within the structure of the compound.     

Crystal Structure and Magnetic Property of a Two-dimensional Manganese Compound [Mn(PhCOO)_2(4,4'-bipyridine)]_n

A new two-dimensional polymeric manganese compound [Mn(PhCOO)2(4,4'-bi-pyridine)]n 1 has been prepared and structurally characterized by X-ray diffraction. The complex crystallizes in space group Pbcn with a = 18.7158(2), b = 11.6919(3), c = 9.4799(2) , V = 2074.42(7) 3, Z = 4, Mr = 453.34, Dc = 1.452 g/cm3, μ = 0.670 mm-1 and F(000) = 932. The final refinement gave R = 0.0458 and wR = 0.1439 for 1358 observed reflections with I > 2σ(I). The complex consists of repeating units of Mn(PhCOO)2(4,4'-bipyridine). Each Mn center is six-coordinated by four carboxylate O atoms of four benzoate anions and two pyridyl N atoms from bipy ligands to furnish a slightly distorted octahedral geometry. The two adjacent Mn atoms are connected by a pair of μ1,3-carboxylate groups to form infinite chains, which are further interlinked by bipy to complete a 2D grid network. The magnetic property of the polymeric complex has also been investigated.     

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 and Structure Characterization of a Tetranuclear Manganese(Ⅲ) Complex:[Mn_4O_2(O_2CMe)_6(MeOH)_2(dbm)_2]·2MeCOOH·2CH_2Cl_2

The title compound, [Mn4O2(O2CMe)6(MeOH)2(dbm)2]·2MeCOOH·2CH2Cl2 (Hdbm = dibenzoylmethane), has been synthesized and structurally determined by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P1, with a = 10.729(3), b = 12.269(3), c = 13.085(4) , α = 106.367(3), β = 107.643(2), γ = 94.771(2)o, V = 1547.9(7) 3, Z = 1, C50H64Cl4Mn4O24, Mr = 1410.57, Dc = 1.513 g/cm3, F(000) = 724, Rint = 0.0147, T = 293(2) K and μ = 1.046 mm–1. The final R = 0.0359 and wR = 0.0938 for 5791 observed reflections with I > 2σ(I). The structure of the complex consists of one [Mn4(μ3-O)2]8+ core with four coplanar Mn atoms disposed in an extended “butterfly-like” arrangement and two O atoms triply bridging each “wing”, and the peripheral ligation is provided by six μ2-MeCO2– , two terminal μ2-dbm– groups at the two ends of the molecule, and two MeOH molecules on the central Mn atoms. Intermolecular O…H–O hydrogen bonding interactions are found within the structure of the compound.     

Synthesis and Crystal Structure of a New Complex [Cu（C_（14）H_9O_3）_2（C_5H_5N）_2（C_2H_5OH）_2]

The title compound of Cu(C14H9O3)2(C5H5N)2(C2H5OH)2(1) was synthesized via the hy- drothermal reaction of CuCl2·2H2O and 9-hydroxy-fluorene-9-carboxylic acid(HHF) with pyridine, and characterized by elemental analysis and infrared spectra. The crystal belongs to triclinic, space group P1 with a = 8.8302(12), b = 10.1625(14), c = 12.2708(17), α = 86.207(2), β = 69.562(2), γ = 64.932(2)o, V = 930.3(2) 3, Z = 1, Mr = 764.30, Dc = 1.364 g/cm3, F(000) = 399, S = 1.059 and μ(MoKα) = 0.644 mm-1. The final R = 0.0459 and wR = 0.1274 for 3414 observed reflections with I 2σ(I). The copper atom is six-coordinated by two oxygen atoms from two different 9-hydroxy-fluorene-9-carboxylate ligands, two pyridine nitrogen atoms and two ethanol oxygen atoms, forming a distorted octahedral coordination geometry. The extensive O–H···O hydrogen bonding connects the molecules to form a one-dimensional chain structure. Between adjacent one-dimensional chains, a two-dimensional layered structure was formed by fluorene ring π-π packing interaction. Between the layers, a three-dimensional structure was formed through the π-π packing interaction of the pyridine ring. Moreover, the thermal stability and photoluminescent property of the complex has been investigated.     

Synthesis and Crystal Structure of 3,3＇-Bis（2-benzimidazolyl）-2,2＇-dipyridine with Hydrated Zinc（Ⅱ） Perchlorate

The reaction of Zn(ClO4)2·6H2O with 3,3'-bis(2-benzimidazolyl)-2,2'-dipyridine (L) gave a mononuclear zinc(II) complex: [ZnL2](ClO4)2·2DMF·4H2O, which was structurally characterized by EA, IR, UV, 1H NMR, fluorescence spectrum and single-crystal X-ray diffraction. The crystal (C54H54Cl2N14O14Zn, Mr = 1259.38) belongs to the monoclinic system, space group C2/c with a = 20.874(2), b = 14.9953(16), c = 20.462(3) , β = 101.553(2)°, V = 6274.8(13) 3, Z = 4, Dc = 1.333 g/cm3, F (000) = 2608, μ(MoKα) = 0.548 mm–1, R = 0.0682 and wR = 0.1931 for 4984 observed reflections with I > 2σ(I). The Zn(II) is four-coordinated in a slightly distorted tetrahedral geometry through four N atoms from four benzimidazole units of two ligands. In the crystal lattice, the [ZnL2]2+ cations are linked to each other by extensive intermolecular hydrogen bonds between nitrogen atoms of benzimidazole rings, water and DMF molecules.     

Synthesis, Crystal Structure and Electrochemical Properties of a One-dimensional Chain Coordination Polymer [Mn（phen）（2,4,6-TMBA）2（H2O）]n

A one-dimensional chain-like coordination polymer [Mn(phen)(2,4,6-TMBA)2(H2O)]n has been synthesized from 2,4,6-trimethylbenzoic acid, 1,10-phenanthroline and anhydrous manga- nese(Ⅱ ) sulfate and then characterized. Crystal data for this complex: tetragonal, space group I41, a = 2.05643(16), b = 2.05643(16), c = 1.3939(2) nm, V = 5.8946(11) nm3, Mr = 579.54, Z = 8, Dc = 1.306 g/cm3, μ(MoKα) = 0.490 mm-1, F(000) = 2424, S = 0.985, the final R = 0.0411 and wR = 0.0950. The Flack factor is -0.01(2). The crystal structure shows that two neighboring man- ganese(Ⅱ ) ions are linked together by one bridge-chelating 2,4,6-trimethylbenzoic group, forming a one-dimensional chain structure. The manganese(Ⅱ ) ion is coordinated with two nitrogen atoms of one 1,10-phenanthroline, three oxygen atoms from three 2,4,6-trimethylbenzoic acids and one water oxygen atom, giving a distorted octahedral coordination geometry. The cyclic voltametric behavior of the complex was also investigated.     

Synthesis and Crystal Structure of (CH2)3(3, 5-Me2Pz)2·[PhBr2Sn(CH2)SnBr2Ph]·2HBr·2H2O (Pz = pyrazole)

The reaction of bis(dibromophenylstannyl)methane with 1, 3-bis(3, 5-dimethyl- pyrazol-1-yl)propane in a 1:1 or 1:2 ratio yields only 1:1 adduct which partly hydrolyzes to the title complex (C26H38Br6N4O2Sn2, Mr = 1155.42) during crystal growing. The title complex is of triclinic, space group P ī with a = 10.886(1), b = 12.508(1), c = 13.879(1) ?, α = 85.762(2), β = 85.159(2), γ = 84.020(2)°, V = 1868.8(4) ?3, Z = 2, Dc = 2.046 g/cm3, λ(MoKα) = 0.71073 ?, μ = 7.778 mm-1, F(000) = 1088, R = 0.0488 and wR = 0.1157 for 7560 observed reflections with I ≥ 2σ(I). The crystal structure analysis indicates that there is no direct interaction between the ligand and bis(dibromophenylstannyl)methane, and two tin atoms are bridged by two bromide atoms from the partial hydrolysis of this adduct.     

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.     

Synthesis,Crystal Structure and Luminescent Property of Cadmium Complex Based on 2-（2-（1Hbenzo[d]imidazol-2-yl）benzyl）-1H-benzo[d]-imidazole

The complex [Cd(bbb)Cl2]·DMF·H2O, where bbb is 2-(2-(1H-benzo[d]imidazol-2-yl)benzyl)-1H-benzo[d]imidazole, was synthesized and characterized by X-ray single-crystal structure analyses. For the complex: C24H25Cl2CdN5O2, Mr = 598.77, crystal system, triclinic, space group P1, a = 9.9878(12), b = 10.0008(12), c = 13.2217(15) , α = 80.674(2), β = 72.158(2), γ = 86.776(2)°, V = 1240.5(3) 3, Z = 2, Dc = 1.598 g/cm3, λ = 0.71073, μ(MoKα) = 1.127 mm–1, F(000) = 600, S = 1.04, R = 0.0905 and wR = 0.3088 for 4805 observed reflections with I 2σ(I). It is a neutral complex. The distorted tetrahedral geometry of cadmium ion is coordinated by two nitrogen atoms of ligand and two chloride ions. The complex emits blue green luminescence with emission peaks at 480 nm in DMF solution.     

Synthesis,Structure and Near-infrared Photoluminescent Property of a Tetranuclear Er(Ⅲ) Complex

A tetranuclear erbium complex with pyridine-2,4,6-tricarboxylic acid(H3ptc), [Er4(ptc)4(H2O)18]·6H2O(1), has been synthesized by hydrothermal method. The complex crystallizes in triclinic system, space group P1, with a = 7.620(2), b = 10.459(3), c = 17.418(5) ?, α = 92.351(5), β = 92.080(5), γ = 95.627(4)°, V = 1379.1(7) ?3 and Z = 2. One Er(III) cation is eight-coordinated and the other is nine-coordinated. The complex exhibits characteristic luminescence of erbium cation in near-infrared region upon the excitation of UV-rays. Furthermore, a three-dimensional supramolecular complex was formed by weak hydrogen bonds among the tetranuclear units.