Hydrothermal Synthesis and Crystal Structure of a Zinc Complex:[Zn_(2.5)(phen)(BDC)_2(OH)] (phen = 1,10-Phenanthroline, BDC = Benzene-1,4-dicarboxylic Acid)

A metal-organic coordination polymer [ZnE.s（phen）（BDC）2（OH）]2 （phen = 1,10- phenanthroline, BDC = benzene-1,4-dicarboxylic acid） 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses and IR spectroscopy. The complex crystallizes in the triclinic system, space group PI with a = 11.199（2）, b = 11.593（2）, c = 11.865（3）/A, α= 99.330（1）, β = 111.506（1）, γ = 104.804（1）^o, V= 1328.4（5）A^3, Dc= 1.722 g/cm^3, Z = 1, Mr = 1377.82, F（000） = 692,μ（MoKa） = 2.306 mm^-1, S = 1.093, R= 0.0281 and wR = 0.0756 for 4179 observed reflections （I 〉 2σ（/））. The coordination polyhedron around Zn（II） can be described as a tetrahedron, trigonal bipyramid and octahedron. It is worth noting that the crystal structure of 1 is composed of tetranuclear zinc clusters linked by {ZnO6} units.

Hydrothermal Synthesis,Crystal Structure and Thermal Stability of a Binuclear Copper(Ⅱ) Complex with 3-(Pyridin-2-yl)-1,2,4-triazole

One novel binuclear copper（Ⅱ） complex [Cu 2 （Hpt） 2 （CO 3） 2 （H 2 O） 2 ]·H 2 O with copper carbonate and 3-（pyridin-2-yl）-1,2,4-triazole （Hpt） was hydrothermally synthesized and characterized by IR and X-ray diffraction analysis.The complex crystallizes in triclinic,space group P2 1 /n with a=0.6862（1）,b=0.7805（1）,c=1.1983（2） nm,α=72.03（2）,β=107.72（3）,γ=75.28（2）o,V=0.5884 nm 3,D c=2.105 g/cm 3,Z=1,F（000）=357,GOOF=1.041,the final R=0.01859 and wR=0.04348.The whole molecule is composed of two cooper ions,two Hpt molecules,two carbonate and three water molecules,forming a binuclear structure.The crystal structure shows that the cooper ion is coordinated with three nitrogen atoms from two Hpt molecules,two oxygen atoms from one carbonic acid and one water molecule,forming a distorted square pyramidal geometry.The TG analysis result shows that the title complex is stable under 131.0 ℃.

Hydrothermal Synthesis, Crystal Structure and Fluorescent Property of a Cd(Ⅱ) Complex Based on Biimidazole and Isonicotinate-N-oxide

A new complex [Cd（H2biim）2（H2O）2]·（ino）2·4H2O （H2biim = 2,2＇-biimidazole, ino = isonicotinate-N-oxide） has been prepared and characterized by single-crystal X-ray diffraction analysis, IR and fluorescence spectra analysis. The crystal is of triclinic system, space group P1 with a = 7.5380（6）, b = 8.0402（7）, c = 13.5094（11） , α = 104.269（1）, β = 93.604（1）, γ = 98.349（1）°, V = 780.93（11） 3, Mr = 765.00, Dc = 1.627 g/cm3, F（000） = 390, μ = 0.776 mm-1 and Z = 1. The final R = 0.0322 and wR = 0.0825 for 7038 observed reflections with I 2σ（I） and R = 0.0341 and wR = 0.0832 for all data. The title complex exhibits an infinite chain-like structure through bridging isonicotinate-N-oxide. Strong interchain hydrogen bonds between isonicotinate-N-oxide and H2biim result in the robust 3-D supramolecular architecture. Moreover, the complex shows strong photoluminescence with emission maximum at λ = 401 nm upon λex = 330 nm.

Hydrothermal Synthesis,Crystal Structure and Thermal Analysis of a Dinuclear Complex Cd_2(3,5-Dinitrobenzoate)_4(pyridine)_4

A dinuclear complex Cd2（dnba）4（pyridine）4 （dnba = 3,5-dinitrobenzoate） has been synthesized by hydrothermal method and characterized by X-ray single-crystal diffraction, elemental analysis, FT-IR spectroscopy, DSC and TG-DTG techniques. The complex with empirical formula C48H32Cd2NI2024 （Mr = 692.83） crystallizes in monoclinic, space group P21/n with a - 12.0344（14）, b = 10.5752（13）, c = 21.578（3） A, β = 104.150（2）°, V = 2662.8（6） A^3, Z = 2, D, = 1.728 g/cm^3,μ（MoKa） = 0.897 mm^-1, F（000） = 1384, S = 1.016 and （△/σ）max = 0.001. R = 0.0638 and wR = 0.0737 for all data; the final R = 0.0337 and wR = 0.0644. In this complex, four carboxylates are bidentate-or chelate-coordinated with the Cd（Ⅱ） centers to give the dinuclear structure. The other coordination positions of Cd（Ⅱ） are occupied by the lone pair electrons from N of four pyridines. Thermal analyses DSC and TG-DTG have been used to determine the thermal decomposition mechanism of the title complex.

Hydrothermal Synthesis, Crystal Structure and Photoluminescent Property of a Zinc(II) Complex with 2,2′-Diphenic Acid and 2,2′-Bipyridine Ligands

A new dinuclear complex [Zn（dpa）（bipy）（H2O）]2 （dpa = 2,2＇-diphenic acid, bipy = 2,2＇-bipyridine） 1 has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, fluorescence spectrum and single-crystal X-ray diffraction. The complex crystallizes in monoclinic, space group P21/c with a = 10.960（2）, b = 9.4841（18）, c = 20.599（4）, β = 104.452（3）o, V = 2073.4（7）3, C48H36N4O10Zn2, Mr = 959.55, Dc = 1.537 g/cm3, μ（MoKα） = 1.225 mm-1, F（000） = 984, Z = 2, the final R = 0.0364 and wR = 0.0843 for 2788 observed reflections （I 〉 2σ（I））. In the crystal structure, the zinc atom is five-coordinated with two carboxylate oxygen atoms from different dpas, one coordinated water molecule and two nitrogen atoms from bipy ligands, showing a slightly distorted triangular bipyramidal geometry. Furthermore, it exhibits a zero-dimensional network structure with a sixteen-membered ring and shows yellow photoluminescent property at room temperature.

Hydrothermal Synthesis, Crystal Structure and Fluorescence Properties of a Three-dimensional Triply-bridged Binuclear Zinc(Ⅱ) Complex [Zn_2(Mba)_3(Phen)_2EtOH)]·ClO_4

The novel complex [Zn2（Mba）3（Phen）2EtOH）]·ClO4 （Hrnba = methoxybenzoic acid, Phen = 1,10-phenanthroline, EtOH = ethanol） was synthesized by hydrothermal reactions, and its structure was determined by X-ray diffraction. The crystal belongs to the triclinic system, space group Pi with a = 1.15362（1）, b = 1.3655（3）, c = 1.61451（1） nm, α= 72.842（2）, β = 83.259（3）, y = 72.083（2）°, V = 2.3112（6） nm3, Z = 2,μ（MoKa） = 11.71 cm-1, F（000） = 1120, R = 0.0552 and wR = 0.1157 （I 〉 2σ（I））. The two centric zinc（H） ions in the complex locate in a distorted octahedral coordination geometry and a distorted trigonal bipyramid coordination geometry, respectively. Two bridging bidentate carboxyl groups and a μ2-O carboxyl group from three methoxybenzoic acids act as the bridge to link two Zn（Ⅱ） ions. The asymmetric units are connected by π-π packing interactions between aromatic rings to form a three-dimensional supramolecular network. The experimental results show a good fluorescence property for the complex.

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 Manganese(Ⅱ) Complex:Mn_(1.5)(cbba)_3(phen)

A new metal-organic complex Mn1.5（cbba）3（phen）（Hcbba = 2-（4＇-chlorine-ben-zoyl）benzoic acid,phen = 1,10-phenanthroline） 1 has been hydrothermally synthesized and struc-turally characterized by single-crystal X-ray diffraction,elemental analyses,TG and IR spectro-scopy.The compound crystallizes in triclinic,space group P1 with a = 12.137（2）,b = 14.535（3）,c = 14.894（3）,α = 86.380（3）,β = 70.381（3）,γ = 72.647（3）°,V = 2360.3（8）3,C107H64Cl6Mn3N4O18,Mr = 2071.14,Dc = 1.457 g/cm3,μ（MoKα） = 0.638 mm-1,F（000） = 1055,Z = 1,the final R = 0.0638 and wR = 0.1905 for 6155 observed reflections（I 2σ（I））.It exhibits a 3D supramolecular network through hydrogen bonding and π-π stacking interactions.

Hydrothermal Synthesis and Crystal Structure of a Novel Dinuclear Co(Ⅱ) Complex:[Co2(2,2'-bpy)_2(μ-L)_2(L)_2(μ-H_2O)](HL=4-Chlorobenzoic Acid)

A new 4-chlorobenzoic acid bridge Co（Ⅱ ） complex [[Co2（2,2＇-bpy）2（μ-L）e（L）2（μ-H2O）] （HL = 4-chlorobenzoic acid） has been obtained by hydrothermal synthesis, and X-ray single-crystal diffraction analysis shows that it crystallizes in the monoclinic system, space group C2/c with a = 22.537（5）, b = 16.212（3）, c = 15.306（3） A, β= 124.37（3）°, V= 4616.1（16）A3, Mr = 1070.45, Dc = 1.540 g/cm3, Z = 4, p = 1.012 mm-1, F（000） = 2176, the final R = 0.0338 and wR= 0.0810. The title complex is composed of dinuclear [Co2（2,2＇-bpy）2（μ-L）2（L）2（μ-HaO）] molecules. Each Co（Ⅱ ） atom is coordinated by two nitrogen atoms from one 2,2’-bipyridine ligand, three oxygen atoms from three 4-chlorobenzoic ions and another oxygen atom from one water molecule. The two Co（Ⅱ） atoms are connected by two 4-chlorobenzoic ions and one bridged water molecule. The dinuclear molecules are interlinked by hydrogen bond and π-π stacking interactions into a three-dimensional supramolecular network.

Hydrothermal Synthesis, Crystal Structure and Luminescence Properties of a New 2D Cadmium Complex Based on the 4,4'-Bis(benzimidazol-1-ylmethy1)biphenyl and Glutaric Acid Ligands

A new polymeric complex {[Cd2（bbmb）2（gt）2]＇（H2O）2}, （bbmb = 4,4＇-bis（benzimidazol-l-ylmethyl）biphenyl, H2gt = glutaric acid） has been obtained by hyclrothermal method and structurally characterized by elemental analysis, IR, XRD, TGA and single-crystal X-ray diffraction. The complex belongs to the triclinic system, space group P1 with a = 10.2417（15）, b = 13.752（2）, c = 22.201（3） A, a = 73.899（2）, β = 88.416（2）, y = 78.305（2）°, V = 2940.4（7） A3, Z = 2, C66H56Cd2N808, Mr = 1313.99, Dc = 1.484 g/cm3, F（000） = 1336 and μ = 0.787 mm-1, and features a 2D network. In the solid state at room temperature, the cadmium（Ⅱ） complex exhibits strong fluorescence absorption at 435 nm （λmax）.

Hydrothermal Synthesis, Crystal Structure and Electrochemical Properties of Complex Zn(phen)(m-CBA)_2(H_2O)

A novel complex Zn（phen）（m-CBA）2（H2O） with m-chlorobenzoic acid （m-CBA）, 1,10-phenanthroline （phen） and zinc chloride has been hydrothermally synthesized and characterized. Crystal data for this complex： triclinic, space group P1^-, a = 0.8361（5）, b = 1.2455（7）, c = 1.3107（7） nm, α = 115.637（8）, β = 91.014（9）, γ = 104.857（8）°, V = 1.1763（11） nm^3, Dc = 1.623 g/cm^3, Z = 2, F（000） = 584, GOOF = 1.078, the final R = 0.0453 and wR = 0.1192. Structure analysis shows that the zinc ion coordinates with two nitrogen atoms of one 1,10-phenanthroline molecule, three oxygen atoms from two m-chlorobenzoic acid molecules and one water molecule, giving a distorted square-pyramidal coordination geometry. The cyclic voltametric behavior of the complex was also investigated.

Hydrothermal Synthesis and Crystal Structure of Complex Mn_2(phen)_2(p-MBA)_4(H_2O)

A novel Mn（Ⅱ） complex Mn2（phen）2（p-MBA）4（H2O） has been hydrothermally synthesized by the reaction of p-methyl benzoic acid （p-MBA） with 1,10-phenanthroline （phen）. Crystal data for this complex： monoclinic, space group C2/c, a= 2.3328（3）, b =1.5549（2）, c = 1.5557（2） nm, β = 121.726（2）°, V= 4.7997（11） nm^3, Mr = 1028.85, Dc = 1.424 g/cm^3, Z = 4, F（000） = 2128, μ（MoKa） = 0.590mm^-1, GOOF = 1.060, R = 0.0333 and wR = 0.0767. In the crystal, each Mn（Ⅱ） ion is coordinated by two nitrogen atoms from one o-phenanthroline molecule, three oxygen atoms from three p-methyl benzoic acids and one oxygen atom from one water molecule, giving a six-coordinate distorted octahedral coordination geometry. Two neighboring Mn（Ⅱ） ions are bridged by two p-methyl benzoic acid groups and one water molecule, and their end positions are respectively coordinated by one 1,10-phenanthroline and one p-methyl benzoic acid molecule, giving a binuclear cage structure, of which the Mn（Ⅱ）…Mn（Ⅱ） distance is 0.3502 nm.

A Layered Vanadium Oxide with Cobalt(Ⅱ) Coordination Complex: Hydrothermal Synthesis and Crystal Structure of (py)_5Co_2(H_2O)_3[V_4O_(12)]

A novel layered mixed metal vanadium-cobadt complex, （py）5Co2（H2O）3[V4O12] 1 （py = pyridine）, was hydro（solvo）thermally synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in orthorhombic, space group Pca21 with a = 17.473（4）, b = 11.447（2）, c = 17.509（4）A^°, V = 5005.3（7）A^°3, Z = 4, Mr = 3502.1（12）, Z = 4, Dc = 1.827 g/cm^3,μ（MoKα） = 2.023 mm^-1, F（000） = 1928, S = 1.020, the final R = 0.0400 and wR= 0.1063 for 6035 observed reflections with I 〉 2σ（I） and 460 variables. Complex 1 consists of tetrahedral VO4 groups to form the large layers which are alternately bonded by two cobalt complex species Co（py）2（H2O）2 and Co（py）3（H2O）.

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.

Hydrothermal Synthesis, Crystal Structure and Magnetic Properties of a Novel Zero-dimensional Manganese(Ⅱ) Complex with 2,2′-Diphenic Acid and 1,10-Phenanthroline Ligands

A novel metal-organic coordination polymer [Mn3（2,2′-dipha）3（phen）6]n·3nH2O （2,2′-dipha = 2,2′-diphenic acid, phen = 1,10-phenanthroline） 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses, IR spectroscopy, and magnetic susceptibility measurements. The crystal crystallizes in triclinic, space group P1 with a = 16.921（5）, b = 18.307（5）, c = 18.450（5）A , α = 113.369（5）, β = 108.529（5）, γ = 102.984（5）°, V = 4553（2）A^ 3, C114H72Mn3N12O14.25, Mr = 2002.66, Dc = 1.461 g/cm^3, μ（MoKα） = 0.488 mm^-1, the final F（000） = 2058, Z = 2, R = 0.0491 and wR = 0.0980 for 9087 observed reflections （I 〉 2σ（I））. In the crystal structure, the manganese atom is six-coordinated with two carboxylate oxygen atoms from different carboxylate groups of the same dipha and four nitrogen atoms from two different phen ligands, showing a slightly distorted octahedral geometry. Fur- thermore, it exhibits a zero-dimensional structure with dipha-Mn-phen- as building units. Variable- temperature magnetic measure shows an overall anti-ferromagnetic behavior for compound 1.

HETERONUCLEAR COMPLEX CONTAINING COPPER-LANTHANIDE ARRAYS: THE SYNTHESIS AND CRYSTAL STRUCTURE OF Ln_2Cu_4L_8 (HL)_4(OH)_2(CIO_4)_4(H_2O)_(10)·2CH_3COCH_3 (Ln = Tb (1), Y (2); HL = 2-Pyridone C_5H_5NO)

Reaction of 2-pyridone, copper acetate and terbium(or yttrium) perchlorate in acetone with the mole ratio 6: 2: 1 results in the formation of heteronuclear complex Ln_2Cu_4L_8 (HL)_4 (OH)_2 (ClO_4)_4 (H_20)_(10) 2CH_3COCH_3(Ln = Tb (1), Y (2)). By recrystallizing (1) in CHCl_3 single crystals were obtained and the structure was determined by four-circle diffractometer. Data showed that the crystal is in space group C2/m with a=27. 454(9)A, b=13, 608A, c=30. 556(11)A, β=99. 89(3)°, v=11245. 7(7. 5)A^3. The structure was solved by a combination of Patterson method and Fourier technique. The final R value is 0. 103. In the structure, four copper and two terbium ions are bridged by 2-pyridone anions to form an essentially octahedral Cu_4Tb_2 core. The terbium atoms are each eight-coordinate and the copper atoms are five-coordinate.

STUDIES ON SOLID STATE REACTIONS OF COORDINATION COMPOUNDS(LXⅡ)Solid state synthesis and crystal structure of the complex ICu_(0.84)Au_(0.16)(PPh_3)_2(SC(Ph)NHPh)CIJ·0.5CS_2

[Cu_(0.84)Au_(0.16)(PPh_3)_2(SC(Ph)NHPh)Cl]·0.5CS_2=,Mr=895.79,monoclinic,space group P2_1/a,a=17.231(3),b=14.611(2),c=18.000(3) ,β=105.56(2)°,V=4365(1) ~3, Z=4,D_c=1.37g/cm^3.,λ(MoK_α)=0.71073 ,μ=12.15cm^(-1),F(000)=1855,R=0.052, R_W=0.045 for 3930 observed reflections with Ⅰ>1.5σ(Ⅰ).The central metal atom has a dis. torted tetrahedral geometry with bond lengths Cu-S=2.384(2) (Au-S=2.389(4)), Cu-Cl=2.481(3)(Au-Cl=2.474(1))and Cu-P=2.269(2)-2.289(2)(Au-P=2.270(4)-2.279(4)) .

A Novel Organic-Inorganic Complex: Synthesis and Crystal Structure of [Ca(DMSO)_5(H_2O)]_2SiMo_(12)O_(40)

A novel organic-inorganic complex [Ca(DMSO)5(H2O)]2SiMo12O40 was synthesized from CaCl2, DMSO and H4SiMo12O40nH2O in mixed solvent of acetonitrile and water. Its structure was characterized with elemental analysis, IR and X-ray diffraction analysis.

Hydrothermal Synthesis,Crystal Structure and Antimicrobial Activity of a New Ni(Ⅱ) Complex

The title complex [NiL]·H2O（C20H24N2NiO5,L = paeonol-ehylenediamine） was synthesized by the hydrothermal method and characterized by IR,cyclic voltammetry and X-ray single-crystal diffraction.The complex belongs to the monoclinic system,space group P21/c with a=13.4361（13）,b=7.3290（10）,c=20.981（2）,β=109.244°,V=1950.6（4）3,Z=4,F（000）=904,Dc=1.468 g/cm3,μ（MoKα）=1.029 mm-1,the final R=0.0588 and wR=0.1577.The complex exhibits antimicrobial activities（antimicrobial activities against Staphylococcus aureus and Escherichia codi） by agar diffusion measurement.