Hydrothermal Synthesis and Crystal Structure of a New Supramolecular Channel Framework Based on Cu Complexes and Polyoxovanadate:[Cu(I)(phen)_2]_5[HV_(15)O_(36)(Cl)]_(0.65)[H_3V_(16)O_(38)(Cl)]_(0.35)·2H_2O

A new compound [Cu（I）（phen）2]5[HV15O36（Cl）]0.65[H3V16O38（Cl）]0.35·2H2O 1 （phen = 1,10′-phenanthroline） has been prepared from the hydrothermal reaction of V2O5, CuCl, phen, H2C2O4·2H2O, THMAM （tris（hydroxymethyl）aminomethane） and H2O in the molar ratio of 3：1：1：0.5：2.5：1400. Compound 1 crystallizes in the space group P42212 of the tetragonal system with a = b = 21.5009（8）, c = 28.401（2） A, V= 13129.5（12） A^3 Z = 4, Dc = 1.800 g/cm^3, μ（MoKa） = 1.932 mm^-1, λ（MoKa） = 0.71073 A, F（000） = 7063.4, C120H81.20ClCu5N20O38.7V15.35, Mr = 3557.58, the final R = 0.0594 and wR= 0.1320 for 7761 observed reflections （I 〉 2σ（I））. Structure analysis shows that 1 exhibits a 3D channel framework formed by the supramolecular assembly of Cu complexes and polyoxovanadate clusters via intermolecular hydrogen bonding, and the channels contain Cu complexes. Other characterizations by elemental analysis, XPS, IR, XRD and thermal analysis are also described.

Hydrothermal Synthesis and Crystal Structure of a New Polyoxovanadate:[Mn(en)_3]_2en_(0.5)[HV_8~ⅤV_8~ⅣO_(38)(Cl)]·4.5H_2O(en=Ethylenediamine)

A new compound has been synthesized under hydrothermal conditions and characterized by IR, elemental analysis, XPS and single-crystal X-ray diffraction analysis. The title compound [Mn（en）3]2en0.5[HV8VV8IVO38（CI）]·4.5H2O crystallizes in monoclinic, space group C2/c, with a = 17.016（4）, b = 18.858（4）, c = 18.872（4） A, β = 93.667（4）°, V = 6043（2）A3, Z = 4, Dc = 2.242 g/cm3, Mr = 2040.12, F（000） = 4020,μ = 2.895 mm-1, Rint = 0.0921, R = 0.0649 and wR = 0.1325. Single-crystal X-ray structure analysis indicates that the title compound consists of a polyanion [HV8VV8IVO38（CI）]4- cage, two [Mn（en）3]2^2＋ cations, four and a half lattice waters and a half ethylenediamine. In addition, intermolecular O-H...N, O-H...O, N-H...O and C-H...O hydrogen bonds link the molecules together to form a three-dimensional structure.

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 Photoluminescent Property of a Zinc(II) Coordination Polymer Assembled by Phthalate and 4,4′-Bipyridine

A metal-organic coordination polymer {[Zn（Pht）（4,4＇-bipy）（H2O）2]·2H2O}n （Pht = phthalate, 4,4＇-bipy = 4,4＇-bipyridine） 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. Yellow crystals crystallize in the monoclinic system, space group P2/n, a = 7.6346（14）, b = 11.316（2）, c = 10.8133（19） ,A, β = 92.A.A,A.（3）°, V = 933.3（3） A^3, C18H20N2O8Zn, Mr = 457.73, Dc = 1.629 g/cm^3, F（000） = 472, Z = 2,μ（MoKa） = 1.367 mm^-1, the final R = 0.0323 and wR = 0.0821 for 1859 observed reflections （Ⅰ〉 2σ（Ⅰ））. The structure of 1 exhibits a two-dimensional bilayer framework formed by hydrogen bonding interactions. Furthermore, 1 shows yellow photoluminescent property at room temperature.

Hydrothermal Synthesis, Crystal Structure and Photoluminescent Property of a New Isophthalate- bridged Zinc(II) Polymer with One-dimensional Chain Structure: [Zn(ipt)(im)_2]_(2n)·3nH_2O (ipt = Isophthalate, im = Imidazole)

A new metal-organic coordination polymer [Zn（ipt）（im）2]2n·3nH2O 1 has been obtained by using hydrothermal synthesis and characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. The complex crystallizes in monoclinic, space group P2（1/n） with a = 10.653（3）, b = 17.891（6）, c = 10.743（4）A^°,β= 117.093（5）°, V= 1822.9（10） A^°3, Mr= 413.65, Dc = 1.507 g/cm^3,/t（MoKa） = 1.390 mm^-1, F（000） = 840, Z = 4, the final R = 0.0444 and wR = 0.1066 for 2434 observed reflections （I〉 2σ（I））. Furthermore, compound 1 shows blue photoluminescent property at room temperature.

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 and Crystal Structure of a New Three-dimensional Heterometallic Coordination Polymer

A new 3d-4fheterometallic polymer {[Sm2Cu（PDC）2（SO4）2（H20）6]·2H2O}n 1 has been synthesized by Sm2O3, Cu（SO4）2·5H2O and pyridine-3,5-dicarboxylic acid under hydrothermal conditions. The compound crystallizes in triclinic system, space group Pi, with a = 6.352（7）, b = 10.040（10）, c = 10.315（11） A, α = 94.958（14）, β = 95.556（7）, γ = 99.747（14）°, V = 641.7（12）A3, Z = 1, M, = 1030.63, Dc= 2.651 Mg/m3,μ = 5.615 mm-1, F（000） = 491, the final R = 0.0491 and wR = 0.1345 for 2098 observed reflections with I 〉 2σ（I）. The compound is a three-dimensional network structure in which infinite lanthanide-carboxylate chains are linked by [Cu（$04）2]2- metalloligands to form a mixed-metal coordination network.

Hydrothermal Synthesis,Crystal Structure and Fluorescence Spectrum Studies of a Supramolecular Compound {[2-(2-Pyridyl)benzimidazoleH_2]^(2+)·[SbCl_5]^(2-)}_2

A new supramolecular compound, { [2-（2-pyridyl）benzimidazoleH2]2＋.[SBC15]2-}2, was synthesized by the hydrothermal reaction of o-diaminobenzene, 2-pyridinecarboxylie acid and SbCl3 in 1：1 HC1 solution, and characterized by chemical analysis, elemental analysis, IR spectra, thermogravimetfic analysis and fluorescence spectra. The crystal structure was deter- mined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P211c, with a = 16.0397（13）, b = 14.3189（12）, c = 15.6370（13） A, β = 105.8980（10）°, V = 3454.0（5） A3, Z = 4, C24H22Cl10N6Sb2, Mr = 992.48, Dc = 1.909 g/cm3,/z = 2.366 mm-1, S = 1.010, F（000） = 1920, R = 0.0254 and wR = 0.0555. The coordination anion, [SbCl5]2- which is a distorted tetragonal pyramid, is composed by coordinating action with Sb3＋ ion and five adjacent chloride ions. Every four coordination anions of [SbCl5]2- form a biquaternion ring structure through the secondary bonding of Sb...Cl. Moreover, the compound adopts a three-dimensional network supramolecular structure because of the hydrogen bonds and π-π stacking between the rings and the 2-（2-pyridyl）benzimidazole divalent cations. The title compound also shows good fluorescent behaviors.

Hydrothermal Synthesis and Crystal Structure of a New Nickel(Ⅱ) Complex with 3,4-Pyridinedicarboxylic Acid and 1,4-Bis(imidazol-1-ylmethyl)-benzene Ligands

A metal-organic coordination polymer [Ni（PDB）（bix）（H20）]n （H2PDB = 3,4-pyri- dinedicarboxylic acid, bix = 1,4-bis（imidazol-l-ylmethyl）-benzene） 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. Blue crystals crystallize in the triclinic system, space group PI with a = 9.1849（8）, b = 9.2065（9）, c = 12.9308（12） °, a = 103.3070（10）, β = 104.7160（10）, y = 90.5900（10）°, V = 1026.42（16）/k3, C21H19NsNiOs, Mr = 480.12, Dc = 1.553 g/cm3, F（000） = 496, Z = 2,/l（MoKa） = 0.991 mm-1, the final R = 0.0325 and wR = 0.0799 for 3561 observed reflections （I 〉 2σ（I））. The structure of 1 exhibits a two-dimensional network structure.

Hydrothermal Synthesis and Crystal Structure of a Cobalt(II) Coordination Polymer: [Co(C_2O_4)(bix)]_n (bix = 1,4-Bis(imidazol-1-ylmethyl)-benzene)

A new two-dimensional cobalt coordination polymer has been prepared and fully characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. The compound [Co（C2O4）（bix）]n 1 crystallizes in the monoclinic system, space group C2/c, with a = 11.549（3）, b = 15.700（3）, c = 9.260（2） A, β = 102.984（3）°, V = 1636.0（6） A^3, C16HIaCON4O4, Mr= 383.23, Dc = 1.556 g/cm^3, μ（MoKa） = 1.078 mm^-1, F（000） = 780, Z = 4, the final R = 0.0455 and wR = 0.1286 for 1483 observed reflections （I 〉 2σ（I））. Of the compound, the Co center is octahedrally coordinated with oxalate acting as a tetra-dentate ligand coordinated to the cobalt atom and each bix serving as a bridging ligand by employing two N-donors to coordinate with the Co center. An infinite {Co2（C2O4）2}∞ chain is formed along the α axis. Furthermore, the 1D chains are held together via bix ligands to generate a two-dimensional network structure with 1D coronal-like channels （ca. 5.691A × 15.700A）.

Hydrothermal Synthesis and Crystal Structure of a Novel Isophthalate-bridged Copper(II) Polymer with Two-dimensional Network Structure: [Cu_2(phen)(ipt)_2]_(2n)·nH_2O (ipt = isophthalate, phen = 1,10-phenanthroline)

A novel metal-organic coordination polymer [Cu2（phen）（ipt）2]2n-nH2O 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. The complex crystallizes in monoclinic, space group P21/c with a = 12.338（3）, b = 12.167（3）, c = 18.167（4）A, β= 111.686（14）°, V = 2534.1（10）A^3, C28H18Cu2N2O9, Mr = 653.52, Dc = 1.713 g/cm^3,μ（MoKα） = 1.740 mm^-1, F（000） = 1320, Z = 4, the final R = 0.0443 and wR = 0.0853 for 3543 observed reflections （1 〉 2σ（I））. It exhibits a novel two-dimensional network with tetra-Cu-ipt-as building units.

Hydrothermal Synthesis and Crystal Structure of a Zinc(II) Polymer with a Two-dimensional Layer Structure: [Zn(pzdc)(phen)]_n·nH_2O

A metal-organic coordination compound formulated as [Zn（pzdc）（phen）]n·nH2O 1 （H2pzdc = pyrazine-2,3-dicarboxylic acid, phen = 1,10-phenanthroline） has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, fluorescence spectrum and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/n with a = 11.607（2）, b = 11.719（2）, c = 13.140（3）A^°, β = 110.707（3）°, V= 1671.9（6）A^°3, C18H12ZnN4O5, Mr= 429.69, De = 1.707 g/cm^3,μ（MoKa） = 1.511 mm^-1, F（000） = 872, Z = 4, the final R = 0.0356 and wR = 0.0853 for 2713 observed reflections （I 〉 2σ（I））. It exhibits an interesting two-dimensional layer structure and shows yellow photoluminescent property at room temperature.

Hydrothermal Synthesis and Crystal Structure of a Cadmium(II) Polymer with One-dimensional Chain Structure: [Cd(bpy)(BDC)]_n·nbpy

A metal-organic coordination polymer [Cd（bpy）（BDC）]n·nbpy （bpy = 2,2-bipyri-dine, H2BDC = terephthalic acid） has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, TG and single-crystal X-ray diffraction. The complex crystallizes in monoclinic, space group C2/c with a = 15.723（5）, b = 21.695（5）, c = 7.576（5） A, β = 116.171（7）°, V = 2319.3（18）A^3, C28H20CdN4O4, Mr = 588.88, Dc = 1.686 g/cm^3, μ（MoKα） = 0.987 mm^-1, F（000） = 1184, Z = 4, the final R = 0.0464 and wR = 0.0831 for 1882 observed reflections （Ⅰ〉 2σ（Ⅰ））. It exhibits a three-dimensional network with channels constructed from one-dimensional coordination chains via C–H…O hydrogen bonds and significant aromatic π-π stacking interactions.

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 and Crystal Structure of a Lead(Ⅱ) Polymer with a Two-dimensional Network Structure:[Pb_2(PDB)_2(phen)]_n·nH_2O

A new metal-organic complex [Pb2（PDB）2（phen）]n·nH2O （H2PDB=pyridine-3,4-dicarboxylic acid,phen=1,10-phenanthroline） 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 P1 with a=7.2472（5）,b=10.6966（8）,c=16.2376（12）,α=98.2960（10）,β=91.6430（10）,γ=97.4810（10）o,V=1233.53（16）3,C26H16O9N4Pb2,Mr=942.81,Dc=2.538 g/cm3,μ（MoKα）=13.697 mm-1,F（000）=872,Z=2,the final R=0.0247 and wR=0.0654 for 3886 observed reflections （I 〉 2σ（I））.In the crystal structure,the Pb（1） atom is six-coordinated with four carboxylate oxygen atoms from three different PDB ligands and two nitrogen atoms from phen ligand,showing a distorted octahedral geometry;the Pb（2） atom is four-coordinated with four carboxylate oxygen atoms from four different PDB ligands,showing a distorted tetrahedral geometry.It exhibits a three-dimensional supramolecular network structure formed by hydrogen bonds and π-π interactions.

Hydrothermal Synthesis and Crystal Structure of a Three-dimensional Cadmium(Ⅱ) Complex

A metal-organic coordination polymer [Cd2（PDC）2（bix）（H2O）2]n·nH2O （H2PDC = 2,4-pyridinedicarboxylic acid, bix = 1,4-bis（imidazol-l-ylmethyl）-benzene） 1 has been hydrother- mally synthesized and characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. Brown crystals crystallize in the orthorhombic system, space group P212121 with a = 11.741（3）, b = 14.190（4）, c = 18.963（5） A, V= 3159.4（14） A3, C28H26Cd2N6O11, Mr= 847.35, Dc = 1.781 g/cm3, F（000） = 1680, Z = 4,μ（MoKa） = 1.415 mm-1, the final R = 0.0381 and wR = 0.0882 for 5472 observed reflections （1 〉 2σ（I））. The structure of 1 exhibits a threedimensional network structure.

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

A novel manganese（Ⅱ） coordination polymer [Mn（L^1）2（H2O）]·2H2O （HL^1 = 2,6- dichlorobenzoic acid） 1 has been synthesized and structurally characterized. X-ray diffraction analyses reveal that 1 is a one-dimensional chain structure bridged by water molecules and 2,6- dichlorobenzoic acid. The crystal is of monoclinic, space group P21/c with α = 12.9701（19）, b = 20.592（3）, c = 7.3759（10） A, β = 102.660（2）°, V = 1.9221（5）. nm^3, Z = 4, C14H12Cl4MnO7, Mr= 488.98, Dc= 1.690 g/cm^3, p = 1.275 mm^-1, F（000） = 980, Rint = 0.0348, R = 0.0350, and wR = 0.0755. In the crystal the manganese atom is six-coordinated by two oxygen atoms from water and four oxygen atoms from four 2,6-dichlorobenzolate molecules, completing an octahedral geometry.