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）.

Hydrothermal Synthesis, Crystal Structure and Thermal Analyses of Pyrazine-2,3-dicarboxylic Acid Bridged Co(II) Coordination Polymer of _∞~2[Co(phen)(μ-L)_(3/3)]·H_2O (H_2L = Pyrazine-2,3-dicarboxylic Acid)

A novel pyrazine-2,3-dicarboxylic acid bridged Co(II) phen complex 2 ∞ [Co- (phen)(μ-L)3/3]?H2O (H2L = pyrazine-2,3-dicarboxylic acid) has been hydrothermally synthesized, and X-ray single-crystal diffraction analysis shows that it crystallizes in the monoclinic system, space group P21/n with a = 11.480(2), b = 11.885(2), c = 12.939(3) ?, β = 110.55(3)°, V = 1653.1(6) ?3, Mr = 423.25, Dc = 0.425 g/cm3, Z = 4, R = 0.0361 and wR = 0.1011. The title complex consists of 2D 2 ∞ [Co(phen)(μ-L)3/3] layers and crystal water molecules. Each Co atom is octahedrally coordinated by three N atoms and three O atoms to form 2D 2 ∞ [Co(phen)(μ-L)3/3] polymeric layers. Furthermore, such 2D layers are stacked into 3D supramolecular frameworks via Van der Waals’ intermolecular forces, strong and weak hydrogen-bond interactions. The coordination phen and crystal water molecules are resided into cavities of the frameworks.

Hydrothermal Synthesis and Structure of [CH3NH3]2[(VⅣO)2(VⅤO4)2]:A New Layered Mixed-valence Vanadium Oxide Incorporated with Organic Cations

A new layered mixed valence vanadium oxide, [CH 3NH 3] 2[(V ⅣO) 2(V ⅤO 4) 2], which contains interlamellar organic cations was prepared under hydrothermal conditions and its single crystal structure was determined. It crystallizes in a triclinic system with space group P 1, a =0 625 59(8) nm, b =0 639 84(9) nm, c =0 747 19(10) nm, α =78 718(2)°, β =80 099(2)°, γ =77 100(2). The compound contains mixed valence V 4+ /V 5+ vanadium oxide layers constructed from VO 4 tetrahedra, pairs of edge sharing VO 5 square pyramid and methylamine with protonated organic amines occupying the interlayer space.

Hydrothermal Synthesis and Crystal Structure of Inorganic-organic Hybrid Compound [H_3NC_2H_4NH_2]VOPO_4

An inorganic-organic hybrid compound, [H_3NC_2H_4NH_2]VOPO_4 was synthesized by means of the hydrothermal method. It was crystallized in a monoclinic system, a space group P2_1/c, with the crystal cell parameters: a=0.92285(11) nm, b=0.72994(9) nm, c=0.98495(11) nm, β=101.280(3)°, V=0.65067(13) nm^3, M_r=223.02 g/mol, D_c=2.277 g/cm^3, Z=4, R=0.0315, ωR=0.0865, GOF=1.085. The VO_5N octahedra chains are corner-linked by PO_4 tetrahedra; the VO_5N octahedra are all trans-linked with V—O bonds being alternately short and long. The monoprotonated ethylenediamine was intercalated between the layers with one end coordinating to V and the other end as an H-bond donor interacting with a terminal O atom of PO_4 from a neighboring sheet. The elementary analysis, infrared spectrum characters and thermal stability were also given.

Mild Hydrothermal Synthesis,Crystal Structure and Magnetic Behavior of AgCu(IO_3)_3:a Quasi-one-dimensional S=1/2 Chain Compound

A new complex AgCu（IO3）3 is synthesized by mild hydrothermal method and characterized by single-crystal X-ray diffraction and magnetization measurement.AgCu（IO3）3 is triclinic,space group P1,with a = 7.3081（1）,b = 7.8089（1）,c = 8.2447（1）A,α = 67.159（1）,β = 74.982（1）,γ = 80.982（1）°,and Z = 2.AgCu（IO3）3 is isostructral with Ag Pb（IO3）3.The structure of Ag Cu（IO3）3 consists of CuO6 chain columns parallel to the c axis,formed by corner-sharing Cu（1） and Cu（2） octahedra and flanked by corner-sharing IO3 groups; these CuO6 columns are cross-linked into a three-dimensional framework through I–O and Ag–O bonds.I（1）,I（2） and I（3） are coordinated respectively with 3 oxygens on the same side to form trigonal pyramids confirming the presence of a stereochemically active lone pair of each I^5＋ cation.In the CuO6 chain columns,Cu（1）O6 and Cu（2）O6 octahedra are tetragonally distorted with four shorter bonds in the square planes and two longer apical bonds.Cu（1）O6 octahedra were corner sharing with Cu（2）O6 octahedra with a shorter Cu（1）–O（1） bond in the square planes and a longer apical Cu（2）–O（1） bond,which forms a Cu（1）–Cu（2） magnetic chain along the c direaction.Magnetization measurement shows weak antiferromagnetic property in low temperature range.Ag Cu（IO3）3 provides a new example of a quasi-one-dimensional magnetic system.

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 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 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 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.