Hydrothermal Synthesis,Crystal Structure and Properties of a Novel Polyoxometalate {[Cu~Ⅱ(1,10-phen)]_2[PMo~Ⅵ_(11)Mo~ⅤO_(40)]} [Cu~Ⅰ(C_8N_4H_6)(C_9H_6NO)(H_2O)]

A new pseudo three-dimensional framework structure of the title compound {[CuⅡ(1,10-phen)]2[PMoⅥ11MoⅤO40]}[CuⅠ(C8N4H6)(C9H6NO)(H2O)](1) has been prepared by the hydrothermal method for the first time and characterized by elemental analyses,X-ray single-crystal diffraction and IR spectra.1 consists of two building blocks,one {[CuⅡ(1,10-phen)]2[PMoⅥ11MoⅤO40]} and one [CuⅠ(C8N4H6)(C9H6NO)(H2O)] coordinated group.Singlecrystal X-ray diffraction revealed that 1 crystallizes in the monoclinic system,space group P2/c with a=13.498(4),b=12.890(3),c=21.465(8),β=97.314o,V=3704(2)3,Mr=2693.61,Z=2,Dc=2.415 Mg/m3,μ=2.915 mm-1,F(000)=2562,S=1.009,the final R=0.0583 and wR=0.1406 for 5129 observed reflections with I2σ(I).Furthermore,compound 1 shows strong fluorescent properties in the solid state at room temperature.The electrochemical behavior of 1 has also been studied by cyclic voltammograms.     

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·nH_2O 1 (H_2pzdc=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 P2_(1/n) with α=11.607(2),b=11.719(2),c=13.140(3)(A),β=110.707(3)°,V=1671.9(6)(A)~3,C_(18)H_(12)ZnN_4O_5,Mr=429.69,D_c=1.707 g/cm~3,μ(MoKα)=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.     

Synthesis and Structure of a Hydrogen-bonding Assembled Three-dimensional Supramolecular Indium（Ⅲ） Compound Involving One-dimensional Helices

The title compound [In（H2ip）（pdc）（H2O）] （H3ip = 5-hydroxyisophthalic acid, H2Pdc = pyridine-2,6-dicarboxylic acid） has been synthesized and characterized by single-crystal X-ray diffraction analysis. It crystallizes in monoclinic, space group P21/c with a = 13.830（8）, b = 6.488（4）, c = 17.632（10）A^°, β = 92.510（10）°, C15H10InNO10, Mr= 479.06, V = 1580.6（15）A^°3, Z = 4, De= 2.013 g/cm^3, F（000） = 944,μ = 1.557 mm^-1, the final R = 0.0413 and wR = 0.0793 for 2950 observed reflections with I 〉 2σ（I）. The In（Ⅲ） ion is seven-coordinated in a slightly distorted penta-bipyramidal geometry. The mixed ligands connect the In（Ⅲ） ions into 21 helical chains along the [010] direction, and the hydrogen bonds assemble the chains into a three-dimensional supramolecular network.     

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 [Mn_2(PDC)_2(bipy)_2(H_2O)_2] (H_2PDC=2,4-pyridinedicarboxylic 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 α=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,C_(34)H_(26)Mn_2N_(6O)O_(10),M_r=788.49,D_c= 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.     

Fe3(CO)8(C6H5NC)(μ3-S)2的合成和晶体结构

The title compound Fe_3(CO)_8(C_6H_5NC)(μ_3-S)_2 (Ⅰ) was synthesized by the reaction of C_6H_5NCS with Fe_3(CO)_12 at room temperature. The crystal and molecular structure of the title compound were determined by single ctystal diffraction method. Crystal data: monoclinic, space group P2_1/C, a=12.718(4)Å, b=26.164(10) Å, c=l3.741(7) Å, β=117.18(2) °, V=4067(2) Å3, Z=8, Dc=1.825 g/cm3. The structure was solved by direct method and difference Fourier synthesis, and refined by full-matrix Least-squares with anisotropic thermal paramaters, using 1990 observed reflections [Ⅰ＞3σ(Ⅰ)].The final residual factor was R＝0.076, Rw＝0.082. The substituted ligand (C_6H_5NC)in Fe_3(CO)_8(C_6H_5NC)(μ_3-S)_2 is connected to the Fe(3) atom of the distorted tetragonal pyramid Fe_3S_2 framework.     

Synthesis and Single-crystal Structure of a Silver(Ⅰ) Carboxyarylphosphonate: [Ag(H_2BCP)(4,4'-bipy)]·2H_2O

The title compound, a novel Ag(Ⅰ) carboxyarylphosphonate [Ag(H2BCP)(4,4'- bipy)]·2H2O (H3BCP = p-H2O3PCH2C6H4COOH, 4,4'-bipy = 4,4'-bipyridine), was synthesized by a hydrothermal reaction and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. It belongs to monoclinic system, space group P21/c with a = 5.7038(11), b = 22.397(4), c = 5.602(4) ?, β = 106.26(3)°, V = 1913.4(7) 3, Z = 4, C18H20N2O7PAg, Mr = 515.20, Dc = 1.788 g/cm3, μ = 1.182 mm-1, F(000) = 1040, the final R = 0.0404 and wR = 0.1216 for 4178 observed reflections with I 2σ(Ⅰ). In the structure, the Ag(Ⅰ) cations are bridged by 4,4'-bipy to give rise to 1D chains running along the b axis. These chains are linked further by the interactions of O (from BCP ligands) and Ag atoms to yield 2D layers. Hydrogen bonding interactions and weak π-π stacking interactions between 4,4'-bipy rings assemble such adjacent layers to generate a 3D supramolecular architecture.     

A Layered Vanadium Oxide with Cobalt（Ⅱ） Coordination Complex： Hydrothermal Synthesis and Crystal Structure of （py）5Co2（H2O）3[V4O12]

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）.     

Synthesis and Crystal Structure of 3-{[（1E） 1-（2- Hydroxyphenyl） methylidene]amino}-4-cyanopyrazole

The title Schiff base compound （C11H8N4O）, a derivative of pyrazole, has been synthesized by the reaction of salicylaldehyde and 3-amino-4-cyanopyrazole in absolute ethanol and characterized by elemental analyses, IR, ^1H NMR and X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P21/n, with a = 7.5594（7）, b = 18.3342（19）, c = 22.461（2） A^°, β = 98.419（2）°, V = 3079.5（5） A^°3, Mr = 212.21, Z = 12, F（000） = 1320, Dc = 1.373 g/cm^3, T = 298（2） K, 2 = 0.71073 A^°, the final R = 0.0571 and wR = 0.0493. A total of 5412 unique reflections were collected, of which 1612 with I 〉 2σ（I） were observed. The molecular structure adopts a trans configuration about the C=N double bond. The preliminary biological tests show that the compound has high antibacterial activities.     

Synthesis and Crystal Structure of [(NH_4)_6][Gd_2Mo_(36)O_(112)(H_2O)_(20)]·52H_2O

1 INTRODUCTION There is considerable interest in the heteropolymetalates in view of their potential applications in many fields, such as, catalysis, biology, medicine, magnetochemistry, and materials science[1～5]. It has been well- known that the rare earth elements are highly oxophilic and the anion of polyoxomolybdates have oxygen-rich composition, which can be used as synthons for the construction of novel heteropolymetalates. Since the structure of polyoxoanion 36-molybdate Mo36O1128…     

[Co(Phen)2(H2O)2](HL)NO3·3H2O的合成及晶体结构

在水溶液中,以邻菲咯啉、丁二酸与硝酸钴为原料合成了一个新的超分子化合物[Co(Phen)2(H2O)2].(HL).(NO3).3H2O,并经元素分析、IR、X射线单晶衍射分析进行了结构表征.结构分析表明,晶体属三斜晶系,P1-空间群,a=0.968 0(2)nm,b=1.370(3)nm,c=1.394 9(3)nm,α=61.714(3)°,β=71.495(4)°,γ=79.575(4)°,V=1.543 7 nm3,Z=2,ρ=1.481 g/cm3,C28H31CoN5O12,Mr=688.51,F(000)=714 andμ=0.627 mm-1,7 754个独立衍射点中,5 428个可观察点满足I≥2σ(I),R1=0.074 5,wR2=0.210 7.晶体中[Co(Phen)2(H2O)2]2+通过π-π相互作用堆积成二维层状结构,层间通过氢键作用构成三维超分子.     

[(C_6H_5NO_2)Pr(H_2O)_4](CrMo_6O_(24)H_6)·(C_6H_5NO_2)·2.5H_2O的合成与晶体结构

用常规合成方法制备了基于Anderson结构阴离子的二维层状化合物[(C6H5NO2)2Pr(H2O)4](CrMo6O24H6)·2.5H2O,通过红外光谱和X射线单晶衍射对其进行了表征.结果表明,该化合物属于单斜晶系,C2/c空间群.a=2.3442(9)nm,b=1.3291(5)nm,c=2.458(1)nm,β=103.08(1)°,V=7.460(5)nm3,R1=0.0727,wR2=0.1903.结构分析表明,[CrMo6O24H6]3-阴离子通过端氧担载一个配位的Pr3+离子形成中性的(C6H5NO2)Pr(H2O)4(CrMo6O24H6)基团,相邻的中性基团在Ot—Pr—Ot桥联下形成一维链,链与链又通过异烟酸的桥联形成二维层状结构.     

Synthesis,Crystal Structure and Theoretical Calculation of [2-（2,6-Dioxacyclohexyl）-5-methoxylphenols]2

The title compound [2-（2,6-dioxacyclohexyl）-5-methoxylphenols]2 was synthesized by the reaction of 2-hydroxyl-3-methoxylbenzaldehyde and 1,3-propanediol in the presence of DMF-DMS adduct and characterized by IR spectrum, UV-Vis spectrum and X-ray crystallography. The title compound belongs to monoclinic, space group P21 with a = 9.8967（10）, b = 8.2240（9）, c = 13.3654（14） A^°, β= 90.016（2）°, C11H14O4, Mr = 210.22, V = 1087.8（2）A^°3, Z = 4, Dc = 1.284 Mg/m^3, F（000） = 448,μ = 0.098 mm^-1, the final R = 0.0300 and wR = 0.0761 for 2070 observed reflections with I 〉 2σ（I）. The molecules are connected via intermolecular O-H…O hydrogen bonds into a 2D network structure. Moreover, theoretical investigations of the title compound with HF/6-31G（d） method were performed, and its stability, frontier molecular orbital composition and Mulliken charge distribution were also discussed. The compound is a bis-molecule. The two molecules stay together and could not be separated. Two crystallographically independent molecules exist in an asymmetric unit. The bond lengths and bond angles of the two molecules are slightly different with each other.     

Synthesis and Crystal Structure of Bi（Hsal）3（1,10- phenanthroline） （Hsal = O2CC6H4-2-OH）

A new bismuth compound Bi（Hsal）3（1,10-phenanthroline） （Hsal = O2CC6H4-2-OH） has been synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in the triclinic system, space group P1, with a = 10.243（2）, b = 11.905（3）, c = 12.934（3） A, α= 76.780（6）, β= 68.683（6）,γ= 80.930（7）°, V = 1425.6（5） A^3, Dc = 1.865 g/cm^3, Mr = 800.51, F（000） = 780, μ= 6.247 mm^-1, Z = 2, R = 0.0456 and wR = 0.1131 for 5612 observed reflections （I 〉 2σ（I））. In this compound, three salicylate ligands coordinate to the Bi atom through the carboxylate groups to form a four-membered chelate ring, and phenanthroline ligand chelates the metal through two N atoms. The structure of the title compound manifests a possible coordination mode between bismuth subsalicylate and N atom containing amino acid in the biological system.     

Synthesis,Structure and Electrochemical Property of a Supramolecular Compound（H2en）2[Cu（en）2（H3O）2][Mo8O28]

A supramolecular compound(H2en)2[Cu(en)2(H3O)2][Mo8O28](en=ethylenediamine) was hydrothermally prepared and confirmed by elemental analysis and TG analysis.Single-crystal X-ray analysis reveals that the crystal crystallizes in the triclinic system,space group P1 with a=9.4635(4),b=9.8645(5),c=10.9794(5),α=69.2050(10),β=72.3730(10),γ=78.4510(10)o,Mr=1559.55,V=908.24(7)3,Z=1,Dc=2.851 g/m3,F(000)=749,μ=3.350 mm-1,S=1.000,the final R=0.0217 and wR=0.0567.The compound consists of(H2en)2+,[Mo8O28]8-anion and [Cu(en)2(H3O)2]2+ cations and constructs a 3D supramolecular structure through hydrogen bonds between the nitrogen atoms from en of [Cu(en)2(H3O)2]4+ fragments and the terminal oxygen atoms from the [Mo8O28]8-polyoxoanions.The electrochemical behavior of this compound has been studied in detail based on a solid bulk modified carbon paste electrode of compound(CPE).     

Synthesis and Crystal Structure of 7-Amino-2,3,4,5-tetrahydro- 1,3-dimethyl- 5-（2-nitrophenyl）-2,4-dioxo-lH-pyrano[2,3- d]pyrimidine-6-carbonitrile DMF Solvate

The title compound 7-amino-2,3,4,5-tetrahydro-1,3-dimethyl-5-（2-nitrophenyl）- 2,4- dioxo-1H-pyrano[2,3-d] pyrirnidine-6-carbonitrile DMF solvate 1 （C19H20N6O6, Mr = 428.41） was synthesized and crystallized. The crystal belongs to the monoclinic system, space group P2 1/c with a = 11.383（2）, b = 13.372（2）, c = 13.673（2）A, β = 97.380（4）°, Z = 4, V = 2063.8（6）A^3, Dc = 1.379 g/cm^3,μ（MoKα） = 0.105 mm^-1, F（000） = 896, the final R = 0.0738 and wR = 0.1647 for 2964 observed reflections （I〉 2σ（I））. X-ray analysis reveals that the new pyran ring is coplanar, which is obviously different from those of other similar compounds. In addition, the unclassical hydrogen bonds of C-H…O and C-H…N are presented in the crystals except for the normal hydrogen bonds of N-H…O.     

Syntheses and Structures of Two Cadmium Complexes with Isophthaloylbisglycine Acid and 4,4'-Bipyridine

The two title complexes [{Cd（IBG-CH3）（4,4＇-bipy）（H2O）2}·NO3]n 1 and [{Cd（IBG）- （4,4＇-bipy）（H2O）2}·2H2O]n 2 （H2IBG = isophthaloylbisglycine and 4,4＇-bipy = 4,4＇-bipyridine） have been synthesized and characterized by single-crystal structure determination,IR and TG analyses. Complex 1 crystallizes in monoclinic,space group C2/c with a = 27.221（2）,b = 11.6093（7）,c = 16.3571（9）A,V = 5149.2（6） A^3,Z = 8,C23H23N5O11Cd,Mr = 657.86,Dc = 1.697 g/cm^3,F（000） = 2656.00,μ（MoKα） = 0.919 mm^-1,the final R = 0.0478 and wR = 0.0882 for 3728 observed reflections with I 〉 2σ（I）. Complex 2 crystallizes in triclinic,space group Pī with a = 9.0940（4）,b = 11.6852（5）,c = 13.1119（6）A,V = 1230.26 A^3,Z = 2,C22H26N4O10Cd,Mr = 618.87,Dc = 1.671 g/cm^3,F（000） = 628.0,μ（MoKα） = 0.951 mm^-1,the final R = 0.0567 and wR = 0.1124 for 3713 observed reflections with I 〉 2σ（I）. In both structures,the CdII metal centers are coordinated by seven atoms to form a distorted pentagonal bipyramidal geometry.     

A Novel 2D Architecture from Bismuth and Flexible Ligand N,N'-Diacetic Acid Imidazolium Chloride

A new compound {[Bi（trans-DAM）（cis-DAM）（H2O）]NO3·H2O}n 1 derived from bismuth and the flexible ligand N,N＇-diacetic acid imidazolium chloride （H2DAMCl） was obtained by hydrothermal synthesis and characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic P21/c space group with a = 9.2298（18）, b = 13.339（3）, c = 17.090（3） , β = 105.38（2）°, V = 2028.7（7）A^3, Z = 4, C14H18N5O13Bi, Mr = 673.31, Dc = 2.204 g/cm^3, F（000） = 1296, μ = 8.772 mm-1, the final R = 0.0472 and wR = 0.1441 for 4129 observed reflections （I 〉 2σ（I））. In 1, the carboxylic groups from DAM- ligands adopt a cheating mode to link bismuth ions to form a 2D sheet network. These sheets are further connected by hydrogen bonding interactions to give an interesting 3D supramolecular framework. 2D correlation analysis of IR of 1 with thermal and magnetic perturbation was introduced to ascertain the characteristic adsorption of the groups overlapped in the 1D IR spectrum. Additionally, compound 1 exhibits fluorescent emission at room temperature.     

Structural,Photoluminescent and Theoretical Evidence for Ligand-unsupported Argentophilic Interactions in a Supramolecular Aggregate of [Ag2（Hida）（NH3）2]

A new neutral [Ag2（Hida）（NH3）2] molecule （1, H3ida = 1H-imidazole-4,5-dicarboxylic acid） has been synthesized and structurally characterized by single-crystal diffraction. Compound 1 crystallizes in monoclinic, space group C2/c with a = 18.3928（8）, b = 8.3299（5）, c = 13.682（7） A, β = 113.179（2）°, V = 1926.9（10）A^3, Z = 8 and Dc = 2.784 g·cm^-3. In the solid state, this disilver（I） compound can aggregate to furnish the energetically stable ligand-unsupported Ag^I-Ag^I interaction concomitant with significant photoluminescence changes in different aggregate states, and such argentophilicity interaction is also supported by molecular orbital calculations.     

Locking the Absolute Configuration of Achiral Amine Ligand: A Strategy for Helicity Introduction in Coordination Polymers

A novel coordination polymer {[Mn（m-cpdba）（H2O）4]·H2O}n 1 has been synthesized and characterized. Single-crystal X-ray diffraction analysis reveals that compound 1 contains one-dimensional single-stranded helical chains, in which the chirality of a stereochemically labile amine of the ligands can be locked by the Mn（II） ion via coordination bonds and transferred to the whole coordination polymeric chain, exhibiting an identical absolute configuration. Crystal data for 1： C14H17Mn1N3O13, Mr = 490.25, space group C2/c, a = 18.5177（18）, b = 6.6194（5）, c = 31.563（4）A, β = 105.046（5）°, Z = 8, V = 3736.2（7）A^3, Dc = 1.743 g/cm^3, F（000） = 2008 and μ = 0.786 mm^-1.     

A Chiral Helical Compound Based on Achiral Components

The title compound, [Cu(dpa)(2,2'-bipy)(H2O)2]n 1 (H2dpa = diphenic acid and 2,2'- bipy = 2,2'-bipyridine), has been synthesized and its structure was determined by single-crystal X-ray diffraction. The crystal is of orthorhombic, space group P212121 with a = 10.597(4), b = 11.317(4), c = 17.630(7) , V = 2114.3(14) 3, C24H20CuN2O6, Mr = 495.97, Z = 4, Dc = 1.558 g/cm3, μ = 1.079 mm-1, F(000) = 1020, Flack value = 0.052(18), R = 0.0430 and wR = 0.1016 for 3381 observed reflections (I > 2σ(I)). In compound 1, the dpa ligands link metal ions into helical structures in the same direction.