Synthesis and Crystal Structure of an Interpentateing 3-D Framework Constructed from Mixed Ligands

A novel organic-inorganic hybrid compound constructed from mixed ligands, Co3（SIP）2（bipy）4（H2O）6·6.5H2O （H3SIP = 5-sulfoisophthalic acid, bipy = 4,4′-bipyridyl）, has been hydrothermally synthesized and characterized by IR, TGA and single-crystal X-ray diffraction. The crystal belongs to orthorhombic, space group P212121 with a = 11.395（2）, b = 19.395（4）, c = 30.675（6） A^°, Mr = 1513.05, V= 6779（2） A^°^3, Dc= 1.482 g/cm^3, F（000） = 3120, μ = 0.873 mm^-1, Z= 4, the final R = 0.0439 and wR = 0.119 for 13421 observed reflections with I〉 2σ（I）. The structure of the compound presents a 3-D framework containing Co-bipy 1-D chain and 2-D bilayer motifs and carboxylate spacers, and the connection of 1-D chain and 2-D bilayer motifs by carboxylate ligand results in the final open framework with twofold interpenetration net. A probe reaction of the oxidation of benzaldehyde with H2O2 using the title compound as catalyst was carded out in a liquid-solid system, showing that the compound has high oxidative catalytic activity to the reaction.     

A 3-D Supramolecular Network with 1-D Cation Metal.organic Coordination Polymers and Diverse Motifs from Hydrogenbonded [M（H2O）4]-Carboxylates

One-pot solvothermal reaction of Iransition metal Znn salt with 4,4-bipyddyl （bpy） and 1,4-benzenediacrylic add （H2L） in the presence of Et3N generates a three-dimensional （3-D） supramolecular network with 1-D cation metal-organic coordination polymer, [Zn（H20）a（bpy）]-L 1, and structurally characterized by single-crystal X-ray diffraction, elemental analyses, IR spectroscopy, and photoluminescent property. The complex crystallizes in triclinic, space group P1 with a = 7.1291（2）, b = 7.3784（3）, c = 10.5042（3）A, α = 95.049（2）, β = 102.162（2）, 7 = 97.027（3）0, V= 532.38（3）A3, C22H24N2O8Zn, Mr = 509.82, De= 1.590 g/cm3, p（MoKa）= 1.207 ram-l, F（000） = 264, Z = 1,the finalR=O.0438and wR=O.lOll for 1589 observed reflections （I 〉 2σ（I））. In the crystal structure, the second building unit composed of [Zn（H2O）4].L constructs two distinct 2-D supramolecular sheets and a neutral 3-D architecture. The title compound 1 shows strong photoluminescence with emission maximum at 2 = 455 nm upon λex.max = 355 nm.     

Crystal Structure and Biological Activities of N-（5-（4-Chloro-2-（trifluoromethyl）phenyl）furan-2-carbonyl）-N＇-（4,6,dimethylpyrimidin-2-yl）thiourea

The new title compound N-（5-（4-chloro-2-（trifluoromethyl）phenyl）furan-2-carbon-yl）- N＇-（4,6-dimethylpyrimidin-2-yl）thiourea （C19H14C1F3N4O2S） has been synthesized, and its crystal structure and biological behaviors were studied. The title compound crystallizes in the monoclinic system, space group P21/c with a = 7.932（5）, b = 33.46（2）, c = 7.556（5） A, β = 98.058（9）°, V = 1986（2） A^3 Mr = 454.85, Z = 4, Dc = 1.521 g/cm^3, μ = 0.349 mm^-1 and F（000） = 928. The structure was solved by direct methods and refined to R = 0.0724 and wR= 0.1429 for 3494 observed reflections （I 〉 2σ（I））. Intermolecular hydrogen bonds along the b axis together with the continuous π-π interactions construct the three-dimensional architecture of the title compound. The preliminary biological tests show definite herbicidalactivity for the title compound.     

Synthesis,Crystal structure and Luminescent Property of a New 3D Supramolecular Compound （C6H6NO2）3（C6H5NO2）（PW12O40）·2H2O

A supramolecular compound （C6H6NO2）3（C6H5NO2）（PW12O40）·2H2O including the Keggin-type [PW1O40]3- polyanion, [HC6H5NO2]＋ （protonated pyridine-4-carboxylic acid molecule）, C6H5NO2 （pyridine-4-carboxylic acid molecule） and two free H20 molecules has been synthesized by the hydrothermal method and characterized by elemental analysis, IR spectra, single-crystal X-ray diffraction and powder X-ray diffraction. The crystal belongs to orthorhombic, space group Pnnm with a = 1.0483（3）, b = 1.4368（6）, c = 2.0526（7） nm, V= 3.0918（18） nm3,Z = 2, F（000） = 3004, Mr= 3406.07, Dc= 1.757 g.m-3,μ = 41.241 mm-1, the final R = 0.0387 and wR = 0.1089 for 2091 observed reflections withI〉 2σ（I）. A total of 30431 reflections were collected, of which 3083 were independent （Rint = 0.0605）. S is 1.182. The title compound presents a 3-D structure via intermolecular hydrogen bonds among [PW12O40]3- polyanions and pyridine-4-carboxylic acid ligands. The ultraviolet and luminescence spectra have been studied at room temperature, of which the purple fluorescent emission is located at 363 nm when excited at 264 nm. Fluorescent emission of the compound derives from the π-π＊ transitions in the pyridine-4-carboxylic acid ligands.     

Synthesis,Crystal Structure and Biological Activity of 1-（β-D-Glucopyranosyl）-3- amino-5-methyl-1H-1,2,4-triazole

The title compound 1-（β-D-glucopyranosyl）-3-amino-5-methyl- 1H- 1,2,4-triazole was synthesized and characterized by IR, 1H-NMR and elemental analysis. Its single crystals of 2H2O adduct suitable for X-ray analysis were obtained by the slow evaporation of a H2O solution and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to orthorhombic, space group P212121 with a = 7.7490（15）, b = 10.424（2）, c = 17.447（4） A^°, V = 1409.3（5） A^°^3, Z= 4, C9H20N4O7, Mr = 296.29, Dc = 1.396 g/cm^3,μ = 0.120 mm^-1, S = 1.007, F（000） = 632, R = 0.0686 and wR = 0.1560 for 1217 observed reflections with I 〉 20（I）. The title molecules are linked through intermolecular hydrogen bonds to form two 1-D chain structures, and such adjacent chains are further linked by intermolecular hydrogen bonds and H2O bridges to form a 3-D supramolecular network structure. The preliminary bioassay results showed that the title compound exhibits fungicidal activities against Gibberella zeae and Colletotrichum orbiculare.     

Hydrothermal Synthesis, Crystal Structure and Fluorescent Property of a Novel Polyoxometalate [H6MoVI8O27]·3C4N2H10

A new infinite three-dimensional framework structure of the title compound [H6Mo^VI8O27]·3C4N2H10 has been synthesized under mild hydrothermal conditions and characterized by elemental analyses, IR, fluorescent spectra and single-crystal X-ray diffraction. C12H36Mo8N6O27 crystallizes in the triclinic system, space group P1^- with a = 8.820（3）, b = 9.534（3）, c = 10.993（4）A, α= 99.985（17）, β = 106.65（2）, γ= 101.650（14）°,V = 840.6（5）A^3, Mr = 1463.99, Z = 1, Dc = 2.892 g/cm^3,μ = 2.993 mm^-1, F（000） = 702, the final R = 0.0676, wR = 0.1920 and S = 1.074 for 2196 observed reflections with I 〉 2σ（I）. The title compound exhibits a novel infinite three-dimensional （3D） framework composed of a [H6Mo^VI8O27] subunit and three dissociated piperazine fragments. The complex exhibits two strong fluorescent emission bands at ca. 417 and 440 nm （λex = 378nm） in the solid state at room temperature.     

Synthesis,Crystal Structure and Biological Activities of N-（4-Cyanopyrazole-3-yl）- α-（3,5-difluorophenyl）- O,O-diisopropyl- α-aminophosphonate

The title compound has been synthesized by the addition reaction of N-（4-cyanopyrazole-3-yl）-3,5-difluorophenyl-imine and diisopropyl phosphate. Its structure was confirmed by means of IR, ^1H NMR and elemental analysis. The single-crystal structure of the title compound was determined by X-ray crystallography. The compound crystallizes in monoclinic, space group C2/c with a = 18.9959（14）, b = 9.2212（7）, c = 22.1108（16）A^°, β= 90.1540（10）°, V = 3873.0（5） A^°^3, Dc = 1.366 g/cm^3, Z = 8, μ = 0.185, F（000） = 1664, and the final R = 0.0503 and wR = 0.1539 for 2996 observed reflections （I 〉 2σ（I））. The results demonstrate that the dihedral angle between the pyrazole and benzene rings is 105.5°, and there is a full delocalized pyrazole system with sp^2 hydridization of N（3）. The crystal structure is stabilized by two intermolecular hydrogen bonds of N（1）-H（1）…O（3） and N（3）-H（3A）…N（4）. The preliminary biological test shows that the title compound has a moderate antifungal activity.     

Synthesis,Crystal Structure and Antitumor Activities of Ethyl 5-methyl-4-morpholino- 2-（3-Methyl-phenylamino）-furo [2,3-d] pyrimidine-6-carboxylate

The title compound （C21H24N4O4, Mr = 396.44） has been synthesized by the func- tionalized ethyl 4-chloro-6-methyl-2-arylamino-furo[2,3-d]pyrimidine-5-carboxylates and mor- pholine. Its structure was confirmed by means of 1H NMR IR, MS and elemental analysis. The crystal structure of the title compound was determined by X-ray single-crystal diffraction. The compound crystallizes in triclinic system, space group P1, a = 7.9919（8）, b = 9.9312（1）, c = 12.9380（13） A, aα = 86.987（2）, β = 83.604（2）, γ = 89.641（2）°, V = 1019.08（18） A3, Z = 2, F（000） = 420, Dc = 1.292 g/cm3,μ = 0.091 mm-1, R = 0.0602 and wR = 0.1548 for 3943 independent （Rint = 0.0639） and 3414 observed （I 〉 2σ（I）） reflections, lntermolecular N-H…O and π-π stacking interactions contributed to the stability of the structure. The preliminary biological test indicated the title compound exhibited cytotoxicity against human lung cancer cell lines.     

Synthesis,Crystal Structure andDNA Binding Studies of α,α′-Bis（3,5-bismethyl-1-pyrozolyl）-carbene-acetyl-isopropenyl Hydrazine

The title compound α,α′-bis（3,5-bismethyl-pyrozole-N-yl）-carbene-acetyl-isopropenyl hydrazine （C16H22N6O, Mr = 314.40） has been prepared. It was characterized by elemental analysis as well as IR, MS, ^1H-NMR and ^13C-NMR spectra. Its crystal structure was determined by single-crystal X-ray diffraction, getting the following data： triclinic, space group P1^- with a = 6.9734（16）, b = 10.773（3）, c = 12.001（3）A, α = 75.311（4）, β = 82.695（4）, ）,γ = 77.143（4）°, Z = 2, V = 847.9（3）A^3, Dc = 1.231 g/cm^3, F（000） = 336 and/μ（MoKα） = 0.082 mm^-1 （λ= 0.71073A）. The results of crystal structure determination show that there exist intermolecular and intramolecular hydrogen bonds, resulting in a two-dimensional supramolecular framework of the title compound. The binding of the title compound to DNA was investigated by absorption, emission, and viscosity measurements. The title compound shows absorption hyperchromicity accompanied by a blue shift at about 254 nm. The binding constant Kb for the title compound has been determined to be 1.89 × 10^4 M^-1 from absorption measurements. The addition of the title compound to DNA pretreated with EB causes appreciable reduction in the emission intensity, indicating that the DNA-bound EB fluorophore is partially replaced by the title compound. The value of K is 3.093 × 10^4 M^-1. The relative viscosity of DNA decreased with the addition of the title compound. Results suggest that the title compound binds to DNA with a non-classical intercalative or groove interaction mode. The observed efficient nuclease activity of the title compound is interesting and may have further influences on the chemistry of DNA minor groove binders.     

Synthesis and Crystal Structure of a New Cadmium（Ⅱ） Supramolecular Network Containing Chelating Imidazole-4-carboxylate Ligand

A new complex, [Cd（Himc）2（H2O）2] 1, obtained from imidazole-4-carboxylatic acid （H2imc） and Cd（ClO4）2·6H2O, has been synthesized. The crystal structure was determined by X-ray diffraction. The title compound crystallizes in the orthorhombic system, space group Pccn, with a = 7.4886（11）, b = 11.9667（18）, c = 13.550（2） A, V= 1214.3（3） A3, Z = 4, Mr= 370.60, Dc = 2.027 mg/m3, F（000） = 728,μ （MoKa） = 1.829 mm^-1, the final R = 0.0243 and wR = 0.0591 for 1150 unique reflections with I 〉 2σ（I）. The cadmium（II） center in the title complex is coordinated with two oxygen and two nitrogen atoms from two bidentate chelated imidazole-4-carboxlate ligands together with two water molecules, giving a distorted octahedral coordination geometry. A one-dimensional hydrogen bonding chain is formed via intermolecular O-H...O hydrogen bonds, and such adjacent chains are further stacked through intermolecular π-π and hydrogen bonding interactions to form a 3D supramolecular framework. Complex 1 exhibits a fluorescent emission band at 290 nm （λex = 236 nm） in the solid state.     

Distinct Hydrogen-bonded MII(H2O)8 Clusters as Second Building Units for 1-D, 2-D and 3-D Supramolecular Architectures (M = Cobalt and Nickel)

Two mononuclear metal-organic complexes, [Co(Hmpdc)2(H2O)4]·4H2O 1 and [Ni(Hfmpdc)2(H2O)4]·6H2O 2, were prepared from 2,6-dimethylpyridine-3,5-dicarboxylic acid (H2mpdc) and 4-furyl-2,6-dimethylpyridine-3,5-dicarboxylic acid (H2fmpdc) with M(NO3)2 salts, respectively, and characterized by single-crystal X-ray diffraction, elemental analyses, IR spectroscopy, and photoluminescent measurement. Complex 1 crystallizes in triclinic, space group P with a = 7.634(5), b = 8.695(5), c = 10.757(6)(A), α = 69.647(7), β = 69.957(8), γ = 83.733(7)°, V = 628.9(7)(A)3, Dc = 1. 561 g/cm3, μ(MoKα) = 0.763 mm-1, F(000) = 309, Z = 1, the final R = 0.0553 and wR = 0.1469 for 1909 observed reflections (I > 2σ(I)). Complex 2 crystallizes in monoclinic, space group P21/n with a = 9.5934(16), b = 12.422(2), c = 14.826(3)(A), β = 105.201(2)°, V = 1705.0(5)(A)3, Dc = 1. 479 g/cm3, μ(MoKα) = 0.655 mm-1, F(000) = 796, Z = 2, the final R = 0.0351 and wR = 0.0889 for 2387 observed reflections (I > 2σ(I)). In the crystal structures of 1 and 2, diverse supramolecular motifs from 1-D chains/ladders to 3-D networks are constructed from corresponding distinct [MⅡ(H2O)8] ion clusters as the second building units, respectively. The solid state compounds of 1 and 2 show similar photoluminescent spectra with emission maximum at ca. 466 nm at room temperature.     

Synthesis and Crystal Structure of [La（BTC）（H2O）6]n

1 INTRODUCTION desired topologies owing to their rich coordination modes[8~12] and we have been exploring the chemi- The assembly of metal-organic infinite frame- stry of coordination polymers constructed by tran- works via coordination of metal ions with multifunc- sition metals and benzoic multicarboxylic acids[13~16]. tional organic ligands is a field of increasing inte- In addition, lanthanide ions have high affinity for rest[1~4]. A rational designed and predictable coor- hard donor a…     

Ni（bpy）（H2O）（V2O6）和[Ni（bpy）2]2（V6O17）的水热合成与晶体结构

用NiCl2·6H2O,2,2＇-联吡啶（bpy）,NH4VO3,WO3在443K下通过水热反应法得到了两种多钒酸镍配合物Ni（bpy）（H2O）（V2O6）（1）和[Ni（bpy）2]2（V6O17）（2）．单晶X射线衍射结果表明化合物（1）属于正交晶系,空间群为Pcα2（1）,晶胞参数为0=0．91704（18）nm,b=1．0519（2）nm,c=1．4336（3）nm,V=1．3830（5）nm^3,Z=4;化合物（2）属于单斜晶系,空间群为P2（1）／c,晶胞参数为α=1．5467（3）nm,b=1．4740（3）nm,c=1．0457（2）nm,β=91．99（3）°,V=2．3826（8）nm^3,Z=4．化合物（1）由2,2’-联吡啶修饰的二维[Ni（V2O6）（H2O）]∞电中性层构成,而化合物（2）则由2,2＇-联吡啶修饰的、呈正弦波浪状的[Ni：（V6O17）]∞二维电中性层构成．     

Synthesis and Crystal Structure of [Cu2（DMF）（H2O）（C7H4NO4）2（C7H3NO4）]2·3.5DMF

A new copper（H） complex [Cu2（DMF）（H2O）（C7H4NO4）2（C7H3NO4）]2-3.5DMF has been synthesized and its structure was determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1^- with a = 10.722（3）, b = 18.170（4）, c = 20.923（7）A,α = 105.297（9）, β = 101.701（10）, γ = 105.74（1）°, V= 3615（1）A^3, Z = 2, C58.50H64.50Cu4N1l.50O3150, Mr = 1686.90, Dc = 1.550 g/cm^3,μ= 1.255 mm^-1, F（000） = 1728.00, T = 150（2） K, the final R = 0.0640 and wR = 0.173 for 11310 observed reflections with I 〉 2σ（I）. In the crystal, each formular unit consists of two dinuclear copper（H） compounds, between which the O-H…O hydrogen bonds exist. Each Cu^Ⅱ cation is six-coordinated in an octahedral geometry. The intermolecular hydrogenbonding interaction leads to a 3-D framework of the title compound.     

Synthesis and Crystal Structure of a Novel Three-dimensional Supramolecular Compound [（AgI3）（4-HBPFA）2（H2O）]

1 INTRODUCTION In recent years, the rational design and synthesisof metal-directed supramolecular frameworks throughintermolecular hydrogen bonds, π-π stacking interac-tion or other weak interactions have received muchattention because of their interesting molecular topo-logies and various potential applications in catalysis,superconductor, magnetism, nonlinear optics, sen-sors and molecular recognition[1～4]. On the otherhand, the attachment of mono- or polypyridyl frag-ments to a ferr…     

Crystal Structure of Calcium Complex with Cyanuric Acid Ligand［Ca（C_3H_3N_3O_3－O）（H_2O）_6］［（OH）（C_3H_2N_3O_3）］

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Synthesis, Properties and Crystal Structure of a Novel Coordinated Polymer: {(H2en)(H3O)[(BiPb(C2O4)4(H2O)2)]·2(H2O)}n

A novel oxalate compound {(H2en)(H3O)[BiPb(C2O4)4(H2O)2]·2(H2O)}n 1 (en = ethylenediamine) containing lead and bismuth has been synthesized by hydrothermal methods, and structurally characterized by X-ray single-crystal diffraction. It crystallizes in monoclinic, space group P21/c with a = 11.6160(1), b = 12.7426(1), c = 15.5683(5) (A), β = 108.442(4)°, BiPbC10N2O21H21, Mr = 921.46, V = 2186.0(4) (A)3, Z = 4, Dc = 2.800 g/cm3, F(000) = 1712 and μ(MoKα) = 15.837 mm-1. The final R = 0.0502 and wR = 0.1261 for 3391 observed reflections with I > 2(σI). The title com- pound consists of 2-D polyanions and protonized organic amine cations, and they are combined to each other by static attractive force and H-bonds to form the so-called organic-inorganic hybrid material.     

Synthesis and Crystal Structure of [Cu(phen)2(SO4)(H2O)]·0.5C4H4O4·7H2O

The title compound, [Cu(phen)2(SO4)(H2O)]·0.5C4H4O4·7H2O (phen = 1,10-phe-nanthroline and C4H4O4 = fumaric acid), has been synthesized and characterized by single-crystal X-ray diffraction. The crystal is of triclinic, space group P with a = 11.4827(2), b = 11.9086(2), c = 13.77350(10)(A), α = 80.6830(10), β = 66.6480(10), γ = 64.0480(10)o, V = 1554.63(4) (A)3, Mr = 722.17, Z = 2, Dc = 1.543 g/cm3, μ = 0.845 mm-1, F(000) = 750, R = 0.0349 and wR = 0.0837 for 4754 observed reflections (I > 2σ(I)). The compound contains a six-coordinated copper(II) center, which is surround by four N atoms of two phen ligands (Cu-N distances in the range of 1.997(2)～2.225(2)(A)), one sulfate O atom (Cu-O = 2.0037(17) (A)) and one water O atom (Cu-O(5w) = 2.719(2) (A)) in a distorted octahedral geometry. Extensive hydrogen-bonding interactions are involved in water molecules, ligated sulfate anions and fumaric acid molecules. In addition, π-π interactions via aromatic nitrogen-containing ligands are also discussed. The combination of non-covalent interactions leads to the formation of a 3-D network structure.