Crystal Structure and Catalytic Properties of Tetrakis（4-hydroxyphenyl）Porphyrinato Manganese （Ⅲ） Chloride （MnTHPPCI）

The crystal structure of meso-tetrakis （4-hydroxyphenyl） porphyrinato manganese chloride （MnTHPPC1） and its supramolecular architecture based on the hydrogen bonds of one counter C1 anion with four hydrogen atoms of four-OH groups from different MnTHPPC1 molecules cooperated by self-assembly of the porphyrin units were first repor-ted. This compound crystallized in the tetragonal space group 14/m with a = 1.39928（7） nm, b = 1.39928（7） nm, c =0.94498（10） nm, V= 1.8503（2） nm^3, and Z =2. As a catalyst, MnTHPPC1 also showed a high catalytic acti-vity in the conversion from 1-naphthylamine （1-NA） to his （4-oxo-benzo-2-cyclohexen-l-yl） amine （BOBCHA） v/a oxidative coupling under mild conditions.     

四(4-乙烯基吡啶)硝酸铜(Ⅰ)配合物的结构、电化学和热稳定性能研究(英文)

The title complex Cu(Vpy)NO3 (Vpy=4-vinylpyridine) has been synthesized and structurally characterized by X-ray single crystal diffractometry. The complex crystallizes in triclinic system, P1 space group with the cell parameters of a=1.004 2(2) nm, b=1.631 7(3) nm, c=1.887 7(4) nm, α=81.54(2)°, β=77.44(2)°, γ=79.39(2)°, V= 2.948 9(11) nm3, Z=4, and Dc=1.230 g·cm-3, the final R1=0.075 2, wR2=0.139 1. The complex crystallizes with two molecules in the asymmetric unit. Each Cu(Ⅰ) ion is coordinated by four N atom from the Vpy ligands and one O atoms from the nitrate anion, resulted in a square pyramidal geometry. The electrochemical studies reveal that redox of Cu2+/Cu+ in the complex is a quasi-reversible process. CCDC: 736638.     

Synthesis,Structure Characterization and Biological Activity of a Novel Amino Acid Salt(HAla)_8(H_3O)_(10)[PMo_(12)O_(40)]_6·22H_2O

A novel compound was synthesized and characterized by means of elemental analysis, IR and UV spectra, TG, CV and single crystal X-ray diffraction. The compound crystallized in an orthorhombic space group C222 with a = 1. 622 4(3) nm, b=3. 498 4(7) nm, c=l. 301 5(3) nm,V=7. 387(3) nm3, Z = 6, R1 = 0. 037 3, wR2 = 0. 114 0. The Ala (Ala = alanine) molecules were protonated at the amino nitrogen N (1) and the C (2) of Ala group with the terminal oxygen atom O(15), O(14), O(26) and O(27) of the polyoxometalates participating in the hydrogen bond network. The anti-tumor activity of the title compound was estimated against Hela and Pc-3m cancer cells.     

Bis(1-(4-(dimethylamino)benzylidene)-4-phenylthiose micarbaznato)palladium(Ⅱ):Synthesis,Crystal Structure and Its Dual Fluorescence Property

The title compound bis(1-(4-(dimethylamino)benzylidene)-4-phenylthiosemicar-bazato)-palladium(Ⅱ)(PdL2) was obtained by reacting 1-(4-(dimethylamino)benzylidene)-4-phenyl-thiosemicarbazide with dichlorobis(benzonitrile)palladium(Ⅱ) in methanol,and its structure was characterized by single-crystal X-ray diffraction.The crystal of PdL2 was obtained in dimethyl-formamide(DMF) solvent with solvent molecules involved in the cell and crystallizes in the monoclinic system,space group C2 with a = 18.485(15),b = 7.090(5),c = 17.595(11) ,β = 121.21(3)o,V = 1972(2) 3,Z = 2,Mr = 847.40,Dc = 1.427 g/cm3,μ = 0.624 mm-1,F(000) = 880,R = 0.0607 and wR = 0.1358.The Pd atom adopts a distorted square planar coordination geometry with two Pd-N and two Pd-S bonds.The ligand loses a proton from its tautomeric thiol form and coordinates to the Pd atom via mercapto sulfur and the imine nitrogen atom,which binds to palladium as bidentate N,S-donors forming five-membered chelate rings.The complex formed hydrogen bonding interaction with solvent DMF molecules from the hydrogen of phenylamine to the oxygen of DMF and several intramolecular hydrogen bonds.Pd(Ⅱ) perturbed ligand π-π* transition and metal-to-ligand charge transfer(MLCT) transition are observed in its electronic absorption spectra.The complex exhibits intraligand 1π-π*(IL) state and MLCT state dual fluorescent emissions in organic solvent at room temperature.     

配合物[Tb(p-ClBA)_3(phen)]_2的结构和性能(英文)

Terbium p-chlorobenzoate complex with 1,10-phenanthroline, [Tb( p-ClBA)_3phen]_2 (1) has been obtained in the ethanol solution, where p-ClBA=p-chlorobenzoate and phen=1,10-phenanthroline. It crystallizes in the triclinic system, space group P1, a=1.008 1(2) nm, b=1.185 7(2) nm, c=1.431 1(3) nm, α=110.826(4)°, β=96.436(4)°, γ=101.737(4)°, Z=2. The two Tb(Ⅲ) ions are linked by four carboxylate groups through their bidentate bridging modes, forming a dimeric unit with crystallographic inversion center. Each terbium ion has an eight-coordinate geometry with four of the coordination sites occupied by four oxygen atoms from the four bridging carboxylates, respectively, two oxygen atoms from bidentate carboxylate, and the remaining positions occupied by two nitrogen atoms from a 1,10-phenanthroline molecule. The Tb(Ⅲ) ion adopt a distorted square antiprism coordination geometry. The excitation and luminescence data observed at room temperature show that the title complex emits very intensive green fluorescence under ultraviolet light. The result of thermal analysis indicates the complex [Tb(p-ClBA)_3phen]_2 is quite stable to heat. CCDC: 221921.     

Primary Organicamine Templated Indium Iodate (H_2en)KIn(IO_3)_6·2(H_2O) with Hydrogen-bonded Helices

The first primary organicamine templated indium iodate with the formula (H2en)KIn(IO3)6·2(H2O) was hydrothermally synthesized via reaction at 100 °C for 7 d and characterized by single-crystal X-ray diffraction and thermal analysis. The compound crystallized in a triclinic system with space group P1, a=0.69803(14) nm, b=0.70863(14) nm, c=1.2091(2) nm, α=76.417(4)°, β=79.953(4)°, γ=72.206(3)°, V=0.55012(19) nm3. Structure determination indicates that it is made up of zero-dimensional units each of which consists of [In(IO3)6]3-anion, potassium, water and ethylenediamine cation. The most striking feature of the compound is that it possesses helical hydrogen bonds formed by organic amine template, water molecules and inorganic network.     

Synthesis and characterization of a new open-framework zinc phosphite (4,4′-(C5H4N)2(CH2)3)·[Zn3(HPO3)4]

Employing 4,4-trimethylenedipyridine as a template,a new two-dimensional zinc phosphite (4,4-(C5H4N)2(CH2)3)· [Zn3(HPO3)4 ] has been prepared at room temperature and characterized by single-crystal X-ray diffraction,FTIR,elemental analysis,powder X-ray diffraction,and thermogravimetric analysis.The compound crystallizes in the monoclinic space group P2 1 /c,with cell parameters,a=9.3309(19),b=14.798(3),c=33.637(7),β=91.11(3),V=4643.8(16) nm 3 and Z=4.The connectivity of the ZnO4 tetrahedra and HPO 3 pseudo pyramids results in infinite corner-sharing 4-membered ring chains as second building units which are further linked by Zn O P bonds to form a 2-D layer that with interesting 8-membered ring channels along the [100] direction.The diprotonated 4,4-trimethylenedipyridine molecules sit in the middle of the layers along the [100] direction and interact with the framework via hydrogen bonds.     

Syntheses, Crystal Structures and Photoluminescence Properties of Cadmium(Ⅱ) and Nickel(Ⅱ) Complexes with 2-(2-Benzimidazolyl)quinoline

Two novel complexes, [Cd2(BMQU)2Cl4] (1) and [Ni(BMQU)2HPO4]·1.5H2O (2) (BMQU = 2-(2-benzimidazolyl)quinoline), were synthesized by the hydrothermal method and characterized by elemental analysis, IR, and TG-DTG. The crystal structures were determined by single-crystal X-ray diffraction. Both 1 and 2 crystallize in the triclinic system, space group P . The data for 1: a = 0.8342(7), b = 0.9226(9), c = 1.0646(8) nm, α = 90.819(2), β = 97.466(2), γ = 98.280(2)°. The Cd(Ⅱ) is coordinated with three chlorine atoms and two nitrogen atoms of a BMQU molecule, generating a distorted square-pyramidal geometry. The dinuclear Cd(Ⅱ) complex is formed by two chlorine bridge bonds, and the one-dimensional chain structure is constructed with the hydrogen bond N-H…Cl and π-π stacking interaction. The data for 2: a = 1.2251(1), b = 1.2451(1), c = 1.2868(1) nm, α = 107.510(2), β = 98.630(1), γ = 109.921(2)°. The Ni(Ⅱ) is coordinated with four nitrogen atoms of two BMQU molecules and two oxygen atoms of a HPO42-, forming a distorted-octahedral geometry. The two-dimensional layer structure is formed by the hydrogen bonds and π-π stacking interaction between neighboring molecules. Complex 1 shows a strong blue fluorescence emission (λmax= 456 nm) at solid state.     

Synthesis,Structure and Photochromism of a New Diarylethene and Its Ag(Ⅰ) Complex

A new symmetric diarylethene containing cyano group was synthesized and structurally characterized by elemental analysis,IR,1 H NMR and X-ray single-crystal diffraction.It belongs to the monoclinic system,space group C2/c with a = 18.848(6),b = 8.561(2),c = 16.875(5) ?,β = 100.398(6)o,V = 1344.6(11) ?~3,Z = 4,μ = 0.262 mm~(-1),Dc = 1.415 g/cm~3,M_r = 570.56,F(000) = 1160,the final R = 0.0808 and wR = 0.2107 with I 2σ(I).The two thienyls adopt reactive anti-parallel conformation and the carbon distance of photocyclization is 3.57 ?.The neighboring molecules are stacked closely with C–H…F hydrogen bonding.In addition,the photochromism of the new compound was investigated in solvents with different polarity and PMMA film.The alternative photo-irradiation of 254 nm light and ≥550 visible light can induce the reversible photo-cyclization and photo-reversion with the color interconversion between colorlessness and blue.In THF solution,the λ_(max) of diarylethene in PSS in visible band is 585 nm.The diarylethene further reacted with AgBF_4 in benzene to give rise to complex 1,which was structurally characterized by elemental analysis,IR,ESI-MS and TG.1 demonstrated reversible photochromism in both solution and PMMA film.The complexation of metal ions with diarylethene leads to a minor red-shift of the λ_(max) of 1 in THF in PSS to 590 nm.     

Structure and electrospray mass spectrometry studies on dithiacyclooctan-3-ol-containing palladium (II) complex of trans -[Pd(dtco-3-OH)_2](ClO_4)_2·2DMSO

The structure of trans-[Pd(dtco-3-OH)2] (ClO4)2·2DMSO, in which dtco-3-OH is dithiacyclooctan-3-ol and DMSO is dimethyl sulfoxide, was determined by X-ray crystallographic analysis. The crystal data: space group pi, a = 0.7077(2) nm, b = 1.0788(1) nm, c = 1.1111(1) nm, α=67.710(8)°, β = 73. 59(2)°, γ = 85. 39(2)°,R1 = 0 . 0368 and Rw = 0.0998. The palladium (II) is coordinated by four sulfur atoms with a regular square planar configuration. The Pd-S distances are 0.2314(1) and 0.2317(1) nm, respectively. Both dtco-3-OH ligands are in the boat-chair configuration and two hydroxyl groups are on the opposite sites of the PdS4 coordination plane and are towards Pd(II). The Pd-O distance is 0. 285 nm, indicating a weak interaction between them. A typical hydrogen bond between the hydroxyl group of dtco-3-OH ligand and DMSO was observed in the crystal structure. An aqueous solution prepared with the crystals of the complex was used for the investigation of electrospray mass spectrometry ( ESMS ). Besid     

Synthesis, Crystal Structure and Photoluminescent Property of a Novel Silver(I) Compound {[Ag(bpp)]_2(Hphth)(NO_3)·(H_2O)_2}_n

Self-assembly of Ag(I) nitrate, 1,3-bis(4-pyridyl)propane (bpp) and phthalic acid monopotassium salt (KHphth) in CH3OH-H2O solution produced the title complex, {[Ag(bpp)]2(Hphth)(NO3)·(H2O)2}n, which was characterized by single-crystal X-ray diffraction, elemental analysis, IR spectrum, and photoluminescent spectrum. Single-crystal X-ray analysis revealed that the complex crystallizes in a monoclinic system, space group P21/c, with a = 15.4174(5), b = 8.6398(2), c = 25.2466(8) , β = 91.072(1)o, V = 3362.34(17) 3, Z = 4, C34H37N5O9Ag2, Mr = 875.43, Dc = 1.729 g/cm3, μ = 1.228 mm-1, F(000) = 1768, the final R = 0.0749 and wR = 0.1580 for 5754 reflections with I > 2σ(I). The Ag atom is coordinated by two N atoms from two bpp molecules in an approximately linear geometry. The Ag(I) ions are linked by the bpp molecules to form one-dimensional zigzag chains propagating along the c axis. The Hphth- and nitrate counter-ions are bridged by solvent water molecules through hydrogen bonds to generate a one-dimensional chain extending along the b axis. Electrostatic interactions between cations and anions, extensive hydrogen bonds and π-π interactions are responsible for the three-dimensional supramolecular structure. In the solid state, the compound exhibits blue photoluminescence with the maximum at 436 nm upon excitation at 344 nm.     

Hydrothermal Synthesis and Characterization of Ce_(1-x)Mn_xO_(2-δ) Solid Solutions

Nanocrystals of Ce1-xMnxO2-δ(x=0.00,0.05,0.10,0.15,and 0.20) were synthesized by a hydrothermal reaction route.The solid solutions crystallized in a cubic fluorite structure with a particle size in the range of 11～15 nm.The incorporation of Mn ions in CeO2 resulted in a lattice volume reduction.Mn ions showed a mixed valence state of +2,+3 and +4 in CeO2 lattice.An obvious red-shift of the absorption threshold edge was observed from the UV-visible spectrum.Compared with the bulk CeO2,Ce1-xMnxO2-δ nanocrystals exhibited a lower releasing oxygen temperature as indicated by TPR technique.     

一维链状锰配位聚合物[Mn(1,5-nds)(Him)_4]_n的合成、晶体结构及热稳定性研究(英文)

The synthesis,structural characterization and thermal behavior of a novel one-dimensional manganese (Ⅱ) complex of formula [Mn(1,5-nds)(Him)4]n [1,5-nds=naphthalene-1,5-disulfonate,Him=imidazole] is reported.The complex crystallizes in the triclinic system,space group P1,with a=0.835 42(13) nm,b=0.983 45(18) nm,c= 0.987 42(19) nm,α=60.523 0(10)°,β=97.748(2)°,γ=87.189(2)° and Z=2.The 1,5-nds ligand assumes the μ2 coordination mode and interlinks Mn(Ⅱ) ions into infinite one-dimensional chain structure along [111] direction,with the adjacent Mn…Mn distance being 1.144 99(12) nm.The chains are assembled into a three-dimensional supramolecular architecture via hydrogen bonds and C-H…π interactions.IR spectra and thermal analysis data are in agreement with the crystal structure.     

Synthesis,Structure and Properties of a New Terbium(Ⅲ) Complex Tb_2(C_(15)H_(11)O_3)_6(phen)_2

A new terbium(Ⅲ) complex Tb_2(C_(15)H_(11)O_3)_6(phen)_2 has been synthesized with 2-(4-methylbenzoyl)benzoic acid and 1,10-phenanthroline as ligands.Crystal data for the complex are as follows:monoclinic,space group P2_1/n,a=15.0786(6),b=13.5762(5),c=22.9683(9) A,β=104.130(4)°,V=4559.6(3) A~3,D_c=1.540_g/cm~3,Z=2,μ(MoKα)=1.615 mm~(-1),F(000)=2136,the final R=0.0528 and wR=0.0740.The Tb(Ⅲ) ion is coordinated by eight atoms to give a distorted square antiprism coordination geometry.The complex shows four fluorescence emission bands arising from the transitions of Tb~(3+5)D_4→~7F_6(490 nm),~5D_4→~7F_5(546 nm),~5D_4→~7F_4(588 nm) and ~5D_4→~7F_3(622 nm).The complex is an antiferromagnet in the range of 300～2 K.Also reported in the paper is the thermal stability property of the title complex.     

二维网状Pd(Ⅱ)配合物的合成、晶体结构及电化学性质(英文)

A novel palladium(Ⅱ) complex [Pd(H2bpdc)Ala]Cl·3H2O (where H2bpdc is 2,2′-bipyridine-3,3′-dicar- boxylic acid and Ala is L-alanine) has been synthesized and characterized by IR spectra and elemental analysis. The crystal structure of the complex has been determined by single-crystal X-ray diffraction analysis. It crystallizes in triclinic system, space group P1 with a=0.685 5(2) nm, b=0.988 4(4) nm, c=1.349 6(4) nm, α=98.375(8)°, β= 97.900(15)°, γ=90.118(15)°, V=0.895 9(5) nm3, Z=2. In the molecule, Pd(Ⅱ) atom is four-coordinated and located at the centre of a planar quadrangle. The complex is assembled via intramolecular π-π stacking interactions and hydrogen bonds, which forms 2D network. The cyclic voltammetric behavior of the complex was also investigated.     

Synthesis, Crystal Structure and Photoluminescent Property of a Novel Silver(Ⅰ) Compound {[Ag(bpp)]2(Hphth)(NO3)·(H2O)2}n

Self-assembly of Ag(Ⅰ) nitrate, 1,3-bis(4-pyridyl)propane (bpp) and phthalic acid monopotassium salt (KHphth) in CH3OH-H2O solution produced the title complex,{[Ag(bpp)]2(Hphth)(NO3)·(H2O)2}n, which was characterized by single-crystal X-ray diffraction,elemental analysis, IR spectrum, and photoluminescent spectrum. Single-crystal X-ray analysis revealed that the complex crystallizes in a monoclinic system, space group P21/c, with α =15.4174(5), b = 8.6398(2), c = 25.2466(8) (A), β = 91.072(1)°, V = 3362.34(17) (A)3, Z = 4,C34H37N5O9Ag2, Mr = 875.43, Dc = 1.729 g/cm3, μ = 1.228 mm-1, F(000) = 1768, the final R =0.0749 and wR = 0.1580 for 5754 reflections with I ＞ 2σ(I). The Ag atom is coordinated by two N atoms from two bpp molecules in an approximately linear geometry. The Ag(Ⅰ) ions are linked by the bpp molecules to form one-dimensional zigzag chains propagating along the c axis. The Hphth-and nitrate counter-ions are bridged by solvent water molecules through hydrogen bonds to generate a one-dimensional chain extending along the b axis. Electrostatic interactions between cations and anions, extensive hydrogen bonds and π-π interactions are responsible for the three-dimensional supramolecular structure. In the solid state, the compound exhibits blue photoluminescence with the maximum at 436 nm upon excitation at 344 nm.     

Synthesis, Crystal Structure and Photoluminescent Property of a Novel Silver(Ⅰ) Compound {[Ag(bpp)]2(Hphth)(NO3)·(H2O)2}n

Self-assembly of Ag(Ⅰ) nitrate, 1,3-bis(4-pyridyl)propane (bpp) and phthalic acid monopotassium salt (KHphth) in CH3OH-H2O solution produced the title complex,{[Ag(bpp)]2(Hphth)(NO3)·(H2O)2}n, which was characterized by single-crystal X-ray diffraction,elemental analysis, IR spectrum, and photoluminescent spectrum. Single-crystal X-ray analysis revealed that the complex crystallizes in a monoclinic system, space group P21/c, with α =15.4174(5), b = 8.6398(2), c = 25.2466(8) (A), β = 91.072(1)°, V = 3362.34(17) (A)3, Z = 4,C34H37N5O9Ag2, Mr = 875.43, Dc = 1.729 g/cm3, μ = 1.228 mm-1, F(000) = 1768, the final R =0.0749 and wR = 0.1580 for 5754 reflections with I ＞ 2σ(I). The Ag atom is coordinated by two N atoms from two bpp molecules in an approximately linear geometry. The Ag(Ⅰ) ions are linked by the bpp molecules to form one-dimensional zigzag chains propagating along the c axis. The Hphth-and nitrate counter-ions are bridged by solvent water molecules through hydrogen bonds to generate a one-dimensional chain extending along the b axis. Electrostatic interactions between cations and anions, extensive hydrogen bonds and π-π interactions are responsible for the three-dimensional supramolecular structure. In the solid state, the compound exhibits blue photoluminescence with the maximum at 436 nm upon excitation at 344 nm.     

Crystal Structure, Nano-particle Morphology and Interaction with ATP of[NH3CH2CH(NH2)CH3]2[M(Ⅵ)O2(OC6H4O)2] (M=Mo0.6W0.4) and Its Activity to Promote DNA Cleavage

The title complex[NH3CH2CH(NH2)CH3]2[M(Ⅵ)O2(OC6H4O)2](M=Mo0.6W0.4)was synthesized via a simple solution-phase chemical route. The determination of single crystal X-ray diffraction revealed that the title compound is crystallized in a monoclinic system with P2(1)/n space group, a=1.0913(10) nm, b=1. 0442(10) nm,c=1.8842(19) nm, α=90°, β=96.530(17)°, γ=90°,Z=4, and V=2. 133(4) nm3. The mononuclear anionic unit [M(Ⅵ)O2(OC6H4O)2]2- displays chiral pseudo-octahedral [MO6] coordination geometry and is ges show that the title complex is comprised of nano-particles with diameters ranging from 20 to 50 nm. The NMR study shows the 1 H downfield chemical shifts of [NH3CHaHbCH(NH2)CH3] cations in the title complex when it is mixed with adenosine-triphosphate(ATP), and the chemical shift difference between Ha and Hb is increased greatly,and most of the catecholate ligands dissociate from the central metal atoms. The DNA cleavage activity experiment reveals that DNA cleavage promoted by the title complex is lower than that by Na2MoO4 which possesses antitumor property, but higher than that by Na2WO4.     

含有药物配体依诺沙星的二维配位聚合物的合成、晶体结构和光致发光性质研究

Two new 2D coordination polymers of[M(Enox)_2]·C_2H_5OH(M=Zn,1 and Co,2;HEnox=1,4-dihydro-1-ethyl-6-fluoro-4-oxo-7-piperazine-1,8-naphtyridine-3-carboxylic acid)were synthesized under hydrothermal con-ditions.The single crystal X-ray diffraction analyses showed that 1 and 2 are isostructural.The Zn(Ⅱ)in 1 and Co(Ⅱ)ions in 2 are six-coordinated in an octahedral environment with an equatorial plane composed of four oxygen atoms:two of them from the 4-oxo and the other two from 3-carboxylate of two coordinated Enox ligands,forming a stablesix-membered chelating ring with the apical positions occupied by two N atoms of the piperazinyl rings.Thus,themolecules were self-assembled into a 2D neutral square grid with cavity dimensions of 1.3399 nm×1.3399 nm for1 and 1.3389 nm×1.3389 nm for 2,respectively.Compound 1 emits strong blue fluorescence on irradiation by UVlight in the solid state at room temperature.     

Solvothermal Synthesis, Crystal Structure and Electrochemical Property of Complex [Co(p-MBA)2(2,2'-bipy)(H2O)]·(H2O)

One novel complex [Co(p-MBA)2(2,2'-bipy)(H2O)]·(H2O) has been synthesized by the reaction of p-methylbenzoic acid with 2,2'-bipyridine in the solvent mixture of water and methanol. It crystallizes in triclinic, space group P-1 with a=0.70479(14), b=1.1211(2), c=1.6718(3) nm, α=103.806(3), β=90.795(3), γ=104.207(3)°, V=1.2399(4) nm3, Mr=512.41, Dc=1.373 g/cm3, Z=2, F(000)=532, μ=0.733 mm-1, R=0.0432 and wR=0.0957. The crystal structural analysis shows that the cobalt atom is coordinated with three oxygen atoms from two p-methylbenzoic acids and one water molecule and two nitrogen atoms from one 2,2'-bipyridine,forming a distorted square-pyramidal coordination geometry. The cyclic voltammetry behavior of the complex is also reported.