The title complex Mn(HL)4(NCS)2(CH3CH2OH)2 has been achieved via self- assembly by incorporating manganese(II) into pyridine-3-carbaldehyde thiosemicarbazonate ligand, and characterized by elemental analysis and singl...The title complex Mn(HL)4(NCS)2(CH3CH2OH)2 has been achieved via self- assembly by incorporating manganese(II) into pyridine-3-carbaldehyde thiosemicarbazonate ligand, and characterized by elemental analysis and single-crystal X-ray diffraction study. The crystal crystallizes in triclinic, space group P1, with a = 8.896(2), b = 9.530(2), c = 14.520(4) , α = 87.035(4), β = 88.112(4), γ = 69.434(4)o, V = 1150.9(5) 3, Z = 1, Mr = 984.17, Dc = 1.420 g/cm3, μ(MoKα) = 0.612 mm-1, F(000) = 511, the final R = 0.0574 and wR = 0.1547 for 2855 observed reflections with I > 2σ(I). The complex contains one six-coordinated manganese ion connected by two thiosemicarbazide ligands, in which the thiosemicarbazone ligand acts as a monodentate ligand and coordinates to the center metal atoms via the pyridyl nitrogen atoms, two ethanol molecules and two isothiocyanic anions to give rise to a mononuclear structure. The coordination of a po- tentially tridentate thiosemicarbazone in manganese(II) complex without using its sulfur and imine nitrogen sites is unusual. Hydrogen bonds existing in the complex link the different components to stabilize the crystal structure.展开更多
A cobalt paradodecatungstate [Co(H2O)5]2[Co(H2O)4]3[H2W12O42]·11H2O has been successfully synthesized and structurally characterized by X-ray crystallography. Structure analysis indicates that the title compound ...A cobalt paradodecatungstate [Co(H2O)5]2[Co(H2O)4]3[H2W12O42]·11H2O has been successfully synthesized and structurally characterized by X-ray crystallography. Structure analysis indicates that the title compound is of monoclinic, space group P21/n, with a = 13.449(3), b = 19.585(4), c = 13.990(3) , β = 113.79(3)°, V = 3371.8(12) ?3, Z = 2, R = 0.0519 and wR = 0.1242. The title compound exhibits a novel 3D extended network structure constructed by interconnecting the paradodecatungstate polyanion [H2W12O42]10- clusters and cobaltII coordination ions.展开更多
A 1D zigzag polyoxometalate [(CH3)4N]1.50H3.50[Gd(GeW11O39)(H2O)2]·2.5H2O (1) was synthesized by reaction of the monovacant polyanion [α-GeW11O39]8-with Gd3+ ions in aqueous solution and characterized by IR, UV ...A 1D zigzag polyoxometalate [(CH3)4N]1.50H3.50[Gd(GeW11O39)(H2O)2]·2.5H2O (1) was synthesized by reaction of the monovacant polyanion [α-GeW11O39]8-with Gd3+ ions in aqueous solution and characterized by IR, UV spectra, ICP, and X-ray crystallography. X-ray single-crystal structural analysis indicated that the title compound crystallized in a monoclinic lattice, C2/c space group with a=2.8201(5), b=2.2885(3), c=2.4033(4) nm, β=123.875 (2), V=12.878(4) nm3, Z=8, R1=0.0623, wR2=0.1287. The solid-state structure of the title compound displayed an infinite one-dimensional arrangement built up of [α-GeW11O39]8-polyanions connected by GdIII cations.展开更多
A Schiff base ligand(H2CSF,C13H11NO4,1) derived from 3-carboxylsalicylaldehyde and furfurylamine,and its trinuclear complex [Ni3(CSF)2(CH3COO)2(DMF)2(H2O)2](2) were synthesized.Compound 1 was characterized by elementa...A Schiff base ligand(H2CSF,C13H11NO4,1) derived from 3-carboxylsalicylaldehyde and furfurylamine,and its trinuclear complex [Ni3(CSF)2(CH3COO)2(DMF)2(H2O)2](2) were synthesized.Compound 1 was characterized by elemental analysis,1H NMR,IR,MS and X-ray diffraction analysis.The crystal of 1 belongs to the monoclinic system,space group P21/c with a = 8.472(2),b = 19.743(5),c = 7.2300(18) ,β = 110.278(4)°,V = 1134.4(5) 3,Z = 4,Mr = 245.23,Dc = 1.436 g·cm-3,μ = 0.108 mm-1,F(000) = 512,λ = 0.71073 ,the final R = 0.0440 and wR = 0.1199 for 1426 observed reflections(I > 2σ(I)).In the crystal of 1,there exist intramolecular hydrogen bonds and weak intermolecular C-H···O hydrogen bonds.Compound 2 was characterized by elemental analysis,IR,TG and X-ray diffraction analysis.The crystal of 2 is of triclinic system,space group P1 with a = 10.1237(17),b = 10.4086(18),c = 10.4884(18) ,α = 82.528(2),β = 67.339(2),γ = 83.010(2)°,V = 1008.1(3) 3,Z = 1,Mr = 962.87,Dc = 1.586 g·cm-3,μ = 1.463 mm-1,F(000) = 498,λ = 0.71073 ,the final R = 0.0517 and wR = 0.0805 for 2065 observed reflections(I > 2σ(I)).The geometry of the trinuclear molecule is centrosymmetric,in which every Ni(Ⅱ) ion is coordinated in a slightly distorted octahedron.The three Ni(Ⅱ) ions are arranged in a straight line.The two CSF2-ions act as NOO tridentate ligands with the phenolate and carboxylate oxygen as bridging atoms.The coordination atoms of CSF2-anions and water molecules are coordinated on the equatorial plane,while the two bridging acetate ions and two DMF are trans-coordinated on the apical sites.展开更多
A new hybrid polyoxometalate-based complex, [CuI(phen)2]4(SiW12O40) (phen = 1,10-phenanthroline), has been synthesized by hydrothermal method and characterized with the aid of elemental analysis, IR, UV spectra and th...A new hybrid polyoxometalate-based complex, [CuI(phen)2]4(SiW12O40) (phen = 1,10-phenanthroline), has been synthesized by hydrothermal method and characterized with the aid of elemental analysis, IR, UV spectra and thermal analysis studies. The result of X-ray crystallo- graphy analysis exhibits that the title compound crystallizes in the orthorhombic space group P212121, and the formula is C96H64N16Cu4SiW12O40. Crystal data: a = 18.3574(14), b = 21.1952(16), c = 27.992(2) , Mr = 4570.08, V = 10891.4(14) 3, Z = 4, Dc = 2.787 g/cm3, μ = 13.478 mm–1, R = 0.0364, wR = 0.0638 (I > 2σ(I)) and F(000) = 8360. The complex consists of one α-Keggin anion [SiW12O40]4– and four discrete [CuⅠ(phen)2]+ cations. The valence sum calculations for the Cu atoms suggest that all four Cu atoms are in the +1 oxidation state.展开更多
A novel polyoxometalate-based composite compound [Ni(phen)2][Hphen](AsW12O40) (phen = 1,10-phenanthroline) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TGA, ESR spectroscopy and s...A novel polyoxometalate-based composite compound [Ni(phen)2][Hphen](AsW12O40) (phen = 1,10-phenanthroline) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TGA, ESR spectroscopy and single-crystal X-ray diffraction. Each structure unit of 1 consists of one polyoxoanion AsW12O403-, one free phenanthroline molecule and one coordination cation [Ni(phen)2]2+. The title compound crystallizes in the orthorhombic system, space group P212121, with a = 12.2383(7), b = 21.0884(11), c = 22.3237(12) , V = 5761.4(5) 3, Mr = 3520.44, Z = 4, Dc = 4.059 g/cm3, F(000) = 6204, μ(MoKα) = 24.844 mm-1, GOF = 1.022, the final R = 0.0376 and wR = 0.0742 (I > 2σ(I)) for 865 parameters and 9637 observed reflections with I > 2σ(I).展开更多
The synthesis, X-ray crystal structure, thermal properties and electrochemistry of the new complex formulated as {Er(DMSO)7}PW12O40 are reported. The single-crystal X-ray analysis reveals that the crystal crystallizes...The synthesis, X-ray crystal structure, thermal properties and electrochemistry of the new complex formulated as {Er(DMSO)7}PW12O40 are reported. The single-crystal X-ray analysis reveals that the crystal crystallizes in the monoclinic system, space group P21/c with a = 11.767(2), b = 14.909(3), c = 34.905(7) , β = 98.97(3)°, Mr = 3591.33, V = 6049(2) 3, Dc = 3.944 g/cm3, Z = 4, GOOF = 1.098, F(000) = 6340, R = 0.0490 and wR = 0.1202. Crystal structure analysis indicates that the Er(Ⅲ) is seven-coordinate with a distorted pentagonal bipyramid and combines to the anion [PW12O40]3- via static electric force.展开更多
The title complex Co(L)2Cl·4H2O I has been achieved via self-assembly by incorporating cobalt into 2-benzoylpyridine thiosemicarbazonate ligand, and characterized by elemental analysis, infrared spectra, mass spe...The title complex Co(L)2Cl·4H2O I has been achieved via self-assembly by incorporating cobalt into 2-benzoylpyridine thiosemicarbazonate ligand, and characterized by elemental analysis, infrared spectra, mass spectra and single-crystal X-ray diffraction study. The crystal crystallizes in monoclinic, space group P21/n, with a=10.227(3), b=17.363(4), c=17.459(4), β=100.408(4)o, V=3049.2(13)3, Z=4, Mr=677.08, Dc=1.475 g/cm3, μ(MoKα)=0.834 mm-1, F(000)=1400, the final R=0.0747 and wR=0.0896 for 1663 observed reflections with I > 2σ(I). The complex contains one six-coordinated cobalt ion connected by two thiosemicarbazone ligands which act as a tridentate ligand to coordinate with the center metal atoms via two pyridyl nitrogen atoms, two imine nitrogen atoms and two sulfur atoms giving rise to a mononuclear structure. Hydrogen bonds existing in the complex link the different com-ponents to stabilize the crystal structure. The antitumor activity of the title complex was tested against A549 lung cancer cell line. Complex I exhibits antitumor activity.展开更多
A new compound based on polyoxovanadate [{Ni(en)2}2Sb8V14O42]·5.5H2O(en=ethylenediamine)(1) was synthesised hydrothermally as black rhombus crystals.Compound 1 crystallized in the monoclinic system with space gro...A new compound based on polyoxovanadate [{Ni(en)2}2Sb8V14O42]·5.5H2O(en=ethylenediamine)(1) was synthesised hydrothermally as black rhombus crystals.Compound 1 crystallized in the monoclinic system with space group P21/n,Z=4,a=1.46953(9) nm,b=1.28623(8) nm,c=1.76008(11) nm,β=105.7230(10)°.In the asymmetric unit,cluster {Sb8V14O42} can be considered as an Sb derivative of the {V18O42} unit.Each {Sb8V14O42} cluster as a building block interconnected to four other neighboring units by {Ni(en)2} bridging groups which are linked through the terminal oxygen atoms of the polyoxoanions,forming a two dimensional network.展开更多
A novel double 1:11 series arsenotungstate, [CuI(phen)2]5H6[Sm(AsW11O39)2]·6H2O (phen=1,10-phenanthroline) was synthesized by the hydrothermal method and characterized by elemental analysis, IR spectra, and singl...A novel double 1:11 series arsenotungstate, [CuI(phen)2]5H6[Sm(AsW11O39)2]·6H2O (phen=1,10-phenanthroline) was synthesized by the hydrothermal method and characterized by elemental analysis, IR spectra, and single-crystal X-ray diffraction. The title compound was monoclinic, space group P21/c, a=3.75710(2) nm, b=1.39776(8) nm, c=3.33735(18) nm, β=96.967(10)°, V=17.3969(17) nm3, Z=4. Single crystal X-ray structural analyses revealed that the dimeric polyanion, [SmAs2W22O78]1–, consisted of one central Sm3+ ion and two tetradentate heteropoly ligands [AsW11O39]7–. The Sm3+ ion and two tetradentate defective [AsW11O39]7– anions were joined together by the sharing of four oxygen atoms from each heteropoly ligand. The bond valence sum (BVS) calculations of the title compound suggested that all four Cu atoms were in the +1 oxidation sate.展开更多
A series of ligands,HL1(2-acetylpyridine thiosemicarbazone),H2L2(bis(2-acetyl-pyridine) thiocarbonohydrazone) and H2L3(bis(imidazole-2-carboxaldehyde) thiocarbonohydrazone) was synthesized.H2L2 and H2L3 were character...A series of ligands,HL1(2-acetylpyridine thiosemicarbazone),H2L2(bis(2-acetyl-pyridine) thiocarbonohydrazone) and H2L3(bis(imidazole-2-carboxaldehyde) thiocarbonohydrazone) was synthesized.H2L2 and H2L3 were characterized by elemental analysis,IR spectra and single-crystal X-ray diffraction studies.Hydrogen bonds link different components to stabilize the crystal structure in the two ligands.To comprehend the structure-activity relationship well,the three ligands are all tested against human K562 leucocythemia cell line with IC50 analysis.Different substituent groups on the ligands show different levels of antitumor activity.By comparison with the other species studied,H2L2 with thiocarbonohydrazone along with 2-acetylpyridine is the most active compound with IC50 = 2.48 μM.展开更多
A new pseudo Keggin-type bicapped compound(Et3N)0.5(en)2[SiMo12O40(VO)2]·4H2O(Et3N=triethylamine,en=ethylenediamine) has been hydrothermally synthesized and characterized by IR,elemental analysis,TG and X-ray cry...A new pseudo Keggin-type bicapped compound(Et3N)0.5(en)2[SiMo12O40(VO)2]·4H2O(Et3N=triethylamine,en=ethylenediamine) has been hydrothermally synthesized and characterized by IR,elemental analysis,TG and X-ray crystallography.The title compound crystallizes in monoclinic,space group P21/n with a=17.576(2),b=13.535(1),c=21.587(2),β=103.790(10)°,V=4987.3(8)3,Z=4,Dc=2.925 Mg/m3,Mr=2196.12,F(000)=4148,μ=3.400 mm-1,R=0.0379 and wR=0.1219.The most remarkable structural feature of the compound is that the clusters represent bicapped pseudo-Keggin structure and are linked one by one through V-O-V bonds forming an infinite 1D chain.Furthermore,such chains are interconnected in a cross-like arrangement through multiform hydrogen bonds to yield a 3D supramolecular network.展开更多
The reaction of α-H3[PW12O40] with Y(NO3)3 in the presence of DMF or DMSO leads to two complexes with the formulae {Y(DMSO)7}·PW12O40(1) and {[Y(DMF)7]2PW12O40}·PW12O40(2). The crystal structures indicate t...The reaction of α-H3[PW12O40] with Y(NO3)3 in the presence of DMF or DMSO leads to two complexes with the formulae {Y(DMSO)7}·PW12O40(1) and {[Y(DMF)7]2PW12O40}·PW12O40(2). The crystal structures indicate that complex 1 consists of discrete [YLn]3+ cations and α-Keggin heteropolyanions [PW12O40]3-, whereas, in complex 2, donor-acceptor interaction results in a cation-anion-cation triplet. In addition, the electrochemical behavior of the two complexes indicates the usual successive reduction processes of the W atoms in the anions.展开更多
An organic-inorganic mercury coordination compound [Hg(DMSO)2(H2O)]2 [GeW12O40]· DMSO·H2O (DMSO =dimethyl sulfoxide) has been synthesized and characterized by IR, UV spectra, elemental analysis, TG-DTA and X...An organic-inorganic mercury coordination compound [Hg(DMSO)2(H2O)]2 [GeW12O40]· DMSO·H2O (DMSO =dimethyl sulfoxide) has been synthesized and characterized by IR, UV spectra, elemental analysis, TG-DTA and X-ray single-crystal diffraction. Structural analysis revealed that in the title compound, the mercury is three-coordinated to show the distorted trigonal cone geometry, and depending on the electrostatic interaction to connect the polyanion [α-GeW12O40]4-. TG-DTA study manifests the decomposition temperature of the polyanion framework in the title compound is 513.5℃, which is much higher than that of the anion framework. It means that the formation of the organic-inorganic mercury coordination compound made the polyanion [α-GeW12O40]4- to be more stable.展开更多
A new Ni(II) complex, [Ni(ftsc)2NO3]NO3 (Hftsc=furan-2-carbaldehyde thiosemicarba-zone), has been synthesized and characterized by IR, UV spectra and single-crystal X-ray diffraction analysis. It crystallizes in a mon...A new Ni(II) complex, [Ni(ftsc)2NO3]NO3 (Hftsc=furan-2-carbaldehyde thiosemicarba-zone), has been synthesized and characterized by IR, UV spectra and single-crystal X-ray diffraction analysis. It crystallizes in a monoclinic system, space group P21/n, with a=10.5203(13), b=9.2094(11), c=20.829(3), β=91.518(2)°, V=2 017.3(5)3, Z=4, F(000)=1064, Dc=1.716 g/cm3, and wR= 0.0800. The complex contains a six-coordinated nickel(II) center which is bound to two imine nitrogen atoms and two thiolato sulfur atoms of two ligands as well as two oxygen atoms from a nitrate anion to assume a distorted octahedral coordination geometry. In addition, intermolecular N-H···O and C-H···O hydrogen bonds between adjacent molecules link the molecules together to form a three-dimensional structure.展开更多
A transition metal substituted polyoxotungstate, [Cu(en)2(H2O)]2{PW11.5Cu0.5O40 [Cu(en)2]}·2H2O 1 based on Keggin frameworks, has been hydrothermally synthesized and characterized by IR, TGA and single-crystal X-...A transition metal substituted polyoxotungstate, [Cu(en)2(H2O)]2{PW11.5Cu0.5O40 [Cu(en)2]}·2H2O 1 based on Keggin frameworks, has been hydrothermally synthesized and characterized by IR, TGA and single-crystal X-ray structural analysis. It is interesting to find that the structure unit contains two different valence cations, namely, one [Cu(1)(en)2(H2O)]+ and one [Cu(2)(en)2(H2O)]2+. Data for the crystal: orthorhombic system, space group Pbca, a=21.585(2), b=20.695(2), c=26.137(3), V=11675(2)3 , Z=8, Mr=3428.23, Dc=3.901 g/cm3, F(000)=12156, μ(MoKα)=23.932 mm-1, the final R=0.0468 and wR=0.0969 for 6927 observed reflections (I > 2σ(I)).展开更多
A new one-dimensional polymeric complex [Cd(SCN)2(H2O)]L (L = N,N?-bis(furan- 2-ylmethylene)hydrazine) has been synthesized and characterized by IR, UV spectra, TG-DTA technique and single-crystal X-ray diffraction an...A new one-dimensional polymeric complex [Cd(SCN)2(H2O)]L (L = N,N?-bis(furan- 2-ylmethylene)hydrazine) has been synthesized and characterized by IR, UV spectra, TG-DTA technique and single-crystal X-ray diffraction analysis. It crystallizes in triclinic, pace group P1 with a = 5.9268(8), b = 10.8678(15), c = 13.3671(19) , α = 109.295(2), β = 95.092(2), γ = 97.8580(10)°, V = 796.70(19) 3, Z = 2, C12H10CdN4O3S2, Mr = 434.76, μ = 1.648 mm–1, Dc = 1.812 g/cm3, F(000) = 428, R = 0.0308 and wR = 0.0769. The crystal structure reveals that the structure of [Cd(SCN)2(H2O)]n features di-μ-1,3-thiocyante bridges and 1D chains. The octahedrally coordinated Cd atom is surrounded by one oxygen atom from water molecule, three S atoms and two Natoms from five di-μ-1,3 thiocyanato bridges. The Cd atoms are connected by two di-μ-1,3 thiocyanato bridges with the Cd(1)…Cd(1A) separation of 4.239(1) and Cd(1)…Cd(1B) of 5.852(1). In addition, the one-dimensional straight chain structure is further connected by multiform intermolecular N-H…O hydrogen bonds and π…π interactions to form a three-dimensional supramolecular structure.展开更多
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[HV16O38(Cl)]·4.5H...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[HV16O38(Cl)]·4.5H2O crystallizes in monoclinic,space group C2/c,with a=17.016(4),b=18.858(4),c=18.872(4),β=93.667(4)o,V=6043(2)3,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(Cl)]4-cage,two [Mn(en)3]22+ 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.展开更多
A new complex constructed from a unit with two As3O6 rings capping Anderson-type moieties,[Ni(en)2(H2O)2]2[(NiO6)Mo6O18(As3O3)2]·2H2O(1,en = ethylenediamine),has been hydrothermally synthesized and characterized ...A new complex constructed from a unit with two As3O6 rings capping Anderson-type moieties,[Ni(en)2(H2O)2]2[(NiO6)Mo6O18(As3O3)2]·2H2O(1,en = ethylenediamine),has been hydrothermally synthesized and characterized by IR,single-crystal X-ray diffraction and thermogra-vimetric analysis.The compound crystallizes in triclinic,space group P1 with a = 9.1230(16),b = 11.8078(9),c = 12.2111(9) ,α = 114.5210(10),β = 98.0350(10),γ = 100.0320(10)o,Mr = 2029.80,C8H44As6Mo6N8Ni3O36,V = 1145.0(2) 3,Dc = 2.944 g/cm3,Z = 1,GOF = 0.997,μ = 7.203 mm-1,F(000) = 970,R = 0.0352 and wR = 0.1019.Compound 1 consists of an Anderson-type capped by a two-ring(As3O6) unit [(NiO6)Mo6O18(As3O3)2]4-,two six-coordinate [Ni(en)2(H2O)2]2+ cations and two water molecules.展开更多
Two novel organic-inorganic heteropolyoxometalate compounds [{Cu(1,10- phen)OH}_2]_2[V_2W_4O_19]·6H_2O (1) and [Co(1,10-phen)_3]_2[V_2W_4O_(19)]·5H_2O (2) (1,10-phen = 1,10- phenanthroline) were hydrothermal...Two novel organic-inorganic heteropolyoxometalate compounds [{Cu(1,10- phen)OH}_2]_2[V_2W_4O_19]·6H_2O (1) and [Co(1,10-phen)_3]_2[V_2W_4O_(19)]·5H_2O (2) (1,10-phen = 1,10- phenanthroline) were hydrothermally synthesized and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. Compound 1 contains a di-V substituted classical Lindqvist-type polyanion [V_2W_4O_(19)]^(4-), two dinuclear copper cations [{Cu(1,10-phen)OH}_2]^(2+) and six water molecules of crystallization. Two dinuclear copper cations [{Cu(1,10-phen)OH}_2]^(2+) consist of four transition metal coordination cations {Cu(1,10-phen)}^(2+), bridged by four hydroxyl groups. Meanwhile, both two dinuclear cations are grafted on the Lindqvist polyanion [V_2W_4O_(19)]^(4-) through two terminal oxygen (O(9)) and two μ_2-oxygen (O(6)) atoms. Such an unusual linking fashion is unique in the polyoxometalate chemistry. The basic framework of 2 is similar to that of 1 and contains one Lindqvist-type polyanion [V_2W_4O_(19)]^(4-), two six-coordinated cobalt cations [Co(1,10-phen)_3]^(2+) and five free water molecules.展开更多
基金This work was financially supported by the Natural Science Foundation of Henan Province (No. 0611011900)
文摘The title complex Mn(HL)4(NCS)2(CH3CH2OH)2 has been achieved via self- assembly by incorporating manganese(II) into pyridine-3-carbaldehyde thiosemicarbazonate ligand, and characterized by elemental analysis and single-crystal X-ray diffraction study. The crystal crystallizes in triclinic, space group P1, with a = 8.896(2), b = 9.530(2), c = 14.520(4) , α = 87.035(4), β = 88.112(4), γ = 69.434(4)o, V = 1150.9(5) 3, Z = 1, Mr = 984.17, Dc = 1.420 g/cm3, μ(MoKα) = 0.612 mm-1, F(000) = 511, the final R = 0.0574 and wR = 0.1547 for 2855 observed reflections with I > 2σ(I). The complex contains one six-coordinated manganese ion connected by two thiosemicarbazide ligands, in which the thiosemicarbazone ligand acts as a monodentate ligand and coordinates to the center metal atoms via the pyridyl nitrogen atoms, two ethanol molecules and two isothiocyanic anions to give rise to a mononuclear structure. The coordination of a po- tentially tridentate thiosemicarbazone in manganese(II) complex without using its sulfur and imine nitrogen sites is unusual. Hydrogen bonds existing in the complex link the different components to stabilize the crystal structure.
基金This work was supported by the National Natural Science Foundation of China, Specialized Research Fund for the Doctoral Program of Higher Education, Henan Innovation Project for University Prominent Research Talents, Program for New Century Excellent Talent in University of Henan Province, the Foundation of Educational Department of Henan Province and Natural Science Foundation of Henan Province
文摘A cobalt paradodecatungstate [Co(H2O)5]2[Co(H2O)4]3[H2W12O42]·11H2O has been successfully synthesized and structurally characterized by X-ray crystallography. Structure analysis indicates that the title compound is of monoclinic, space group P21/n, with a = 13.449(3), b = 19.585(4), c = 13.990(3) , β = 113.79(3)°, V = 3371.8(12) ?3, Z = 2, R = 0.0519 and wR = 0.1242. The title compound exhibits a novel 3D extended network structure constructed by interconnecting the paradodecatungstate polyanion [H2W12O42]10- clusters and cobaltII coordination ions.
基金supported by the National Natural Science Foundation of China (20771034,20773035)the Specialized Research Fund for the Doctoral Program of Higher Education (20040475001)+1 种基金Program for New Century Excellent Talents in University of Henan Province (2005KYCX011)the Natural Science Foundation of Henan Province (0611011900)
文摘A 1D zigzag polyoxometalate [(CH3)4N]1.50H3.50[Gd(GeW11O39)(H2O)2]·2.5H2O (1) was synthesized by reaction of the monovacant polyanion [α-GeW11O39]8-with Gd3+ ions in aqueous solution and characterized by IR, UV spectra, ICP, and X-ray crystallography. X-ray single-crystal structural analysis indicated that the title compound crystallized in a monoclinic lattice, C2/c space group with a=2.8201(5), b=2.2885(3), c=2.4033(4) nm, β=123.875 (2), V=12.878(4) nm3, Z=8, R1=0.0623, wR2=0.1287. The solid-state structure of the title compound displayed an infinite one-dimensional arrangement built up of [α-GeW11O39]8-polyanions connected by GdIII cations.
文摘A Schiff base ligand(H2CSF,C13H11NO4,1) derived from 3-carboxylsalicylaldehyde and furfurylamine,and its trinuclear complex [Ni3(CSF)2(CH3COO)2(DMF)2(H2O)2](2) were synthesized.Compound 1 was characterized by elemental analysis,1H NMR,IR,MS and X-ray diffraction analysis.The crystal of 1 belongs to the monoclinic system,space group P21/c with a = 8.472(2),b = 19.743(5),c = 7.2300(18) ,β = 110.278(4)°,V = 1134.4(5) 3,Z = 4,Mr = 245.23,Dc = 1.436 g·cm-3,μ = 0.108 mm-1,F(000) = 512,λ = 0.71073 ,the final R = 0.0440 and wR = 0.1199 for 1426 observed reflections(I > 2σ(I)).In the crystal of 1,there exist intramolecular hydrogen bonds and weak intermolecular C-H···O hydrogen bonds.Compound 2 was characterized by elemental analysis,IR,TG and X-ray diffraction analysis.The crystal of 2 is of triclinic system,space group P1 with a = 10.1237(17),b = 10.4086(18),c = 10.4884(18) ,α = 82.528(2),β = 67.339(2),γ = 83.010(2)°,V = 1008.1(3) 3,Z = 1,Mr = 962.87,Dc = 1.586 g·cm-3,μ = 1.463 mm-1,F(000) = 498,λ = 0.71073 ,the final R = 0.0517 and wR = 0.0805 for 2065 observed reflections(I > 2σ(I)).The geometry of the trinuclear molecule is centrosymmetric,in which every Ni(Ⅱ) ion is coordinated in a slightly distorted octahedron.The three Ni(Ⅱ) ions are arranged in a straight line.The two CSF2-ions act as NOO tridentate ligands with the phenolate and carboxylate oxygen as bridging atoms.The coordination atoms of CSF2-anions and water molecules are coordinated on the equatorial plane,while the two bridging acetate ions and two DMF are trans-coordinated on the apical sites.
基金This work was supported by the Program for New Century Excellent Talents in University of Henan Province (2005HANCET-02)Natural Science Foundation of Henan Province (0611020200)
文摘A new hybrid polyoxometalate-based complex, [CuI(phen)2]4(SiW12O40) (phen = 1,10-phenanthroline), has been synthesized by hydrothermal method and characterized with the aid of elemental analysis, IR, UV spectra and thermal analysis studies. The result of X-ray crystallo- graphy analysis exhibits that the title compound crystallizes in the orthorhombic space group P212121, and the formula is C96H64N16Cu4SiW12O40. Crystal data: a = 18.3574(14), b = 21.1952(16), c = 27.992(2) , Mr = 4570.08, V = 10891.4(14) 3, Z = 4, Dc = 2.787 g/cm3, μ = 13.478 mm–1, R = 0.0364, wR = 0.0638 (I > 2σ(I)) and F(000) = 8360. The complex consists of one α-Keggin anion [SiW12O40]4– and four discrete [CuⅠ(phen)2]+ cations. The valence sum calculations for the Cu atoms suggest that all four Cu atoms are in the +1 oxidation state.
基金This work was supported by the National Natural Science Foundation of China, Specialized Research Fund for the Doctoral Program of Higher Education, Henan Innovation Project for University Prominent Research Talents, Program for New Century Excellent Talents in Universities of Henan Province, the Foundation of Educational Department of Henan Province and Natural Science Foundation of Henan Province
文摘A novel polyoxometalate-based composite compound [Ni(phen)2][Hphen](AsW12O40) (phen = 1,10-phenanthroline) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TGA, ESR spectroscopy and single-crystal X-ray diffraction. Each structure unit of 1 consists of one polyoxoanion AsW12O403-, one free phenanthroline molecule and one coordination cation [Ni(phen)2]2+. The title compound crystallizes in the orthorhombic system, space group P212121, with a = 12.2383(7), b = 21.0884(11), c = 22.3237(12) , V = 5761.4(5) 3, Mr = 3520.44, Z = 4, Dc = 4.059 g/cm3, F(000) = 6204, μ(MoKα) = 24.844 mm-1, GOF = 1.022, the final R = 0.0376 and wR = 0.0742 (I > 2σ(I)) for 865 parameters and 9637 observed reflections with I > 2σ(I).
基金The project was supported by Henan Innovation Project for University Prominent Research Talentsthe Natural Science Foundation of Henan Province (No.0524480020)Natural Science Foundation of Henan University (No. XK04YBRW057)
文摘The synthesis, X-ray crystal structure, thermal properties and electrochemistry of the new complex formulated as {Er(DMSO)7}PW12O40 are reported. The single-crystal X-ray analysis reveals that the crystal crystallizes in the monoclinic system, space group P21/c with a = 11.767(2), b = 14.909(3), c = 34.905(7) , β = 98.97(3)°, Mr = 3591.33, V = 6049(2) 3, Dc = 3.944 g/cm3, Z = 4, GOOF = 1.098, F(000) = 6340, R = 0.0490 and wR = 0.1202. Crystal structure analysis indicates that the Er(Ⅲ) is seven-coordinate with a distorted pentagonal bipyramid and combines to the anion [PW12O40]3- via static electric force.
基金the Natural Science Foundation of Henan Province (No. 0611011900) the Foundation of Educational Department of Henan Province (No. 2007150012)
文摘The title complex Co(L)2Cl·4H2O I has been achieved via self-assembly by incorporating cobalt into 2-benzoylpyridine thiosemicarbazonate ligand, and characterized by elemental analysis, infrared spectra, mass spectra and single-crystal X-ray diffraction study. The crystal crystallizes in monoclinic, space group P21/n, with a=10.227(3), b=17.363(4), c=17.459(4), β=100.408(4)o, V=3049.2(13)3, Z=4, Mr=677.08, Dc=1.475 g/cm3, μ(MoKα)=0.834 mm-1, F(000)=1400, the final R=0.0747 and wR=0.0896 for 1663 observed reflections with I > 2σ(I). The complex contains one six-coordinated cobalt ion connected by two thiosemicarbazone ligands which act as a tridentate ligand to coordinate with the center metal atoms via two pyridyl nitrogen atoms, two imine nitrogen atoms and two sulfur atoms giving rise to a mononuclear structure. Hydrogen bonds existing in the complex link the different com-ponents to stabilize the crystal structure. The antitumor activity of the title complex was tested against A549 lung cancer cell line. Complex I exhibits antitumor activity.
基金Supported by the Program for New Century Excellent Talents in University of Henan Province,China(No.005HANCET-02)the Natural Science Foundation of Henan Province,China(No.0611020200)
文摘A new compound based on polyoxovanadate [{Ni(en)2}2Sb8V14O42]·5.5H2O(en=ethylenediamine)(1) was synthesised hydrothermally as black rhombus crystals.Compound 1 crystallized in the monoclinic system with space group P21/n,Z=4,a=1.46953(9) nm,b=1.28623(8) nm,c=1.76008(11) nm,β=105.7230(10)°.In the asymmetric unit,cluster {Sb8V14O42} can be considered as an Sb derivative of the {V18O42} unit.Each {Sb8V14O42} cluster as a building block interconnected to four other neighboring units by {Ni(en)2} bridging groups which are linked through the terminal oxygen atoms of the polyoxoanions,forming a two dimensional network.
基金the Natural Science Foundation of Henan Province (0611011900)
文摘A novel double 1:11 series arsenotungstate, [CuI(phen)2]5H6[Sm(AsW11O39)2]·6H2O (phen=1,10-phenanthroline) was synthesized by the hydrothermal method and characterized by elemental analysis, IR spectra, and single-crystal X-ray diffraction. The title compound was monoclinic, space group P21/c, a=3.75710(2) nm, b=1.39776(8) nm, c=3.33735(18) nm, β=96.967(10)°, V=17.3969(17) nm3, Z=4. Single crystal X-ray structural analyses revealed that the dimeric polyanion, [SmAs2W22O78]1–, consisted of one central Sm3+ ion and two tetradentate heteropoly ligands [AsW11O39]7–. The Sm3+ ion and two tetradentate defective [AsW11O39]7– anions were joined together by the sharing of four oxygen atoms from each heteropoly ligand. The bond valence sum (BVS) calculations of the title compound suggested that all four Cu atoms were in the +1 oxidation sate.
基金supported by the Natural Science Foundation of Henan Province,the Natural Science Foundation of Educational Department of Henan Province (2010B150003)China Postdoctoral Science Foundation (20090460847)
文摘A series of ligands,HL1(2-acetylpyridine thiosemicarbazone),H2L2(bis(2-acetyl-pyridine) thiocarbonohydrazone) and H2L3(bis(imidazole-2-carboxaldehyde) thiocarbonohydrazone) was synthesized.H2L2 and H2L3 were characterized by elemental analysis,IR spectra and single-crystal X-ray diffraction studies.Hydrogen bonds link different components to stabilize the crystal structure in the two ligands.To comprehend the structure-activity relationship well,the three ligands are all tested against human K562 leucocythemia cell line with IC50 analysis.Different substituent groups on the ligands show different levels of antitumor activity.By comparison with the other species studied,H2L2 with thiocarbonohydrazone along with 2-acetylpyridine is the most active compound with IC50 = 2.48 μM.
基金supported by the National Natural Science Foundation of China (No 20701012)the Key Project of Chinese Ministry of Education (No 207068)+1 种基金the Foundation of Henan Educational Committee of China (No 2007150003 and 2008B150002)the Foundation for University Youth Key Teacher of Henan Province
文摘A new pseudo Keggin-type bicapped compound(Et3N)0.5(en)2[SiMo12O40(VO)2]·4H2O(Et3N=triethylamine,en=ethylenediamine) has been hydrothermally synthesized and characterized by IR,elemental analysis,TG and X-ray crystallography.The title compound crystallizes in monoclinic,space group P21/n with a=17.576(2),b=13.535(1),c=21.587(2),β=103.790(10)°,V=4987.3(8)3,Z=4,Dc=2.925 Mg/m3,Mr=2196.12,F(000)=4148,μ=3.400 mm-1,R=0.0379 and wR=0.1219.The most remarkable structural feature of the compound is that the clusters represent bicapped pseudo-Keggin structure and are linked one by one through V-O-V bonds forming an infinite 1D chain.Furthermore,such chains are interconnected in a cross-like arrangement through multiform hydrogen bonds to yield a 3D supramolecular network.
基金the Specialized Research Fund for the Doctoral Program of Higher Education(No.20040475001)Henan Inno-vation Project for University Prominent Research Talents, and the Natural Science Foundation of Henan Province, China (No.0524480020)
文摘The reaction of α-H3[PW12O40] with Y(NO3)3 in the presence of DMF or DMSO leads to two complexes with the formulae {Y(DMSO)7}·PW12O40(1) and {[Y(DMF)7]2PW12O40}·PW12O40(2). The crystal structures indicate that complex 1 consists of discrete [YLn]3+ cations and α-Keggin heteropolyanions [PW12O40]3-, whereas, in complex 2, donor-acceptor interaction results in a cation-anion-cation triplet. In addition, the electrochemical behavior of the two complexes indicates the usual successive reduction processes of the W atoms in the anions.
文摘An organic-inorganic mercury coordination compound [Hg(DMSO)2(H2O)]2 [GeW12O40]· DMSO·H2O (DMSO =dimethyl sulfoxide) has been synthesized and characterized by IR, UV spectra, elemental analysis, TG-DTA and X-ray single-crystal diffraction. Structural analysis revealed that in the title compound, the mercury is three-coordinated to show the distorted trigonal cone geometry, and depending on the electrostatic interaction to connect the polyanion [α-GeW12O40]4-. TG-DTA study manifests the decomposition temperature of the polyanion framework in the title compound is 513.5℃, which is much higher than that of the anion framework. It means that the formation of the organic-inorganic mercury coordination compound made the polyanion [α-GeW12O40]4- to be more stable.
基金the Ministry of Education of China (No. 207068)the Natural Science Foundation of Henan Province (No. 0611023000)the Education Department of Henan Province (No. 2007150003, 2007150011)
文摘A new Ni(II) complex, [Ni(ftsc)2NO3]NO3 (Hftsc=furan-2-carbaldehyde thiosemicarba-zone), has been synthesized and characterized by IR, UV spectra and single-crystal X-ray diffraction analysis. It crystallizes in a monoclinic system, space group P21/n, with a=10.5203(13), b=9.2094(11), c=20.829(3), β=91.518(2)°, V=2 017.3(5)3, Z=4, F(000)=1064, Dc=1.716 g/cm3, and wR= 0.0800. The complex contains a six-coordinated nickel(II) center which is bound to two imine nitrogen atoms and two thiolato sulfur atoms of two ligands as well as two oxygen atoms from a nitrate anion to assume a distorted octahedral coordination geometry. In addition, intermolecular N-H···O and C-H···O hydrogen bonds between adjacent molecules link the molecules together to form a three-dimensional structure.
基金the Program for New Century Excellent Talent in University of Henan ProvinceNatural Science Foundation of Henan Province
文摘A transition metal substituted polyoxotungstate, [Cu(en)2(H2O)]2{PW11.5Cu0.5O40 [Cu(en)2]}·2H2O 1 based on Keggin frameworks, has been hydrothermally synthesized and characterized by IR, TGA and single-crystal X-ray structural analysis. It is interesting to find that the structure unit contains two different valence cations, namely, one [Cu(1)(en)2(H2O)]+ and one [Cu(2)(en)2(H2O)]2+. Data for the crystal: orthorhombic system, space group Pbca, a=21.585(2), b=20.695(2), c=26.137(3), V=11675(2)3 , Z=8, Mr=3428.23, Dc=3.901 g/cm3, F(000)=12156, μ(MoKα)=23.932 mm-1, the final R=0.0468 and wR=0.0969 for 6927 observed reflections (I > 2σ(I)).
基金supported by the Natural Science Foundation of the Ministry of Education of China (No.207068)Henan Province (No.0611023000)the Education Department of Henan Province (No.2007150003,2007150011)
文摘A new one-dimensional polymeric complex [Cd(SCN)2(H2O)]L (L = N,N?-bis(furan- 2-ylmethylene)hydrazine) has been synthesized and characterized by IR, UV spectra, TG-DTA technique and single-crystal X-ray diffraction analysis. It crystallizes in triclinic, pace group P1 with a = 5.9268(8), b = 10.8678(15), c = 13.3671(19) , α = 109.295(2), β = 95.092(2), γ = 97.8580(10)°, V = 796.70(19) 3, Z = 2, C12H10CdN4O3S2, Mr = 434.76, μ = 1.648 mm–1, Dc = 1.812 g/cm3, F(000) = 428, R = 0.0308 and wR = 0.0769. The crystal structure reveals that the structure of [Cd(SCN)2(H2O)]n features di-μ-1,3-thiocyante bridges and 1D chains. The octahedrally coordinated Cd atom is surrounded by one oxygen atom from water molecule, three S atoms and two Natoms from five di-μ-1,3 thiocyanato bridges. The Cd atoms are connected by two di-μ-1,3 thiocyanato bridges with the Cd(1)…Cd(1A) separation of 4.239(1) and Cd(1)…Cd(1B) of 5.852(1). In addition, the one-dimensional straight chain structure is further connected by multiform intermolecular N-H…O hydrogen bonds and π…π interactions to form a three-dimensional supramolecular structure.
基金supported by the National Natural Science Foundation of China (No. 20701012)the Foundation of the Education Ministry of China (No. 207068)the Education Department of Henan Province (No. 2007150003, 2007150011)
文摘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[HV16O38(Cl)]·4.5H2O crystallizes in monoclinic,space group C2/c,with a=17.016(4),b=18.858(4),c=18.872(4),β=93.667(4)o,V=6043(2)3,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(Cl)]4-cage,two [Mn(en)3]22+ 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.
基金Supported by the National Natural Science Foundation of China (20771034)Natural Science Foundation of Henan Province (2009A150003)
文摘A new complex constructed from a unit with two As3O6 rings capping Anderson-type moieties,[Ni(en)2(H2O)2]2[(NiO6)Mo6O18(As3O3)2]·2H2O(1,en = ethylenediamine),has been hydrothermally synthesized and characterized by IR,single-crystal X-ray diffraction and thermogra-vimetric analysis.The compound crystallizes in triclinic,space group P1 with a = 9.1230(16),b = 11.8078(9),c = 12.2111(9) ,α = 114.5210(10),β = 98.0350(10),γ = 100.0320(10)o,Mr = 2029.80,C8H44As6Mo6N8Ni3O36,V = 1145.0(2) 3,Dc = 2.944 g/cm3,Z = 1,GOF = 0.997,μ = 7.203 mm-1,F(000) = 970,R = 0.0352 and wR = 0.1019.Compound 1 consists of an Anderson-type capped by a two-ring(As3O6) unit [(NiO6)Mo6O18(As3O3)2]4-,two six-coordinate [Ni(en)2(H2O)2]2+ cations and two water molecules.
基金supported by the Foundation of Education Department of Henan Province
文摘Two novel organic-inorganic heteropolyoxometalate compounds [{Cu(1,10- phen)OH}_2]_2[V_2W_4O_19]·6H_2O (1) and [Co(1,10-phen)_3]_2[V_2W_4O_(19)]·5H_2O (2) (1,10-phen = 1,10- phenanthroline) were hydrothermally synthesized and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. Compound 1 contains a di-V substituted classical Lindqvist-type polyanion [V_2W_4O_(19)]^(4-), two dinuclear copper cations [{Cu(1,10-phen)OH}_2]^(2+) and six water molecules of crystallization. Two dinuclear copper cations [{Cu(1,10-phen)OH}_2]^(2+) consist of four transition metal coordination cations {Cu(1,10-phen)}^(2+), bridged by four hydroxyl groups. Meanwhile, both two dinuclear cations are grafted on the Lindqvist polyanion [V_2W_4O_(19)]^(4-) through two terminal oxygen (O(9)) and two μ_2-oxygen (O(6)) atoms. Such an unusual linking fashion is unique in the polyoxometalate chemistry. The basic framework of 2 is similar to that of 1 and contains one Lindqvist-type polyanion [V_2W_4O_(19)]^(4-), two six-coordinated cobalt cations [Co(1,10-phen)_3]^(2+) and five free water molecules.
