A novel composite, [C16H36N][Cu（2,2-bipy）3][PW12O40]·CH3CN·H2O based on Keggin-type phosphotungstate, has been synthesized in acetonitrile at moderate temperature and then characterized by IR and single-crystal X-ray structural analysis. The crystal is of monoclinic system, space group P21/n with a = 20.489（4）, b = 17.249（3）, c = 23.723（4）A, β = 95.114（2）^o, V = 8350（3）A3, Mr = 3710.79, Z = 4, Dc = 2.952 g/cm^3, F（000） = 6676, μ = 16.808 mm^-1, the final R = 0.0551 and wR = 0.1269 for 9460 observed reflections with I 〉 20（I）. Interestingly, it is found that the structure unit contains two different cations of [C16H36N]^＋ and [Cu（2,2-bipy）3]^2＋.
The title complex Mn（HL）4（NCS）2（CH3CH2OH）2 has been achieved via selfassembly 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 PI^-, with a = 8.896（2）, b = 9.530（2）, c = 14.520（4）°A, α = 87.035（4）, β= 88.112（4）, γ= 69.434（4）°, V= 1150.9（5）°A^3, Z = 1, Mr = 984.17, Dc = 1.420 g/cm^3,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 potentially 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.
LI Ming-Xue ZHOU Jing WANG Jing-Ping WANG Zi-Liang
A novel transition metal ion bridging bis（diphosphopentamolybdates） has been synthesized and characterized by elemental analysis,IR spectrum,UV spectrum and single-crystal X-ray diffraction.The single-crystal structure analysis shows that the compound consists of seven charge-compensating 2,2＇-biimidazole cations （BIIM=2,2＇-biimidazole） and one dumbbell-like [Mn（H2O）4（P2Mo5O23）2]10-heteropolyanion which is constructed by two [P2Mo5O23]6-clusters bridged through one [Mn（H2O）4]2＋ cation.
The title complex [Co（L）2]Cl·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 P2 1/n, with a = 10.227（3）, b = 17.363（4）, c = 17.459（4） A, β= 100.408（4）°, V= 3049.2（13） A^3, Z = 4, Mr = 677.08, Dc = 1.475 g/cm^3, 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 components to stabilize the crystal structure. The antiturnor activity of the title complex was tested against A549 lung cancer cell line. Complex ! exhibits antitumor activity.
AID zigzag polyoxometalate [（CH3）4N]1.50H3.50[Gd（GeW11O39）（H2O）2]·2.5H2O （1） was synthesized by reaction of the monova- cant polyanion [α-GeW11O39]^8- with Gd^3＋ 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 α= 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 Gd^Ⅲ cations.
Two transition metal dinuclear complexes of [Mn2（OOCC6H4SSC6H4COO）- （Phen）2（H20）]n 1 and [CuE（OOCC6H4S）2（Phen）2] 2 were hydrothermally synthesized by the reaction of equivalent metal dichloride with 2,2＇-dithiobis（benzoic acid） （HE-DTBB）. Structure analysis indicates that each Mn2＋ ion in I is coordinated by one chelate phen ligand, one bridging water molecule and three DTBB ligands forming Mn2＋ dinuclear units which are further linked into one-dimensional chain by DTBB ligand. Under similar reaction conditions, the 2,2＇-dithio- his（benzoic acid） ligand undergoes thiol reduction to form 2-mercaptobenzoic （H-2-MBA） in 2 where two Cu2＋ ions are coordinated by phen and MBA ligands only constructing a dinuclear unit.
A novel double 1：11 series arsenotungstate, [Cu^I（phen）2]5H6[Sm（AsW11O39）2]·6H2O （phen=1, 10-phenanthroline） was synthesized by the hydrothermal method and characterized by elemental analysis, 1R spectra, and single-crystal X-ray diffraction. The title compound was monoclinic, space group P2 1/c, a=3.75710（2） nm, b=1.39776（8） nm, c=-3.33735（18） nm, β=96.967（10）°, V=17.3969（17） nm^3, Z=4. Single crystal X-ray structural analyses revealed that the dimeric polyanion, [SmAs2W22O78]^1-, consisted of one central Sm^3＋ ion and two tetradentate heteropoly ligands [ASW11O39]^7-. The Sm^3＋ 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.
