Hydrothermal synthesis, structure characterization of a new mixed Mo/V metal-oxygen cluster compound: [Co(phen)(3)](2)[HPMo4V (Mo4V6IV)-V-VI M2O44]center dot 4H(2)O, (M=0.78Mo(V)+0.22V(IV))

A new polyoxometalate [Co(phen)(3)](2)[HPMo4V Mo-4(VI) V-6(IV) M2O44]center dot 4H(2)O (M = 0.78Mo(V)+ 0.22V(IV)) 1 was hydrothermally synthesized and characterized by IR, elemental analyses, X-ray photoelectron spectrum, ESR and single crystal X-ray diffraction. The title compound is in the triclinic space group P (1) over bar with a = 12.0953(7) angstrom, b = 14.0182(6) angstrom, c = 14.6468(7) angstrom, V=2402.55(18) angstrom(3), alpha = 105.134(2), beta = 91.841(3), gamma = 91.401(2), Z = 1, and R-1 (wR(2)) = 0.0617 (0.1701). The compound was prepared from tetra-capped pseudo-Kepin with phosphorus-centered polyoxoanions [PMo8V6M2O44](5-) , [Co(phen)(3)](2+) cations and linked through hydrogen bonds and pi-pi stacking interaction into three-dimensional supramolecular framework. Astudy of the magnetic properties of 1 demonstrates that it exhibits antiferromagnetic coupling interactions.

Structure characterization and physical properties of a complex with supramolecular architectures Co-2(2,6-DPC2Co(H2O)5 center dot 2H(2)O (DPC=2,6-pyridinedicarboxylate)

Reaction of 2,6-pyridinedicarboxylic with CoCl2 . 6H(2)O in aqueous solution give rise to a three-dimensional Complex CO2(2,6-DPC)(2)Co(H2O)(5).2H(2)O (DPC = 2,6-pyridinedicarboxylate) 1. It has been characterized by elemental analyses, infrared spectra (IR) spectrum, thermogravimetric (TG) analysis, EPR spectrum, and single crystal X-ray diffraction. The complex crystallizes in the P2(1)/c space group with a = 8.3906(3) Angstrom, b = 27.4005(8) Angstrom, c = 9.6192(4) A, alpha = 90.00degrees, beta = 98.327(2)degrees, gamma = 90.00degrees, V = 2188.20(14) Angstrom(3), Z = 4. There are two types of cobalt environments: Co(1) is coordinated by four oxygen atoms from four carboxyl groups and two nitrogen 2 atoms which are all from pdc(2). Co(2) is coordinated by six oxygen atoms, five from coordinated water molecules and one from a carboxyl of pdc(2) - of which the other oxygen atom is linked to the Co(1). The extensive intermolecular hydrogen bonds are formed in the crystal by means of the five coordinated water molecules.

A two-dimensional molybdenum (V) phosphate with covalently bonded transition metal coordination complexes: hydrothermal synthesis and structure characterization of Na-2[{Mn(phen)(2)(H2O)}{Mn(phen)(2)}(3){Mn (Mo12O24)-O-V (HPO4)(6)(PO4)(2)(OH)(6)}] center dot 4H(2)O (phen=1,10-phenanthroline)

An organic-inorganic hybrid molybdenum phosphate, Na-2[{Mn(phen)(2)(H2O)} {Mn(phen)(2)}(3){(MnMo12O24)-O-v (HPO4)(6)(PO4)(2) (OH)(6)}] . 4H(2)O (phen=1,10-phenanthroline), involving molybdenum present in V oxidation state and covalently bonded transition metal coordination complexes, has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. Deep brown-red crystals are formed in the triclinic system, space group P (1) over bar, a=16.581(l)Angstrom, b=18.354(1)Angstrom, c=24.485(2)Angstrom, alpha=80.589(l)degrees, beta=71.279(1)degrees, gamma=67.084(1)degrees, V=6493.8(8)Angstrom(3), Z=2, lambda(MoKalpha)=0.71073Angstrom (R(F)=0.0686 for 29,053 reflections). Data were collected on a Bruker Smart Apex CCD diffractometer at 293 K in the range of 1.76 < theta < 28.06degrees using omega-2theta scans technique. The structure of the title compound may be considered to be based on {Mo6O12(HPO4)(3)(PO4)(OH)(3)} units bonded together with {Mn(phen)(2)} subunits into a two-dimensional network. Two types of tunnels are observed in the solid of the title compound.

Synthesis, structure characterization and biological activity of a novel amino acid salt (HAla)(8)(H3O)(10)[PMo12O40](6) center dot 22H(2)O

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=1. 301 5(3) nm, V=7. 387 (3) nm(3), Z=6, R-1= 0. 037 3, wR(2)=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.

Novel macrocyclic aryl thioether ester oligomers: structure characterization and free-radical ring opening polymerization

Novel macrocyclic aryl thioether ester oligomers have been synthesized in high yield from phthaloyl dichloride and 4,4'-thiodiphenol under pseudo high dilution conditions. The cyclic nature was unambiguously confirmed by a combination of MALDI-TOF MS, gel permeation chromatography and NMR analyses. Single-crystal X-ray diffraction of cyclic ester dimer reveals no severe strain on the cyclic structure. The free-radical ring opening polymerization (ROP) of the macrocyclic oligomers was achieved to give high molecular weight polymers via a transthioetherification reaction. The molecular weight of the polymer resulting from ROP decreases as the conversion of cyclic oligomers increases after a polymerization period of 30 min.

Synthesis, structure characterization of the complexes of beta-alkoxycarbonylethyltin trichlorides with Schiff base ligands

Thirty - two title complexes (ROCOCHRCH2SnCl3)-C-1 . (2 - HOC6H4CH = NC6H4 - X) (R = Me, Et, n - Bu; R-1 = H, Me; X = H,4' - Cl, 3' - Pr, 3' - OH, 3', 4' - Cl-2, 4' - OMe) were synthesized and characterized by elemental analysis,UV - vis, IR, H-1 NMR. The crystal structure of n - BuOCOCH2CH2SnCl3 . (2 - HOC6H4CH - NC6H4OMe - 4') were determined by the X - ray diffraction analysis, The crystal belongs to monoclinic system, with a = 1.4661 (3)nm, b = 0.9307 (2)nm, c = 1.7888 (4)nm, beta = 94.04 (3)degrees, V = 2.4348nm(3), D-c = 1.581mg/m(3), Z = 4, F(000) = 1160, mu = 1.405mm(-1), R = 0.0354, R-w = 0,0486, space group: P2(1)/c. The complexes exist as a discrete monomer. The tin atom has a distorted octahedral geometry due to intramolecular coordination of the carbonyl oxygen and the phenolic oxygen of the Schiff base ligands, The coordination number of tin atom is 6.

Synthesis, structure characterization and transesterification of the complexes of beta-alkoxycarbonylethyltin trichlorides

Thirteen title complexes ROCOCH2CH2SnCl3 . L(R = C(1 similar to 5)alkyl;L = DBSO,HMPA) were synthesized and characterized by elemental analysis, IR,H-1 NMR. The crystal structure of n -PrOCOCH2CH2SnCl3 . DBSO was determined by the X-ray diffraction analysis. The crystal belongs to orthorhombic system,space group P2(1)2(1)2(1) with a = 1.062, b = 1.427, c = 1.635nm; Z = 4. The complex exists as a discrete molecule, and the tin atom attains a distorted octahedral geometry via the coordination of intramolecular carbonyl oxygen and the Lewis base donor atom. The transesterification of CH3OCOCH2CH2SnCl3 . L with alcohol was studied, and the intramolecular Lewis acid catalytic mechanism was suggested.

SYNTHESIS AND X-RAY CRYSTAL-STRUCTURE CHARACTERIZATION OF ZN2(HPO4)(3).H3NCH2CH2NH3

A novel framework material, Zn-2(HPO4)(3).H3NCH2CH2NH3, has been synthesised and its crystal structure determined by single crystal X-ray diffraction.

SYNTHESIS AND STRUCTURE CHARACTERIZATION OF LANTHANUM [2,2,2]CRYPTATES, [LACL[2,2,2](H2O)]CL-2-CENTER-DOT-H2O AND [LA(CF3SO3)[2,2,2]1(DMF)](CF3SO3)(2)

Two lanthanum(III) [2,2,2]cryptates, [LaCl[2,2,2](H2O)]Cl-2.H2O (1) and [La(CF3SO3)[2,2,2](DMF)] (CF3SO3)(2) (2) have been prepared by the reaction of LaCl3 and La(CF3SO3)(3) with [2,2,2]cryptand, respectively and their crystal structures have been determ

The structure analysis and characterization of N-100 by NMR

To improve the mechanics properties of polyurethane materials at a high or low temperature, a hydroxy compound N-100 of HDI was synthesized, The structure analysis and characterization were made by NMR (H-1, C-13, H-1-H-1 COSY, C-13-H-1 COSY), In addition, quantitative description of the network was made on the basis of some ideal assumptions, 1D and 2D NMR can differentiate four sorts of carbonyl groups and establish the connections of all carbon and hydrogen atoms of mixed structures that originated from five different substitutions, Besides, the alkene and isocyanate, urea, biuret and trimerized isocyanuric groups were also detected, Therefore, the structure of N-100 was suggested be a polyisocyanate with complicated network which contained nitrogen atom as cross-linkage, isocyanate and alkene as end groups, The consistence of calculated values with tested values of isocyanate content, mean function degree and mean molecular weight demonstrated the correct of structure characterization and the validity of network description.

Synthesis, Reactivity, and Characterization of Sodium and Rare-Earth Metal Complexes Bearing a Dianionic N-Aryloxo-Functionalized -Ketoiminate Ligand

The synthesis and reactivity of a series of sodium and rare-earth metal complexes stabilized by a dianionic N-aryloxo-functionalized beta-ketoiminate ligand were presented. The reaction of acetylacetone with 1 equiv of 2-amino-4-methylphenol in absolute ethanol gave the compound 4-(2-hydroxy-5-methylphenyl)imino-2-pentanone (LH2, 1) in high yield.

Protein structural characterization by scanning tunneling microscopy with electrochemistry

The structure characterization of proteins or enzymes by STM on electrochemically prepared HOPG surface studied in this laboratory is reviewed. The serial structures of Hb were observed. The differences between the denaturation and inactivation of HRP were investigated by in situ and ex situ STM. The structural variation of Hb in an organic solvent was imaged while protein denaturation was easily observed in a polar solvent.

STUDIES ON DEFECT STRUCTURE AND CATALYTIC PROPERTIES OF SN-MO OXIDES

The present work is devoted to the studies on relationship of structure and activity of Sn-Mo oxides by using XRD, ESR, IR, XPS, TEM and SEM. Eight samples with Mo/(Mo + Sn) rations: 0.0, 0.1, 0.2, 0.4, 0.6, 0.8, 0.9, 1.0 were prepared. On the basis of structure characterization, Sn-Mo oxides can be divided into three groups: Catalysts I with Mo/(Mo + So) less-than-or-equal-to 0.2, Catalysts II with 0.2 < Mo/(Mo + Sn) < 0.8, and catalysts III with Mo/(Mo + Sn) greater-than-or-equal-to 0.8. The solid solution of Mo5+ in tin oxide was formed and the cation vacancy was formed in catalysts I. The solid solution of Sn4+ in molybdenum oxide was formed in catalysts III. The lattice oxygen in catalysts III has higher mobility and reactivity than that in catalysts I. The catalysts III showed higher activity but lower selectivity than that of catalysts I.