A highly reduced polyoxoanion with phosphorus-centered alternate layers of Mo/V oxides, [(PMo2Mo6V4O40)-Mo-V-V-VI-O-IV((VO)-O-IV)(2)](9-)

An unusual polyoxometalate [H2N(C2H4)(2)NH2](4)(H3O)[(PMO2Mo6V4O40)-Mo-V-V-VI-O-IV((VO)-O-IV)(2)].H2O is hydrothermally synthesized and characterized by IR, UV-VIS, elemental analyses, X-ray photoelectron spectrum, ESR, TG and Single crystal X-ray diffraction. The title compound crystallizes in the orthorhombic space group Pbca with a = 15-227(5), b = 19.491(4), c = 18.737(3) Angstrom, V = 5123(2) Angstrom(3), Z = 4, and R-1 (wR(2)) = 0.0726(0.1416). The compound contains an unusual highly reduced pseudo-Keggin type polyoxoanion and exhibits an interesting phosphorus-centered alternate arrangement of layers of molybdenum and vanadium oxides.

Hydrothermal synthesis and crystal structure of an unusual compound: [Cu(en)(2)](4)[(SiMo8V4O40)-O-V((VO)-O-IV)(2)][MoO4](2)center dot 5H(2)O

A novel compound [Cu(en)(2)](4)[(SiMo8V4O40)-O-v(V-IV O)(2)] [MoO4](2) . 5H(2)O has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. Black crystals crystallize in the tetragonal. system, space group 14/m, a = b = 14.019(2) Angstrom, c = 20.341(4) Angstrom, V = 3997.9(11) Angstrom(3), Z = 2, lambda(MoKalpha) = 0.71073 Angstrom (R(F) = 0.0443 for 1819 reflections). Data were collected on a Siemens P4 four-circle diffractometer at 293 K in the range of 1.76 < theta < 24.98degrees using the omega-scan technique. The structure was solved by the direct method and refined by the full-matrix least squares on F-2 method using the SHELXL-97 software. X-ray crystallographic study showed that the title compound contained a bicapped alpha-Keggin fragment [SiMo8 (V4O40)-O-v((VO)-O-IV)(2)](4-) polyoxoanion.

PENDANT FUNCTIONAL-GROUP COPOLYETHER SULFONES .1. SYNTHESIS AND CHARACTERIZATION OF NEW COPOLYETHER SULFONES WITH PENDANT ALDEHYDE GROUPS MODIFIED INTO PHENOLIC AZOMETHINE GROUPS

New functional copolyether sulfones with pendant aldehyde groups were synthesized by the classical polycondensation reaction between 4,4' -dichlorodiphenyl sulfone (I) and various bisphenols such as 5,5'-methylene bis-salicylaldehyde (II-2), 2,2-bis( 4-hydroxyphenyl)propane (III), and 2,6-bis(4-hydroxybenzylidene)cyclohexanone (IV). Condensation reaction with 4-aminophenol led to pendant phenolic azomethine groups containing copolyether sulfones. The structures of the resulting polymers were confirmed by IR, H-1-NMR spectra, and elemental analyses. The polymers were characterized by reduced viscosity, solubility, thermal stability, DSC, and x-ray diffraction measurements.

SYNTHESIS AND MOLECULAR-STRUCTURE OF NBU2[(MEO)3C6H2C(O)N2CHC6H4O]SN FORMED IN THE REACTION OF DI-N-BUTYLTIN(IV) OXIDE WITH 3,4,5-TRIMETHOXY-BENZOYL SALICYLAHYDRAZONE

The title complex was synthesized and characterized by H-1, C-13, Sn-119 NMR and IR spectra. A single crystal X-ray diffraction study confirmed its molecular structure and revealed that 3,4,5-trimethoxy-benzoyl salicylahydrazone was a tridentate and approximately planar ligand. The complex crystallizes in the triclinic space group P1BAR with a = 9.208(3), b = 12.536(2), c = 12.187(4) angstrom, alpha = 113.12(2), beta = 90.58(2), gamma = 81.42(2), V = 1277.5(6) angstrom, Z = 2. The structure was refined to R = 0.033 and R(w) = 0.041 for 3944 observed independent reflections. The tin atom has a distorted trigonal bipyramidal coordination. The Sn-C bond lengths are 2.129(5) and 2.113(5) angstrom (av. 2.121(5) angstrom), the C-Sn-C angle is 123.3(2); the bond length between the tin atom and the chelating nitrogen is 2.173(3) angstrom. Two chain carbon atoms and the chelating nitrogen atom occupy the basal plane. The skeleton of two erect oxygen atoms and the tin atom is bent (O-Sn-O angle = 153.5(1)). In the complex, the ligand exists in the enol-form.