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Original Articles

Syntheses and Structures of Oxovanadium (IV) Complexes, HB(pz)3VO(ph‐acac) · 2H2O (pz, Pyrazole) and HB(3,5‐Me2pz)3VO(ph‐acac) · 2H2O and V2O4[HB(pz)3]2 · 2CH3CN

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Pages 203-211 | Received 29 Mar 2006, Accepted 02 Apr 2006, Published online: 25 Apr 2007
 

The reaction of VO(ph‐acac)2 (ph‐acac=phenyacetylacetonato) with NaHB(pz)3 (pz=pyrazole) or NaHB(3,5‐Me2pz)3 in the solution of MeOH gave oxovanadium (IV) complexes HB(pz)3VO(ph‐acac) · 2H2O (1) and HB(3,5‐Me2pz)3VO(ph‐acac) · 2H2O (2), respectively. An oxovanadium complex, V2O4[HB(pz)3]2 · 2CH3CN (3), was obtained by the reaction of VOSO4 · 3H2O with tri(pyrazolyl)borate sodium in MeOH. The complexes 1, 2 and 3 were characterized by elemental analysis, IR, UV‐Vis, NMR. In particular, the crystals of complex 1 and 3 were determined by X‐ray diffraction. They crystallize in space group P2 1/c, a=16.497(5) Å, b=7.6601(19) Å, c=17.199(4) Å, β=107.498(19)°, V=2072.8(9) Å3, Z=4, R=0.0371 (I>2σ(I)) for 1; in the monoclinic, space group Pbca, with cell dimensions of a=15.531(2) Å; b=18.007(2) Å; c=10.725(2) Å; V=2999.4(8) Å3, Z=4, R= 0.0401(I>2σ(I)) for 3. Structure analyses have shown that complex 1 is a monomeric oxovanadium complexe containing polypyrazolylborate and two lattice water. Complex 3 consists of a V2O4(HB(pz)3)2 molecule and two free CH3CN lattice molecules in an unit cell. Both possess a similar coordination mode for the vanadium atom. In addition, luminescence properties and thermal analysis characterization of the complexes also are discussed.

We wish to express our sincere thanks to National Natural Science Foundation of China (No. 20571036), and SRF for ROCS, SEM and Education Foundation of Liaoning Province (No. 05L212) and Japan Society for the Promotion of Science for Postdoc. Grant (2001, 9 – 2003, 9. No: P01072) for financial assistance.

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