A dimeric oxidovanadium(V} complex derived from a hydrazonate ligand with an unusual asymmetrically bridged [i-(oxido]|i-(H20]{oxidovanadium(V}}2 core

摘要

The binuclear oxidovanadium(V) complex [{VO0(L)}2(u-O)(u-H2O)]-2CH3CN (1), where L2~ is the dianion of the Schiff base 2-salicylaldehyde-2-hydroxybenzoylhydrazone, were prepared and characterized by elemental analysis, FTIR, 1H, 13C and 51V NMR. Furthermore, the crystal structure of the compound 1 was determined by single crystal X-ray diffractometry revealing a distorted octahedral OsN-coordination geometry around the V(V) acceptor centers. The vanadium ions are connected by the u-O2- and the U-H2O asymmetric bridges located in the edge between the two octahedrons which keeps a distance of 3.194 A between the two vanadium centers. Crystal data for C32H28N6O10V2 (M =758.48 g/mol): orthorhombic, space group P212121 (no. 19), a = 12.9655(8) A, b = 14.1902(9) A, c = 18.4379(10) A, V= 3392.3(4) A3, Z= 4, T= 293(2) K, u(MoKa) = 0.616 mm1, Dcalc = 1.485 g/cm3, 18803 reflections measured (3.622° < 20 < 56.704°), 8263 unique (Rmt = 0.0473, Rsigma = 0.1020) which were used in all calculations. The final Ri was 0.0509 (I > 2ct(I)) and wR2 was 0.1531 (all data). The (VO)2(n-O)(n-H2O) core in compound 1 represents a rare case and few examples of similar type have been structurally characterized.