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Oxovanadium(IV, V) Complexes with 2‐Acetylpyridine‐2‐furanoylhydrazone (Hapf) as Ligand. X‐Ray Crystal Structures of [VO 2 (apf)] and [V 2 O 2 (μ‐O) 2 (apf) 2 ]
Author(s) -
Deflon Victor M.,
de Oliveira Daniela M.,
de Sousa Gerimário F.,
Batista Alzir A.,
Dinelli Luis R.,
Castellano Eduardo E.
Publication year - 2002
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/1521-3749(200206)628:5<1140::aid-zaac1140>3.0.co;2-f
Subject(s) - chemistry , vanadium , monoclinic crystal system , octahedron , ligand (biochemistry) , crystal structure , crystallography , electron paramagnetic resonance , orthorhombic crystal system , monobasic acid , medicinal chemistry , inorganic chemistry , polymer chemistry , biochemistry , physics , receptor , nuclear magnetic resonance
The preparation of oxovanadium(IV, V) coordination compounds with 2‐acetylpyridine‐2‐furanoylhydrazone (Hapf) is described. [VO(apf)(acac)] was prepared from oxovanadium(IV) diacetylacetonate [VO(acac) 2 ] by reaction with Hapf in methanol or dichloromethane. The complex is paramagnetic and its EPR spectrum is consistent with an octahedral coordination for the vanadium(IV) atom. Voltammetry studies of [VO(apf)(acac)] indicate an irreversible oxidation, in agreement with the chemical behavior of the compound in solution. The vanadium(IV) complex undergoes slow oxidation in alcoholic solution, losing the acetylacetonate ligand to form [VO 2 (apf)] and [V 2 O 2 (μ‐O) 2 (apf) 2 ]. The crystal structures of these last compounds were determined by X‐ray diffraction methods. [V 2 O 2 (μ‐O) 2 (apf) 2 ] crystallizes monoclinic [P2 1 /c, Z = 2, a = 817.400(10), b = 1650.90(3), c = 984.70(2) pm, β = 112.7190(10)°]. The crystal structure consists of dimeric units, in which two μ‐oxo ligands subtend asymmetric bridges between the vanadium atoms in a very distorted octahedral coordination. In the crystal of [VO 2 (apf)], orthorhombic [Pnma, Z = 4, a = 1630.000(10), b = 675.10(4), c = 1136.40(2) pm], the vanadium(V) atom is pentacoordinated.