Synthesis and Characterization of Three Vanadium(Ⅴ) Complexes Incorporating Tridentate Hydrazone Lig

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Divanadium(Ⅴ) complex [VO(aptch)(μ-OCH3)]2(1) and two monovanadium(Ⅴ) complexes [VO(apfah))(OEt)](2a and 2b,H2aptch = 2-hydroxyacetophenone thiophene-2-car-boxylic hydrazone,H2apfah = 2-hydroxyacetophenone 2-furoic acid hydrazone) have been synthesized and characterized.Single-crystal X-ray diffraction studies reveal that 1 is a cen-trosymmetric dimer bridged by two methoxido O-atoms.Complex 1 crystallizes in the monoclinic crystal system,space groups P21/c with a = 7.4825(4),b = 17.0928(11),c = 11.6961(7) ,β = 98.172(4)o,Z = 2,F(000) = 728,μ = 0.829 mm-1,the final R = 0.0457 and wR = 0.1137 for 2654 observed reflections with I > 2(I).The vanadium(V) is coordinated to the tridentate ligand,ethanol molecule to form a distorted square-pyramidal geometry,complexes 2a and 2b.Although 2a and 2b have the same asymmetric unit,they belong to different space groups.Complex 2a crystallizes in the monoclinic crystal system,space groups P21/n with a = 10.2293(2),b = 15.6660(3),c = 10.6298(2) ,β = 116.259(1)o,Z = 4,μ = 0.676 mm-1;complex 2b crystallizes in the triclinic crystal system,space groups P with a = 8.2808(4),b = 9.4704(5),c = 10.0819(5) ,α = 86.133(3),= 81.956(3),γ = 80.248(3)o,Z = 2 and μ = 0.670 mm-1.The hydrogen bonds are found to exist in 2b only.The crystal structure is stabilized by intermolecular hydrogen bonds of C-H···O. (Ⅴ) complexes [VO (apfah)) (OEt)] (2a and 2b, H2aptch = 2-hydroxyacetophenone thiophene-2 -car-boxylic hydrazone, H2apfah = 2-hydroxyacetophenone 2-furoic acid hydrazone has been synthesized and characterized. Single-crystal X-ray diffraction studies have shown that 1 is a cen-trosymmetric dimer bridged by two methoxido O-atoms. Complex 1 crystallizes in the monoclinic crystal system, space groups P21 / c with a = 7.4825 (4), b = 17.0928 (11), c = 11.6961 (7) ) = 728, μ = 0.829 mm-1, the final R = 0.0457 and wR = 0.1137 for 2654 observed reflections with I> 2 (I). The vanadium (V) is coordinated to the tridentate ligand, ethanol molecule to form a distorted squares 2a and 2b have the same asymmetric unit, they belong to different space groups. Complex 2a crystallizes in the monoclinic crystal system, space groups P21 / n with a = 10.2293 (2), b = 15.6660 (3), c = 10.629 Complex 2b crystallizes in the triclinic crystal system, space groups P with a = 8.2808 (4), b = 9.4704 (5) ), c = 10.0819 (5) α, α = 86.133 (3), = 81.956 (3), γ = 80.248 (3) o, Z = 2 and μ = 0.670 mm-1. The hydrogen bonds are found to exist in 2b only. The crystal structure is stabilized by intermolecular hydrogen bonds of CH ··· O.
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