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a = 12.668(5) Å, b = 8.084(3) Å, c = 17.222(6) Å, α = 108.148(12)° A series of vanadium(III) and oxovanadium(IV/V) compounds with the ligands, N-(2-nitrophenyl)pyridine-2-carboxamide (Hpycan), N-(phenyl)pyridine-2-carboxamide (Hpheca), and N-(2-pyridyl)acetamide (Hpyra), containing the amide functionality, was prepared and characterized both in solution and in solid state. All vanadium compounds contain a vanadium - amide oxygen bond. Crystal data for [VOCl2(OC2H5)(Hpheca)] (4) are monoclinic P21la Z = 4. In addition to the synthesis and crystallographic studies, the optical, infrared, and magnetic properties of these compounds are reported. Electron paramagnetic resonance [of oxovanadium(IV) species] and 1H, 13C{'H}, and 51V nuclear magnetic resonance [of oxovanadium(V) compounds] properties are reported as well. 37 26 6785 6794 Cited By :18

3, C19H13N3O2SV, Mr = 398.34, monoclinic, P21/n, a = 12.1108(10) Å, b = 19.4439(18) Å, c = 7.2351(7) Å, β = 103.012(3)°, V = 1660.0(4) Å3, Z = 4, R = 0.0355, and Rw = 0.0376 4·CH3CN, C19H12N3O4VNa·CH 3CN, Mr = 461.31, monoclinic, P21/c, a = 11.528(1) Å, b = 11.209(1) Å, c = 16.512(2) Å, β = 103.928(4)°, V = 2071.0(5) Å3, Z = 4, R = 0.0649, and Rw = 0.0806 5·2CH3OH, C20H10N2O5VNa 2·2CH3OH, Mr = 519.31, triclinic, P1, a = 12.839(1) Å, b = 8.334(1) Å, c = 12.201(1) Å, α = 106.492(2)°, β = 105.408(2)°, γ = 73.465(2)°, V = 1175.6(3) Å3, Z = 2, R = 0.0894, and Rw = 0.1043 Reaction of the amide ligand N-[2·((2-pyridylmethylene)amino)phenyl]pyridine-2-carboxamide (Hcapca) with VCl3 affords the compound trans·[VCl2(capca)] (1), the first example of a vanadium(III) complex containing a vanadium-deprotonated amide nitrogen bond, while reaction of bis(pentane-2,4-dionato)oxovanadium(IV) with the related ligands N-[2-((2-phenolylmethylene)amino)phenyl]pyridine-2-carboxamide (H2phepca), 1-(2-hydroxybenzamido)-2-(2-pyridinecarboxamido)benzene (H3hypyb), and 1,2-bis(2-hydroxybenzamido)benzene (H4hybeb) yields the complexes [VO(phepca)] (2), Na[VO(hypyb)]·2CH3OH (4·2CH3OH), and Na2[VO(hybeb)]·3CH3OH (5·3CH3OH) respectively. The preparation of the complex {N-[2-((2-thiophenoylmethylene)amino)phenyl]pyridine2-carboxamido} oxovanadium(IV) (3) has been achieved by reaction of N-(2-aminophenyl)pyridine-2-carboxamide and 2-mercaptobenzaldehyde with [VO(CH3COO)2]x. Oxidation of complex 5·3CH3OH with silver nitrate gives its vanadium(V) analogue (8·CH3OH), which is readily converted to its corresponding tetraethylammonium salt (10·CH2Cl2) by a reaction with Et4NCl. The crystal structures of the octahedral 1·CH3CN, and the square-pyramidal complexes 3, 4·CH3CN, 5·2CH3OH, and 10 were demonstrated by X-ray diffraction analysis. Crystal data are as follows: 1·CH3CN, C18H13Cl2N4OV·CH 3CN Mr = 464.23, monoclinic, P21/n, a = 10.5991(7) Å, b = 13.9981(7) Å, c = 14.4021(7) Å, β= 98.649(2)°, V = 2112.5(3) Å3, Z = 4, R = 0.0323, and Rw 0.0335 10, C28H32N3O5V Mr = 541.52, monoclinic, P21/c, a = 11.711(3) Å, b = 18.554(5) Å, c = 12.335(3) Å, β = 95.947(9)°, V = 2666(2) Å3, Z = 4, R = 0.0904, and Rw = 0.0879. In addition to the synthesis and crystallographic studies, we report the optical, infrared, magnetic, and electrochemical properties of these complexes. Electron paramagnetic resonance [of oxovanadium(IV) species] and 1H, 13C{1H}, and 51V nuclear magnetic resonance [of oxovanadium(V) complex] properties are reported as well. This study represents the first systematic study of vanadium(III), VIVO2+, and VVO3+ species containing a vanadium-deprotonated amide nitrogen bond. 35 2 357 367 Cited By :84

33 5 845 846 Cited By :33

Reaction of the amide ligand N-[2-(2-pyridylmethyleneamino)phenyl]pyridine-2-carboxamide (Hcapca) with VCl3 affords the compound trans-[VCl2(capca)] 1, the first example of a vanadium(III) complex containing a vanadium-deprotonated amide nitrogen bond, while reaction of bis(pentane-2,4-dionato)oxovanadium(IV) with the related ligands 1,2-bis(2-hydroxybenzamido)benzene (H-4hybeb) and 1-(2-hydroxybenzamido)-2-(2-pyridinecarboxamido)benzene (H-3hypyb) yields the complexes Na2[VIVO(hybeb)] 2 and Na[VIVO(hypyb)] 3 respectively; the X-ray crystal structures of 1 and 3 are reported. Journal of the Chemical Society-Chemical Communications

Reaction of the amide ligand N-[2-((2-pyridylmethylene)amino)phenyl]pyridine-2-carboxamide (Hcapca) with VCl3 affords the compound trans-[VCl2(capca)] (1), the first example of a vanadium(III) complex containing a vanadium-deprotonated amide nitrogen bond, while reaction of bis(pentane-2,4-dionato)oxovanadium(IV) with the related ligands N-[2-((2-phenolylmethylene)amino)phenyl] pyridine-2-carboxamide (H(2)phepca), 1-(2-hydroxybenzamido)-2-(2-pyridinecarboxamido)benz (H(3)hypyb), and 1,2-bis(2-hydroxybenzamido)benzene (H(4)hybeb) yields the complexes [VO(phepca)] (2), Na[VO(hypyb)]. 2CH(3)OH (4 . 2CH(3)OH), and Na-2[VO(hybeb)]. 3CH(3)OH (5 . 3CH(3)OH) respectively. The preparation of the complex {N-[2-((2-thiophenoylmethylene)amino)phenyl]pyridine 2-carboxamido}oxovanadium(IV) (3) has been achieved by reaction of N-(2-aminophenyl)pyridine-2-carboxamide and 2-mercaptobenzaldehyde with [VO(CH3COO)(2)](x). Oxidation of complex 5 . 3CH(3)OH with silver nitrate gives its vanadium(V) analogue (8 . CH3OH), which is readily converted to its corresponding tetraethylammonium salt. (10 . CH2Cl2) by a reaction with Et(4)NCl. The crystal structures of the octahedral 1 . CH3CN, and the square-pyramidal complexes 3, 4 . CH3CN, 5 . 2CH(3)OH, and 10 were demonstrated by X-ray diffraction analysis. Crystal data are as follows: 1 . CH3CN, C18H13Cl2N4OV . CH3CN M(r) = 464.23, monoclinic, P2(1)/n, a = 10.5991(7) Angstrom, b = 13.9981(7) Angstrom, c = 14.4021(7) Angstrom, beta = 98.649(2)degrees, V = 2112.5(3) Angstrom(3), Z = 4, R = 0.0323, and R(w) = 0.0335; 3, C19H13N3O2SV, M(r) = 398.34, monoclinic, P2(1)/n, a = 12.1108(10) Angstrom, b = 19.4439(18) Angstrom, c = 7.2351(7) Angstrom; beta = 103.012(3)degrees, V = 1660.0(4) Angstrom(3), Z = 4, R = 0.0355, and R(w) = 0.0376; 4 . CH3CN, C19H12N3O4VNa . CH3CN, M(r) = 461.31, monoclinic, P2(1)/c, a = 11.528(1) Angstrom, b = 11.209(1) Angstrom, c = 16.512(2) Angstrom, beta = 103.928(4)degrees, V = 2071.0(5) Angstrom(3), Z = 4, R = 0.0649, and R(w) = 0.0806; 5 . 2CH(3)OH, C20H10N2O5VNa2 . 2CH(3)OH, M(r) = 519.31, triclinic, P1, a = 12.839(1) Angstrom, b = 8.334(1) Angstrom, 12.201(1) Angstrom, alpha = 106.492(2)degrees, beta = 105.408(2)degrees, gamma = 73.465(2)degrees, V = 1175.6(3) Angstrom(3), Z = 2, R = 0.0894, and R(w) = 0.1043; 10, C28H32N3O5V M(r) = 541.52, monoclinic, P2(1)/c, a = 11.711(3) Angstrom, b = 18.554(5) Angstrom, c = 12.335(3) Angstrom, beta = 95.947(9)degrees, V = 2666(2) Angstrom(3), Z = 4, R = 0.0904, and R(w) = 0.0879. In addition to the synthesis and crystallographic studies, we report the optical, infrared, magnetic, and electrochemical properties of these complexes. Electron paramagnetic resonance [of oxovanadium(IV) species] and H-1, C-13{H-1}, and V-51 nuclear magnetic resonance [of oxovanadium(V) complex] properties are reported as well. This study represents the firsr systematic study of vanadium(III), (VO2+)-O-IV, and (VO3+)-O-V species containing a vanadium-deprotonated amide nitrogen bond. Inorg Chem