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Journal of Structural Chemistry

2009 year, number 3

CRYSTAL STRUCTURES OF PYRIDINE-4-ALDEHYDE THIOSEMICARBAZONE PERCHLORATE AND TRIFLUOROMETHANE SULFONATE

A. I. Smolentsev, L. G. Lavrenova, V. N. Elokhina, A. S. Nakhmanovich, L. I. Larina
Keywords: perchlorate, triflate, pyridine-4-aldehyde thiosemicarbazone, synthesis, XRD, NMR spectra
Pages: 522-526

Abstract

The new salts of pyridine-4-aldehyde thiosemicarbazone: perchlorate (I) and trifluoromethane sulfonate (II) HN+C5H4-CH=N-NH-C(S)-NH2·X- (X = ClO4, CF3SO3) were synthesized and studied by IR and NMR spectroscopy and X-ray diffraction analysis. The compounds were synthesized by a reaction of pyridine-4-aldehyde thiosemicarbazone with chloric or trifluoromethane sulfonic acid, respectively. Compound I crystallized in the triclinic crystal system, space group P-1, a = 6.8691(2) Å, b = 9.5406(4) Å, c =
9.6348(4) Å, α = 78.838(1)°, β = 77.618(1)°, γ = 69.661(1)°, Z = 2. Compound II crystallized in the monoclinic crystal system, space group P21/c, a = 7.3149(8) Å, b = 11.9830(16) Å, c = 15.143(2) Å, β = 96.949(4)°, Z = 4. The structures are formed by hydrogen-bonded ions. Moreover, the cations are linked in "dimmers" due to the weak N-H…S hydrogen bonds.