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Communication Dans Un Congrès Année : 2007

Low temperature high resolution x-ray diffraction data for 4-methyl-3-thiosemicarbazide

Résumé

Continuing the investigation on the electronic properties of the thiosemicarbazide based compounds [1] we have collected the high resolution low temperature diffraction data for 4-methyl-3-thiosemicarbazide. Here we present the crystal structure of this compound based on the high resolution data set. This preliminary analysis should serve as an indicator of the quality of the data for the following charge density study. The single crystal X-ray analysis revealed that an asymmetric unit in the crystal structure of the analyzed compound contains two crystallographically independent molecules. The molecules show only small differences in bond distances and angles, but they have dissimilar network of intermolecular hydrogen bonds. Both molecules form numerous interactions of N−H···S, N−H···N and C−H···N type. The molecules B form dimers through N3b−H3b···N1b interactions and further via intermolecular N1b−H11b···S1b interactions form a chain of dimers. Preliminary electron density maps, which can serve as pointer of quality of the data, were determined for both independent molecules. These maps clearly indicate that the maxima of charge density are localized in the region of C−N, N−N and C−S bonds. Also, maxima exist in the vicinity of the N1, N2 and S1 atoms corresponding to their free electron pairs. The X-ray diffraction data were collected at 100.0(1) K on a Bruker-SMART three axis diffractometer equipped with a SMART 1000 CCD area detector using monochromated Mo Kα radiation (wavelength λ = 0.71073 Å) in the range 0<θ<51.4º. The total number of the reflections collected was 115688 with the average measurement multiplicity of 10.2. The data sorting and averaging led to a 10361 unique reflections with final Rint = 2.31 %. Crystallographic data: formula C4H14N6S2, monoclinic crystal system, space group P21/c, a = 5.9666(2), b = 8.7396(6), c = 19.1354(2) Å, β = 92.854(2)º, V = 996.59(8) Å3. Structure was solved using the SHELXS97 program and was refined by SHELXL97 to a residual R-factor of 2.78 % for 7506 reflections with I>3σ(I) and 165 refined parameters. [1] S. B. Novakovic, B. Fraisse, G. A. Bogdanovic, A. Spasojevic-de Bire, Crystal Growth Design, 7 (2007), 191-195.

Domaines

Cristallographie
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Dates et versions

hal-00207456 , version 1 (17-01-2008)

Identifiants

  • HAL Id : hal-00207456 , version 1

Citer

Bojana M. Draskovic, Sladjana B. Novaković, Goran A. Bogdanović, Anne Spasojevic - de Biré. Low temperature high resolution x-ray diffraction data for 4-methyl-3-thiosemicarbazide. XIV Conference of Serbian Crystallographic Society, Jun 2007, Soko Banje. ⟨hal-00207456⟩
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