We present a new method for the synthesis of bis-triazolones 3, which result from the processing of novel bis-amidrazones 2 with ethyl chloroformate. The bis-amidrazones 2 are prepared by the reaction of the N1-tosylhydrazonates 1 with two equivalents of aliphatic diamine. The structures of the new products were determined through IR, 1H and 13C NMR studies as well as elemental analysis. The molecular structure of the compound 3c was also determined via an X-ray analysis. The antimicrobial activity of the synthesized compounds was evaluated against a panel of 09 bacterial strains using broth microdilution methods. Results showed that compounds exhibited moderate to strong antibacterial activity against the tested species.
Whereas several studies have been made in the solid state on complexes between antimony(III) and bromide or iodide, only few complexes of antimony(III) chlorides with organic cations have been investigated. In these compounds the metal shows a tendency towards distorted octahedral coordination with some rather long Sb-Cl bonds, which is attributed to the crystalpacking forces, e.g. hydrogen bonds rather than by lone electron-pair repulsion. These compounds are interesting because they exhibit phase transitions (ferro-paraelectric) related to motions of the ammonium cations. Here, we describe the crystal structure of (4-dimethylaminopyridinium) tetrachloroanti monate(III).The complex crystals were obtained by dissolving in a concentrated HCl solution a stoichiometric mixture of 4-dimethylaminopyridine and trichloride antimony(III); the resulting aqueous solution was then kept at room temperature. After several weeks of evaporation, pseudohexagonal prismshaped monocrystals of (4-dimethylaminopyridinium)tetrachloroantimonate(III) appeared in the solution. Chemical analyses of antimony atoms and chloride anions were carried out. 5 The experimental conditions used for single-crystal data collections are reported in Table 1. The positional parameters for the antimony atoms were obtained from a three-dimensional Patterson map, while the remaining atoms were found from a successive difference Fourier map. After introducing anisotropic thermal displacement parameters for the non-hydrogen atoms, the hydrogen atoms were localized and optimized to fixed positions. Their contributions were isotropically introduced into the calculation, but not refined. The final atomic coordinates are given in Table S1 (supporting information).The final anisotropic full-matrix least squares resulted in a convergence of the R factor to 0.0316, incorporating the weighting scheme w = 1/[s 2 (Fo 2 ) + (0.0746P) 2 ] + 0.8242P], where P = (Fo 2 + 2Fc 2 )/3.The molecular structure of the (4-dimethylaminopyridinium)-tetrachoroantimonate is shown in Fig. 1. The crystal structure consists of 4-dimethylaminopyridinium cations and polynuclear anions in which distorted SbCl6 octahedron sharing cis edges are interconnected into chains (Fig. 2). The [SbCl4] -anions share two cis edges with two other neighboring octahedra, and a skew infinite chain is formed parallel to the c axis at x = 0, y = 0 and x = 0.5, y = 0.5. Each Sb atom is surrounded by six Cl atoms, forming a distorted octahedral configuration with Cl-Sb-Cl
X-ray Structure Analysis Online
Synthesis and Crystal Structure of (4-Dimethylaminopyridinium)-tetrachoroantimoniateAfef GHOUILI, Najla CHAARI, † and Fatma ZOUARI
Laboratoire des Sciences des Matériaux et d'Environnement, Faculté des Sciences de Sfax, BP 802, 3018 Sfax, TunisiaThe salt tris(4-dimethylaminopyridinium)tetrachoroantimonate C7H11Cl4N2Sb crystallizes at room temperature in the monoclinic system with space group C2/c. The unit-cell dimensions are: a = 13.6692 (5)
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