Navegando por Autor "Janczak, Jan"
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Item Syntheses and characterization of novel heteroleptic nickel complexes with dithiocarbimates and trithiocarbimates(Inorganica Chimica Acta, 2017-06-01) Castro, Rodrigo A.; Oliveira, Marcelo R. L.; Janczak, Jan; Rubinger, Mayura M. M.The potassium N-R-sulfonyldithiocarbimates, K2(RSO2NCS2) [R = CH3 (1a), CH3CH2 (1b), C6H5 (1c), 2-CH3C6H4 (1d) and 4-CH3C6H4 (1e)], reacted with nickel sulfate or zinc acetate to yield complex anions which were isolated as their tetraphenylphosphonium salts with the formulae (PPh4)2[M(RSO2NCS2)2], were M = Ni (2a–2e) and M = Zn (3a–3e). The compounds 3a–3e readily react with sulfur in dimethylformamide producing bis(trithiocarbimato)-zinc complexes (4a–4e) with the formula (PPh4)2[Zn(RSO2NCS3)2]. Mixed nickel complexes (5a–5e), (PPh4)2[Ni(RSO2NCS2)(RSO2NCS3)], were obtained from the zinc compounds 4a–4e by reaction with nickel sulfate in dimethylsulfoxide. The complexes 5a–5e are the first examples of N-R-sulfonyldithiocarbimate and N-R-sulfonyltrithiocarbimate heteroleptic nickel complexes. The structures of 5a and 5e were determined by X-ray crystallography. Both compounds crystallize in the centrosymmetric space group of the triclinic system. The Ni2+ cation is S,S-chelated by one dithio- and one trithiocarbimate ligands, forming distorted square-planar configurations. The square planar geometry around the nickel atom was confirmed for compounds 5a–5e by electronic, vibrational and nuclear magnetic resonance spectroscopies. High-resolution mass spectrometry and elemental analyses confirmed the molecular formulae.Item Syntheses, crystal structure, spectroscopic characterization and antifungal activity of new N-R-sulfonyldithiocarbimate metal complexes(Journal of Inorganic Biochemistry, 2009-07) Alves, Leandro C.; Rubinger, Mayura M. M.; Lindemann, Renata H.; Perpétuo, Genivaldo Júlio; Janczak, Jan; Miranda, Liany D. L.; Zambolim, Laércio; Oliveira, Marcelo R. L.Five new compounds with the general formula of (Bu4N)2[M(RSO2NCS2)2], where Bu4N = tetrabutylammonium cation, (M = Ni, R = 4-FC6H4) (1), (M = Zn, R = 4-FC6H4, 4-ClC6H4, 4-BrC6H4, 4-IC6H4), (2), (3), (4) and (5), respectively, were obtained by the reaction of the appropriate potassium N-R-sulfonyldithiocarbimate (RSO2NCS2K2) with nickel(II) chloride hexahydrate or zinc(II) acetate dihydrate in metanol:water 1:1. The elemental analyses and the IR data are consistent with the formation of the expected bis(dithiocarbimato)metal(II) complexes. The 1H and 13C NMR spectra showed the signals for the tetrabutylammonium cation and the dithiocarbimate moieties. The compounds 1, 2 and 5 were also characterized by X-ray diffraction techniques. The nickel(II) is coordinated by two N-4-fluorophenylsulphonyldithiocarbimato(2-) ligands forming a planar coordination. The zinc(II) exhibits distorted tetrahedral configuration in compounds 2 and 5 due to the chelation effect of two sulfur atoms of the N-R-sulfonyldithiocarbimate ligands. The antifungal activities of the compounds were tested in vitro against Colletotrichum gloeosporioides, an important fungus that causes the plant disease known as anthracnose in fruit trees. All the complexes were active.Item Syntheses, structural and spectroscopic characterization of novel zinc(II)-bis(trithiocarbimato) complexes and bis(N-methylsulfonyldithiocarbimate) -sulfide(Polyhedron, 2012-01-04) Tavares, Eder do Couto; Oliveira, Marcelo Ribeiro Leite; Janczak, Jan; Vieira, Camila Grossi; Alves, Leandro de Carvalho; Castro, Rodrigo Antunes; Vieira, Lígia Maria Mendonça; Lindemann, Renata Hernandez; Perpétuo, Genivaldo Júlio; Visconte, Leila Léa Yuan; Rubinger, Mayura Marques MagalhãesFour zinc(II)-bis(trithiocarbimato) complexes with the general formula A2[Zn(RSO2NCS3)2] [A = Ph4P+: R = CH3 (1), 4-CH3C6H4 (2); A = Bu4N+: R = CH3 (3), 4-CH3C6H4 (4)] were obtained by the reaction of sulfur with the correspondent zinc(II)-bis(dithiocarbimato) complexes. Additionally, the compound (Ph4P)2[(CH3SO2NCS2)2S)] (5) was prepared from the potassium methylsulfonildithiocarbimate by oxidation with iodine. The compounds were characterized by elemental analyses and IR, 1H NMR and 13C NMR spectroscopies. The compounds 4 and 5 were also characterized by X-ray diffraction techniques. The compound 4 crystallizes in the centrosymmetric space group C2/c of the monoclinic system. The Zn(II) is in a distorted tetrahedral environment (ZnS4) in compound 4, and differ from the coordination mode observed in compound 1, which involves one sulfur and one nitrogen atom of each trithiocarbimate ligand. Compound 5 is the first example of a compound containing a bis(N-alkylsulfonyldithiocarbimate)-sulfide dianion and crystallises in the non-centrosymmetric space group P41212 of the tetragonal system.Item Synthesis, structural and spectroscopic characterization of novel zinc(II) complexes with N-methylsulfonyldithiocarbimato and N-methylsulfonyltrithiocarbimato ligands(Polyhedron, 2007-01-02) Oliveira, Marcelo R. L.; Perpetuo, Genivaldo J.; Janczak, Jan; Rubinger, Mayura M. M.Two new zinc(II)-complexes, dithiocarbimato (Ph4P)2[Zn(CH3SO2N=CS2)2] (1) and trithiocarbimato (Ph4P)2[Zn(CH3SO2N=CS3)2] (2), were obtained in the crystalline form by the reaction of potassium N-methylsulfonyldithiocarbimate (RSO2N=CS2K2) with zinc(II) acetate dihydrate and tetraphenylphosphonium chloride in dimethylformamide. Both complexes crystallize in the monoclinic system. The central Zn(II) ion has a distorted tetrahedral coordination in both compounds. In 1 the dithiocarbimato ligand coordinates via two S atoms while in 2 the trithiocarbimato ligand coordinates via S and N atoms. Both complexes were also characterized by IR, 1 H NMR and 13C NMR spectroscopies. Compound 2 is the first example of a zinc(II)-trithiocarbimato complex.