The vic-dioximes are compounds with various industrial uses and scientific applications [1–3]. Many coordination compounds have been synthesized based on vic-dioximes. This study presents the synthesis and full characterization of two vic-dioximes based on dichloroglyoxime, p-aminobenzoic acid and p-aminotoluene. The reaction proceeded according to the scheme: Their structures were proved by IR, 1H, 13C and 15N NMR spectral analysis and single crystal X-ray diffraction. After diffraction, the new vic-dioxime bis(p-aminobenzoic acid) glyoxime hydrate (H4L1·H2O, 1) and bis(di-p-aminotoluene glyoxime) mono-p-aminotoluene trihydrate ((H2L2)2·pat·3H2O, 2), were obtained. Antimicrobial activity was tested for both ligands. One of the reported vic-dioximes, bis(di-p-aminotoluene)glyoxime mono-p-aminotoluene trihydrate showed good to moderate antimicrobial activity against both non-pathogenic Gram-positive and Gram-negative bacteria (Bacillus subtilis and Pseudomonas fluorescens), phytopathogenic (Xanthomonas campestris, Erwinia amylovora, E. carotovora) and the fungi (Candida utilis and Saccharomyces cerevisiae) at MIC – 70-150 μg/mL (Table). Table 1. In vitro antifungal and antibacterial activities of compound 1 and 2. MBC and MFC, μg/mL Compd Bacillus subtilis Pseudomonas fluorescens Erwinia amylovora Erwinia carotovora Xanthomonas campestris Candida Utilis Saccharomuces cerevisiae 1 N/A N/A N/A N/A N/A N/A N/A 2 70 150 70 150 150 70 150 MBC – minimal bactericidal concentration; MFC - minimal fungicidal concentration; N/A – non active Looking to the data presented in Table it is well seen that compound 2 exhibits variable biological activity depending on the bacterial or fungicidal species. A possible cause of this variation could be the impermeability of the cells of the microorganism or the difference between the ribosomes of the microbial cells [4].