Dr Mala Sharma, Dr Kumari Bandna | International Journal of Energetic Materials | Vol 12, Issue 01 | pp. 1-6 | ISSN: 2456-3976
Abstract
A niobium(V) complex with the composition [NbCl(OC₆H₄CH(CH₃)₂-2)₄] was synthesized by reacting niobium pentachloride with four equivalents of 2-isopropylphenol in carbon tetrachloride as a solvent, yielding the product in good quantity. The complex was characterized using elemental analysis, molar conductance measurements, IR spectroscopy, ¹H and ¹³C NMR spectroscopy, and mass spectrometry. Spectroscopic results indicate that the complex exists in a dimeric form, with bridging occurring through isopropylphenoxo ligands. X-ray diffraction analysis suggests that the complexes are amorphous in nature.
The methanolic solution of the synthesized complex, monochlorotetrakis(2-isopropylphenoxo)niobium(V), [NbCl(OC₆H₄CH(CH₃)₂-2)₄], reacts with equimolar amounts of potassium benzohydroxamate and p-chlorobenzohydroxamate in benzene to form mixed-ligand phenoxo-hydroxamato niobium(V) complexes. These products were confirmed through physicochemical studies along with IR and ¹H NMR spectral analyses. The spectral evidence indicates that potassium benzohydroxamate and p-chlorobenzohydroxamate effectively cleave the isopropylphenoxo bridging bonds, resulting in the formation of monomeric (unimolecular) complexes.
References
[1] Buchard A., Davidson M. G., du Sart G. G., Jones M. D., Kociok-Köhn G., McCormick S. N. and Mckeown P. 2023. Coordination of ε-Caprolactone to a Cationic Niobium(V) Alkoxide Complex: Fundamental Insight into Ring-Opening Polymerization via Coordination–Insertion. Inorganic Chemistry. 62(38). 15688–15699. [2] Srisupap N., Wised K. , Tsutsumi K. and Nomura K. 2018. Synthesis of (Arylmido)niobium(V) Complexes Containing Ketimide, Phenoxide Ligands, and Some Reactions with Phenols and Alcohols. ACS Omega. 3(6). 6166-6181. [3] Schwartz V. and Oyama S. T. 1997. Study of Niobium Oxynitride: Synthesis, Characterization, and Reactivity. Chemistry of Materials. 9(12). 3052-3059. [4] Plaman A . S. and Durr C. B. 2022. Investigating the Ring-Opening Polymerization Activity of Niobium and Tantalum Ethoxides Supported by Phenoxyimine Ligands. ACS Omega. 7(27). 23995-24003. [5] Sheng Y., Wang Y. , Yin S. , Zhao L., Zhang X. and Liu D. 2023, Niobium-Based Oxide for Anode Materials for Lithium-Ion Batteries. Chemistry A Europian Journal. 30(19). [6] Ganeshpurkar A., Kumar D., Singh S.K. 2018. Strategies for the Synthesis of Hydroxamic Acids. Curr. Org. Synth. 15. 154–165. [7] Tretyakov B., Gadomsky S., Terentiev A. 2023. A Reaction of N-substituted Succinimides with Hydroxylamine as a Novel Approach to the Synthesis of Hydroxamic Acids. Beilstein Arch. 6–19. [8] Ali D.B., Abedullah S.A. 2023. Preparation of Some Hydroxamic Acid Derivatives and Study of their Biological Activity as Anti-Cancer and Anti-Bacterial Agents. HIV Nurs. 23. 809–816. [9] Fazary A., Khalil M., Fahmy A., Tantawy T. 2001. The role of hydroxamic acids in biochemical processes. Med. J. Islam. Acad. Sci. 14. 109–116. [10] Saban N., Bujak M. 2009. Hydroxyurea and hydroxamic acid derivatives as antitumor drugs. Cancer Chemother. Pharmacol. 64. 213–221. [11] Citarella A., Moi D., Pinzi L., Bonanni D., Rastelli G. 2021. Hydroxamic Acid Derivatives: From Synthetic Strategies to Medicinal Chemistry Applications. ACS Omega. 6. 21843–21849. [12] Al Shaer D., Al Musaimi O., de la Torre B.G., Albericio F. 2020. Hydroxamate siderophores: Natural occurrence, chemical synthesis, iron-binding affinity and use as Trojan horses against pathogens. Eur. J. Med. Chem. 208. 112791. [13] Adiguzel E. , Yilmaz F., MEmirik M., Ozil M. 2017. Synthesis and characterization of two new hydroxamic acids derivatives and their metal complexes. An investigation on the keto/enol, E/Z and hydroxamate/hydroximate forms. Journal of Molecular Structure. 1127. 403-412. [14] Sharma M. 2018. Synthesis, Spectroscopic Studies and Reactivity of Monochlorotetrakis (2-/4- Isopropylphenoxo) Niobium (V) Complexes. International Journal of Current Advanced Research. 7(4). 11777-11783.