Reaction of a Co(III)-Peroxo Complex and NO: Formation of a Putative Peroxynitrite Intermediate Soumen Saha, Somnath Ghosh, Kuldeep Gogoi, Hemanta Deka, Baishakhi Mondal, and Biplab Mondal* , Department of Chemistry, Indian Institute of Technology Guwahati, North Guwahati, Assam 781039, India * S Supporting Information ABSTRACT: A Co(II) complex, [Co(L) 2 ]Cl 2 , 1 of the ligand L (L = bis(2-ethyl-4-methylimidazol-5-yl)methane) upon reaction with H 2 O 2 in methanol solution at -40 °C resulted in the formation of the corresponding Co(III)-peroxo complex [Co(L) 2 (O 2 )] + (2). The addition of NO gas to the freshly generated solution of the complex 2 led to the formation of the Co(II)-nitrato complex 3 through the putative formation of a Co(II)-peroxynitrite intermediate, 2a. The intermediate 2a was found to mediate the nitration of the externally added phenol resembling the nitration of tyrosine in biological systems. INTRODUCTION Nitric oxide (NO) is an important small molecule that is involved in various physiological processes such as neuro- transmission, vasodilation, immune response, etc. 1-4 Under normal conditions, NO is produced by the nitric oxide synthases (NOS) at low concentration. 5 However, an excess production of NO can have detrimental eects via the formation of secondary reactive nitrogen species (RNS) such as nitrogen dioxide (NO 2 ) and peroxynitrite (ONOO - ). 6 Both of these RNS are known to play important roles in biomolecule oxidation leading to the oxidative and nitrosative stress. 7 The nitric oxide deoxygenases (NODs) are known to control the in vivo level of NO by converting it into the biologically benign nitrate (NO 3 - ) and thereby removing the excess of it. 8 The conversion of NO to NO 3 - by NODs is believed to proceed through the formation of a peroxynitrite intermediate. 8,9 Peroxynitrite is proposed to form in vivo in a diusion- controlled reaction of NO and O 2 - anion or H 2 O 2 and nitrite (NO 2 - ) in the presence of the peroxidase enzymes. 10,11 An aqueous peroxynitrite is known to isomerize to the nitrate (NO 3 - ) very easily. 8 In the literature, peroxynitrites are exemplied to form either in the reaction of oxy-heme (formally, Fe III -O 2 · - ) proteins with NO or metal-nitrosyls with O 2 or O 2 - . 9,12 Recently, the peroxynitrite intermediates have been shown to form in the reaction of NO with Cr- superoxo or peroxo species. A Cr(IV)-peroxo complex ([Cr IV - (12-TMC)(O 2 )(Cl)] + ) {12-TMC = 1,4,8,11-tetramethyl- 1,4,8,11-tetraazacyclotetradecane} is reported to react with NO to result in a Cr(III)-nitrato complex, ([Cr III (12-TMC)- (NO 3 )(Cl)] + ), whereas the reaction of Cr(III)-superoxo complex [Cr III (14-TMC)(O 2 )(Cl)] + and NO resulted in the corresponding Cr(IV)-oxo complex ([Cr IV -(14-TMC)(O)- (Cl)] + ) and NO 2 presumably via the formation of a Cr(III)- peroxynitrite intermediate, [Cr III (14-TMC)(OONO)- (Cl)] + . 13-15 On the one hand, Nam et al. reported the reactivity of an Fe(III)-peroxo complex, [Fe III (14-TMC)- (O 2 )] + , with NO + as an approach for generating the peroxynitrite intermediate, which led to the formation of an Fe(III)-nitrato complex, [Fe III (14-TMC)(NO 3 )(F)] + . 16 On the other hand, Basalo et al. reported the reaction of a Co-nitrosyl with O 2 to result in the Co-nitrite, where the intermediate formation of a peroxynitrite is presumed. 17 Similarly, a nonheme dinitrosyliron complex has been shown to result in the corresponding nitrite in its reaction with O 2 . 18 Recently, Karlin and co-workers reported the reaction of a mixed-valent nitrosyl complex of Cu(I)Cu(II), namely, [Cu I,II 2 (UN-O - )- (NO)] 2+ with O 2 , to result in the superoxide and nitrosyl adduct, [Cu II 2 (UN-O - )(NO)(O 2 - )] 2+ , which was subsequently converted to the corresponding peroxynitrite complex. 19 In our laboratory, we have been working on the reactivity of the metal nitrosyls with O 2 - anion and H 2 O 2 with an aim to generate a peroxynitrite species. For example, {CuNO} 10 complex of the bis(2-ethyl-4-methylimidazol-5-yl)methane ligand was found to react with H 2 O 2 to aord the corresponding Cu(I)-nitrite, and the formation of a Cu(I)- peroxynitrite intermediate is presumed. 20 The same nitrosyl complex, upon reaction with O 2 - anion, was observed to result in Cu(II)-nitrite. 20 In an another example, the {CuNO} 10 complex in the presence of H 2 O 2 was shown to form Cu(II)- nitrite via a presumed peroxynitrite intermediate. 21 Cobalt nitrosyls, both with porphyrin and nonporphyrin ligands, were reported to react with O 2 and O 2 - to aord cobalt-nitrate/ nitrite complexes. 17,22 The involvement of a peroxynitrite Received: May 3, 2017 Article pubs.acs.org/IC © XXXX American Chemical Society A DOI: 10.1021/acs.inorgchem.7b01110 Inorg. Chem. XXXX, XXX, XXX-XXX