Synthesis, structures and speciation studies of ruthenium(<scp>iii</scp>) hydroxamate/hydroximato complexes. Crystal and molecular structure of hydrated [Ru(H<sub>2</sub>edta)(2-methoxyphenylhydroxamate)], the first structurally characterised ruthenium(<scp>iii</scp>)–hydroxamate complex

Two ruthenium(III) complexes containing ethylenediaminetetraacetate(edta), viz. [{Ru(Hedta)} 2 L]· xH 2 O L = 4,4′-bipyridine(bpy) (1) and 4,4′-azopyridine(Azpy) (2), have been synthesized by the reaction between K[Ru(Hedta)Cl]·1.5H 2 O and the corresponding N-heterocycles. Complex 1 was determined by single-crystal X-ray diffraction. The products were characterized by IR, UV-vis, cyclic voltammetry, and magnetic techniques. Their DNA-binding activities were investigated using electronic absorption spectroscopic methods and fluorescence quenching; the experimental results show that these two ruthenium complexes may bind to CT-DNA through intercalation modes.

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“…K[Ru(Hedta)Cl]·1.5H 2 O was prepared as described [9]. 4,4′-Bipyridine and 4,4′-azopyridine were of reagent grade and used without purification.…”

Section: Methodsmentioning

confidence: 99%

Synthesis and characterization of dinuclear (Hedta)Ru(III) complexes with N-heterocyclic ligands: magnetic properties and DNA-binding studies

Wang

Zhao

Fang

et al. 2013

Journal of Coordination Chemistry

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“…Based on previous work, it was reasonable to expect that dihydroxamate or dihydroximate complexes would predominate at low or high pH values, respectively. 51 − 56 The former complexes would more likely be detected by positive ion mode ESI-MS and the latter complexes by negative ion mode. Mixed hydroxamate/hydroximate complexes might form at intermediate pH values, some of which could be intrinsically uncharged and MS-inactive.…”

Section: Resultsmentioning

confidence: 99%

Complexes Formed in Solution Between Vanadium(IV)/(V) and the Cyclic Dihydroxamic Acid Putrebactin or Linear Suberodihydroxamic Acid

et al. 2011

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An aerobic solution prepared from V(IV) and the cyclic dihydroxamic acid putrebactin (pbH2) in 1:1 H2O/CH3OH at pH = 2 turned from blue to orange and gave a signal in the positive ion electrospray ionization mass spectrometry (ESI-MS) at m/zobs 437.0 attributed to the monooxoV(V) species [VVO(pb)]+ ([C16H26N4O7V]+, m/zcalc 437.3). A solution prepared as above gave a signal in the 51V NMR spectrum at δV = −443.3 ppm (VOCl3, δV = 0 ppm) and was electron paramagnetic resonance silent, consistent with the presence of [VVO(pb)]+. The formation of [VVO(pb)]+ was invariant of [V(IV)]:[pbH2] and of pH values over pH = 2–7. In contrast, an aerobic solution prepared from V(IV) and the linear dihydroxamic acid suberodihydroxamic acid (sbhaH4) in 1:1 H2O/CH3OH at pH values of 2, 5, or 7 gave multiple signals in the positive and negative ion ESI-MS, which were assigned to monomeric or dimeric V(V)– or V(IV)–sbhaH4 complexes or mixed-valence V(V)/(IV)–sbhaH4 complexes. The complexity of the V-sbhaH4 system has been attributed to dimerization (2[VVO(sbhaH2)]+ ↔ [(VVO)2(sbhaH2)2]2+), deprotonation ([VVO(sbhaH2)]+ – H+ ↔ [VVO(sbhaH)]0), and oxidation ([VIVO(sbhaH2)]0 –e– ↔ [VVO(sbhaH2)]+) phenomena and could be described as the sum of two pH-dependent vectors, the first comprising the deprotonation of hydroxamate (low pH) to hydroximate (high pH) and the second comprising the oxidation of V(IV) (low pH) to V(V) (high pH). Macrocyclic pbH2 was preorganized to form [VVO(pb)]+, which would provide an entropy-based increase in its thermodynamic stability compared to V(V)–sbhaH4 complexes. The half-wave potentials from solutions of [V(IV)]:[pbH2] (1:1) or [V(IV)]:[sbhaH4] (1:2) at pH = 2 were E1/2 −335 or −352 mV, respectively, which differed from the expected trend (E1/2 [VO(pb)]+/0 < VV/IV–sbhaH4). The complex solution speciation of the V(V)/(IV)–sbhaH4 system prevented the determination of half-wave potentials for single species. The characterization of [VVO(pb)]+ expands the small family of documented V–siderophore complexes relevant to understanding V transport and assimilation in the biosphere.

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“…However, L1H2 has been previously used in constructing the heteroleptic ruthenium(III)hydroxamate complex ([Ru(III)(H2edta)(L1H1)].2H2O). 10 The reaction of anhydrous ferric chloride, L1H2 and Bu4N(OH) in acetonitrile produces a red / brown solution from which red X-ray quality crystals of the dinuclear complex [Fe(III)2(L1H)4Cl2]•2MeCN (2) were obtained. Complex 2 crystallises in the triclinic P-1 space group (Z = 1).…”

Section: (L2)4(no3)2]•3h2omentioning

confidence: 99%

Mono- and ditopic hydroxamate ligands towards discrete and extended network architectures

et al. 2019

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Synthesis, structures and speciation studies of ruthenium(iii) hydroxamate/hydroximato complexes. Crystal and molecular structure of hydrated [Ru(H₂edta)(2-methoxyphenylhydroxamate)], the first structurally characterised ruthenium(iii)–hydroxamate complex

Cited by 15 publications

References 37 publications

Synthesis and characterization of dinuclear (Hedta)Ru(III) complexes with N-heterocyclic ligands: magnetic properties and DNA-binding studies

Synthesis and characterization of dinuclear (Hedta)Ru(III) complexes with N-heterocyclic ligands: magnetic properties and DNA-binding studies

Complexes Formed in Solution Between Vanadium(IV)/(V) and the Cyclic Dihydroxamic Acid Putrebactin or Linear Suberodihydroxamic Acid

Mono- and ditopic hydroxamate ligands towards discrete and extended network architectures

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Synthesis, structures and speciation studies of ruthenium(iii) hydroxamate/hydroximato complexes. Crystal and molecular structure of hydrated [Ru(H2edta)(2-methoxyphenylhydroxamate)], the first structurally characterised ruthenium(iii)–hydroxamate complex

Cited by 15 publications

References 37 publications

Synthesis and characterization of dinuclear (Hedta)Ru(III) complexes with N-heterocyclic ligands: magnetic properties and DNA-binding studies

Synthesis and characterization of dinuclear (Hedta)Ru(III) complexes with N-heterocyclic ligands: magnetic properties and DNA-binding studies

Complexes Formed in Solution Between Vanadium(IV)/(V) and the Cyclic Dihydroxamic Acid Putrebactin or Linear Suberodihydroxamic Acid

Mono- and ditopic hydroxamate ligands towards discrete and extended network architectures

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Synthesis, structures and speciation studies of ruthenium(iii) hydroxamate/hydroximato complexes. Crystal and molecular structure of hydrated [Ru(H₂edta)(2-methoxyphenylhydroxamate)], the first structurally characterised ruthenium(iii)–hydroxamate complex