The redox entity comprising two Schiff base groups attached to a phenyl ring (NCHArHCN) is reported to be active for sodium‐ion storage (Ar=aromatic group). Electroactive polymeric Schiff bases were produced by reaction between non‐conjugated aliphatic or conjugated aromatic diamine block with terephthalaldehyde unit. Crystalline polymeric Schiff bases are able to electrochemically store more than one sodium atom per azomethine group at potentials between 0 and 1.5 V versus Na+/Na. The redox potential can be tuned through conjugation of the polymeric chain and by electron injection from donor substituents in the aromatic rings. Reversible capacities of up to 350 mA h g−1 are achieved when the carbon mixture is optimized with Ketjen Black. Interestingly, the “reverse” configuration (CHNArNHC) is not electrochemically active, though isoelectronic.
Reaction of [Ni(NO)(bipy)(Me2phen)][PF6] with 1 equiv of nitric oxide (NO) in CH2Cl2 results in the formation of N2O and [{(Me2phen)Ni(NO)}2(μ-η(1)-N:η(1)-O)-NO2)][PF6] (3), along with the known complex, [Ni(bipy)3][PF6]2 (4). The isolation of complex 3, which contains a nitrite ligand, demonstrates that the reaction of [Ni(NO)(bipy)(Me2phen)][PF6] with exogenous NO results in NO disproportionation and not NO reduction. Complex 3 could also be accessed by reaction of [Ni(NO)(Me2phen)][PF6] (5) with (Me2phen)Ni(NO)(NO2) (7) in good yield. Complexes 3, 5, and 7 were fully characterized, including analysis by X-ray crystallography in the case of 3 and 7. Furthermore, addition of 0.5 equiv of bipy to [Ni(NO)(bipy)][PF6] results in formation of the hyponitrite complex, [{(bipy)Ni(κ(2)-O2N2)}η(1):η(1)-N,N-{Ni(NO)(bipy)}2][PF6]2 (9), in modest yield. Importantly, the hyponitrite ligand in 9 is thought to form via coupling of two NO(-) ligands and not by coupling of a nucleophilic nitrosyl ligand (NO(-)) with an electrophilic nitrosyl ligand (NO(+)). X-ray crystallography reveals that complex 9 features a new binding mode of the cis-hyponitrite ligand.
Reaction of [Ni(NO)(bipy)][PF6] (2) with AgPF6 or [NO][PF6] in MeCN results in formation of [Ni(bipy)x(MeCN)y](2+) and release of NO gas in moderate yields. In contrast, the addition of the inner sphere oxidant Ph2S2 to 2 does not result in denitrosylation. Instead, the diphenyldisulfide adduct [{(bipy)(NO)Ni}2(μ-S2Ph2)][PF6]2 (3) is formed in good yield. However, oxidation of 2 with 2,2,6,6-tetramethylpiperidine-1-oxyl (TEMPO) does results in cleavage of the Ni-NO bond and generation of NO. The metal-containing product, [(bipy)Ni(η(2)-TEMPO)][PF6] (4), can be isolated as an orange-brown solid in excellent yields. In the solid state, complex 4 contains a side-on bound TEMPO(-) ligand, which is characterized by a long N-O bond length [1.383(2) Å]. The contrasting reactivity of Ph2S2 and TEMPO likely relates to their different redox potentials, as Ph2S2 is a relatively weak oxidant. Finally, the addition of pyridine-N-oxide to 2 results in the formation of the adduct, [(bipy)Ni(NO)(ONC5H5)][PF6] (5). No evidence of NO release is observed in this reaction, probably because of the low one-electron (1e(-)) reduction potential of pyridine-N-oxide.
Objective Both of the above studies aimed to evaluate whether or not low levels of 25-hydroxyvitamin D in pregnancy were associated with an increased risk of developing GDM. The Parlea study measured vitamin D levels in the first trimester between weeks 15 and 18, while the Burris study tested for vitamin D levels during the second trimester between weeks 26 and 28.
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