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6 protocols using 2 2 6 2 terpyridine

1

Terpyridine Compound Electrochemical Characterization

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Unless otherwise noted, all solvents were purchased from Carlo Erba. Hexadistilled mercury was purchased from Ophram and annealed platinum wire was purchased from Alfa Aesar. Anhydrous N,N-dimethylformamide, cobalt(ii) chloride, tetra-n-butylammonium hexafluorophosphate (TBAPF6), sodium methoxide, glacial acetic acid, ammonium hexafluorophosphate, 4′-chloro-2,2′:6′,2′′-terpyridine, 4′-(4-chlorophenyl)-2,2′:6′,2′′-terpyridine, 4,4′,4′′-tri-tert-butyl-2,2′:6′,2′′-terpyridine, 4′-(4-methylphenyl)-2,2′:6′,2′′-terpyridine and 2,2′:6′,2′′-terpyridine of the highest purity available were purchased from Sigma-Aldrich and used as received. 4′-Methoxy-2,2′:6′,2′′-terpyridine and compounds 1–5 were synthesized according to modified literature procedures.40 (link)–42 All electrochemical data were referenced to the potential of the Fc+/Fc couple in the solvent system used and the IUPAC convention was used to report current.
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2

Fabrication of Lithium-Ion Solid Electrolyte

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All chemicals and solvents were used as received without further purification. Titanium foil (99.5%, 100 μm in thickness), copper foil (99.9%, 30 μm in thickness), and copper mesh were purchased from Nilaco Corporation. Iron(ii) chloride tetrahydrate (FeCl2·4H2O, 98%), ammonium tetrafluoroborate (NH4BF4, 97%), 4,4′-bipyridine, 2,2′:6′,2′′-terpyridine (98%), 1-iodohexane, bis(trifluoromethane) sulfonimide lithium salt (LiTFSI, 99.95%), and lithium metal were purchased from Sigma-Aldrich. The Li+-ion solid electrolyte was purchased from Ohara Corporation. Ethylene carbonate (EC, water content < 30 ppm) and dimethyl carbonate (DMC, water content < 30 ppm) were obtained from Kishida Chemicals. The polyvinylidene fluoride (PVDF) binder was obtained from MTI Corporation. N-Methyl-2-pyrrolidone (NMP) was obtained from J&K Chemicals. Super P carbon was obtained from TIMCAL.
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3

Synthesis and Characterization of Metal Complexes

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The following chemicals were purchased and used as received: 1,3-diphenylpropane-1,3-dione (98%, Sigma-Aldrich), 2,4-pentanedione (99%, Acros Organics), 2,2,6,6-tetramethyl-3,5-heptanedione (97%, Combi-Blocks) and 2,2’;6’,2”-terpyridine (98%, Sigma-Aldrich). Solvents used in air were used without further purification unless otherwise stated. Solvents used in the glovebox were dried following a previously published procedure prior to use.27 The CD3CN used in 1H NMR experiments was dried using molecular sieves. 2,6-bis(2’-benzimidazolyl)pyridine (BBP) was prepared following the literature procedure.28 (link) Manipulations performed under an inert N2 atmosphere were conducted in a MBraun Unilab glovebox.
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4

Potentiometric Study of Inositol Phosphate Complexation

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All chemicals were purchased from commercial sources and used without further purification. Mn(ClO4)2•6H2O (Alfa Aesar, >99%) was used as metal source for the synthesis; MnCl2•4H2O (Sigma, >99%) was used for potentiometric measurements. 2,2´:6´2´´-terpyridine (98%) was supplied from Sigma-Aldrich. The dipotassium salt of InsP6, K2H10L•2.5 H2O, was purchased from Sigma-Aldrich and its purity was rechecked by elemental and thermogravimetric analyses. Methanol and ethanol (99%) were obtained from Dorwill. All aqueous solutions were prepared with ultrapure water obtained from a Millipore-MilliQ plus system (up to 18 M cm -1 ) and used immediately after preparation. The ionic strength was adjusted to 0.15 M with NMe4Cl or NaClO4 (Fluka). The standard HCl solutions were prepared by diluting Merck standard ampoules. The titrant solution (0.1 M NMe4OH in 0.15 M NMe4Cl) was prepared by dissolving NMe4OH•5H2O (Fluka), and was standardized with potassium biphthalate. Mn(II) solutions were standardized according to standard techniques. [32]
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5

Cobalamin Complexation with Palladium

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Cyanocobalamin (CblCN), hydroxocobalamin hydrochloride (CblOH∙HCl), palladium(II) chloride, 2,2′:6′,2′-terpyridine, TRIS base and potassium cyanide-15N (KC15N), were obtained from Merck (Sigma-Aldrich, MI, USA). Ammonium tetrachloropalladate(II) was purchased from Alfa Aesar. Methanol (MeOH) and acids (hydrochloric acid 35–38%, nitric acid 65% and perchloric acid 70%) were obtained from Chempur. All chemicals were of at least analytical grade.
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6

Ruthenium-Catalyzed Redox Reactions

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All chemicals were of analytical reagent grade and used without further purification. RuCl3·xH2O was purchased from Abcam. 2-(Aminomethyl)pyridine, 2,2′:6′,2′′-terpyridine, 2,2′-bipyridine, lithium chloride, methanol-d4, deuterium oxide, sodium formate-d, β-nicotinamide adenine dinucleotide sodium salt, and MES sodium salt, were obtained from Merck. Sodium formate, sodium tetrahydroborate, and solvents were purchased from Avantor Performance Materials Poland SA. Deionized water was obtained from a Millipore Milli-Q water reagent system (Millipore, Bedford, MA, USA).
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