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4 protocols using ethanedithiol

1

Solid-Phase Peptide Synthesis Protocol

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Rink amide ChemMatrix® resin, Oxyma, and all other Fmoc-protected amino acids were purchased from Novabiochem®, Sigma-Aldrich (St. Louis, MO, USA). 2-(6-Chloro-1H-benzotriazole1-yl)-1,1,3,3-tetramethylaminium hexafluorophosphate (HCTU) was purchased from Chem Impex International (Wood Dale, IL, USA). Piperidine and ethanedithiol (98+%) were purchased from Alfa Aesar (Tewksbury, MA, USA). Trifluoroacetic acid (TFA, 97%), anisole (99%), thioanisole (≥99%), 4-(2-hydroxyethyl)-1-piperazineethanesulfonic acid (HEPES) and dopamine hydrochloride (H8502, ≥98%) were purchased from Sigma Aldrich (St. Louis, MO, USA). N,N′-Diisopropylcarbodiimide (DIC, 99%), N,N-Diisopropylethylamine (DIEA), Dimethylformamide (DMF, 99.9%), Dichloromethane (DCM, ≥99.8%), Diethyl ether and acetonitrile were purchased from Fisher Scientific (Fisher Scientific, Fairlawn, NJ, USA).
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2

Synthesis of Metal-Organic Coordination Complexes

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Triethylamine, activated carbon (AC), 4-vinylbenzyl chloride (pCMS), and ethanedithiol were purchased from Alfa Aesar (China). Cu(NO3)2·3H2O, benzene tricarboxylic acid (BTC), 2,2′-azobis(2-methylpropionitrile) (AIBN), K2Pt(CN)4, K3Co(CN)6, CuCN, and K3Fe(CN)6 were purchased from Sigma-Aldrich. All other reagents used in this study were commercially available analytical-grade reagents. Cu(CN)32− was prepared according to literature report [11 (link)]. The metal salts were mixed together in water as needed.
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3

Synthesis of Thermoresponsive Hydrogel

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N-Isopropylacrylamide (NIPAm, ≥98%) was acquired from Polysciences Inc. (Warrington, PA). Dialysis membrane tubing was purchased from Spectrum Laboratories (Dominguez, CA). (1H-benzotriazole-1-yl)-1,1,3,3-tetramethyluronium hexafluorophosphate (≥98%, HBTU), N-hydroxybenzotriazole (>97%, HOBT), N,N’-methylenebisacrylamide (99%, MBA), sodium dodecyl sulfate (SDS; 10% w/v in water), 2- acrylamido-2-methyl-1-propanesulfonic acid (99%, AMPSA), dithiothreitol (98%, DTT), fluorescein o-acrylate (98%), N,N-Diisopropylethylamine (99%, DIPEA), potassium persulfate (99%, K2S2O8), N,N’-bis(acryloyl)cystamine (98%, BAC), trifluoroacetic acid and dimethyl sulfoxide (DMSO) were acquired from Sigma-Aldrich (St. Louis, MO). NIPAm, MBA, and AMPSA were stored under nitrogen at 4°C. Acrylate-PEG2000 was purchased from Laysan Bio (Arab, AL). Triisopropyl silane was purchased from TCI America (Boston, MA), and ethane dithiol was purchased from Alfa Aesar (Ward Hill, MA). All water used in synthesis, dialysis, and testing was treated by a Millipore Milli-Q system (Billerica, MA; 18.2 MΩ•cm resistivity).
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4

Fabrication of Platinum Scanning Probe Tips

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Materials. All chemicals were reagent grade and were used as received. All solutions were prepared in mesitylene (99%, Aladdin). Ethanedithiol (C2), butanedithiol (C4), hexanedithiol (C6), octanedithiol (C8), decanedithiol (C10) were purchased from Alfa Aesar. 0.25 mm platinum wire (99.99%) was purchased from Tianjing Lucheng Metal. A ready-to-use fewlayer graphene (10 mm ×10 mm) on top of a nickel layer was purchased from the Graphene Supermarket, US. Tip preparation. Pt tips were prepared using electrochemistry etching previously reported. 28 Briefly, the procedure was divided into two steps. In the first step, the Pt wire was ultrasonically cleaned in acetone for 10 mins. Then a piece of ~15 mm long Pt wire was cut and immersed into a calcium chloride electrolyte with a concentration of 30 wt. %. The amount of wire immersed into the solution was approximately 2-3 mm. An AC voltage of 35 V was applied between the platinum and graphite counter electrode. After 90 s, for the second stage the voltage was then reduced to 18 V for fine etching in order to sharpen the tips. The etching reaction stopped automatically when the platinum wire section immersed the electrolyte broke off.
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