Gold(I) N-heterocyclic carbene precursors for focused electron beam-induced deposition.
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ABSTRACT:
SUBMITTER: Glessi C
PROVIDER: S-EPMC7991619 | biostudies-literature |
REPOSITORIES: biostudies-literature
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Project description:The synthesis, chemical and physical properties of [{AgO2CCH2OMe} n ] (1) and [{AgO2CCH2OMe(PPh3)} n ] (2) are reported. Consecutive reaction of AgNO3 with HO2CCH2OMe gave 1, which upon treatment with PPh3 produced 2. Coordination compound 2 forms a 1D coordination polymer in the solid state as evidenced by single crystal X-ray structure analysis. The coordination geometry at Ag+ is of the [3 + 1] type, whereby the carboxylate anions act as bridging ligands. The formation of PPh3-Ag(I) coordinative bonds results in distorted T-shaped AgPO2 units, which are stabilized further by an additional O-Ag dative bond. TG and TG-MS measurements show that 1 and 2 decompose at 190-250 °C (1) and 260-300 °C (2) via decarboxylation, involving Ag-P (2), C-C and C-O bond cleavages to give elemental silver as confirmed by PXRD studies. In order to verify if polymeric 2 is suitable as a FEBID precursor for silver deposition, its vapor pressure was determined (p170 °C = 5.318 mbar, ?Hvap = 126.1 kJ mol-1), evincing little volatility. Also EI and ESI mass spectrometric studies were carried out. The dissociation of the silver(I) compound 2 under typical electron-driven FEBID conditions was studied by DFT (B3LYP) calculations on monomeric [AgO2CCH2OMe(PPh3)]. At an energy of the secondary electrons up to 0.8 eV elimination of PPh3 occurs, giving Ag+ and O2CCH2OMe-. Likewise, by release of PPh3 from [AgO2CCH2OMe(PPh3)] the fragment [AgO2CCH2OMe]- is formed from which Ag+ and O2CCH2OMe- is generated, further following the first fragmentation route. However, at 1.3 eV the initial step is decarboxylation giving [AgCH2OMe(PPh3)], followed by Ag-P and Ag-C bond cleavages.
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