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Chapter 5 127<br />

(Figure 5.3). This is probably due to the rather small particle size of these Pd NPs and,<br />

therefore, hard to be detected by PXRD technique. Finally, it should be pointed out, that<br />

employing equal molar amounts of Cu- and Pd-salts or only Pd-precursor in the starting<br />

reaction mixtures, formation of only metal/metal-oxide products has been observed<br />

(Figures 7.25 and 7.26).<br />

Figure 5.4. PXRD patterns of the as-synthesized Pd@[Cu 3-X Pd x (BTC) 2 ] n in comparison with<br />

simulated patterns of the non-doped Cu-BTC.<br />

Table 5.1. Calculated cell parameters of the Cu/Pd-BTC_1-3 (TOPAS academic software and<br />

Pawley method [287] have been employed) in comparison with that obtained from the single crystal<br />

data of the reported [Cu 3 (BTC) 2 ] n . [35]<br />

Sample a (Å) V (Å 3 ) Space group R wp R exp<br />

[Cu 3 (BTC) 2 ] [35] n 26.343 18280 Fm-3m - -<br />

Cu/Pd-BTC_1 26.308 18208 Fm-3m 6.018 4.79<br />

Cu/Pd-BTC_2 26.305 18203 Fm-3m 6.618 5.17<br />

Cu/Pd-BTC_3 26.293 18178 Fm-3m 7.201 6.09

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