resolver

Intensity, a. u.
110 Chapter 4
as-synthesized samples D2-D4_as (Figure 4.41) disappear after samples activation (i.e.
heating under vacuum). Thus, the origin of these reflections might come from coordinated
solvent molecules, which under employed activation conditions are subsequently
removed. FT-IR spectra of all activated Cu-DEMOFs samples do not vary from the FT-IR
spectrum of the parent Cu-BTC, displaying also overlapping of the characteristic bands of
ip and BTC (Figure 4.42). However, the typical νs(COO) and νas(COO) bands of
carboxylates are observed at around 1442 cm -1 and 1366 cm -1 , respectively. Moreover, the
absence of [BF4] - (from the used Cu-salts) is confirmed, as no ν(B–F) band was found at
1073 cm –1 . [208]
D4_as
D3_as
D2_as
D1_as
Cu-BTC_sim.
5 10 15 20 25 30
2, degree
Figure 4.41. PXRD patterns of the as-synthesized Cu-DEMOF samples D1-4_as in comparison
with the patterns simulated from the single-crystal XRD data of the reported [Cu 3 (BTC) 2 ] n (Cu-
BTC_sim). Metal source: Cu(BF 4 ) 2 6H 2 O. Solvent used for synthesis of D1 and D2 (blue patterns):
DMF; for D3 and D4 (red patterns): EtOH.