Matrix-isolation studies of alkali-metal and thallium perrhenates. IR spectrum of oxygen-18 enriched thallium perrhenate and dimerization of the MReO4 species

Ion‐ and Liquid‐Assisted Grinding: Improved Mechanochemical Synthesis of Metal–Organic Frameworks Reveals Salt Inclusion and Anion Templating

“…The inclusion of NH 4 ReO 4 and NaReO 4 in 1 b is evident by the absence of salt reflections in the PXRD pattern and by the appearance of a new absorption band at 910 cm −1 in the FTIR spectra (Figure 3 b). This band does not appear in 1 a or 1 b prepared using other salts, and is consistent with one of four ReO 4 − vibrational modes expected between 840 and 980 cm −1 21. In pure salts this band is broadened by coupling to lattice vibrations and we interpret its sharpening as anion inclusion in 1 b .…”

The development of a combined simultaneous XAFS/FTIR facility for the study of matrix species

“…Fig. 2 shows the Re L3-edge XANES and FTIR spectra recorded simultaneously during deposition of RbReO 4 into a solid N 2 matrix at l0 K. The IR spectra are shown for the Re-O stretching region, and are in very good agreement with those published previously (Bencivenni, 1984). The only other significant features in the IR spectra were from the ubiquitous matrix isolated H20 , CO 2 and CO that are always present in such experiments.…”

“…The perrhenate anions have been studied by both matrix isolation IR (Beneivenni et al, 1979(Beneivenni et al, , 1984Arthers et al, 1983) and by vapour phase electron diffraction (Spridonov et al, 1965;Roddatis et al, 1973;Petrov et al, 1980), therefore we decided to use RbReO 4 as a test example for the new apparatus. Whilst the matrix IR spectrum (Bencivenni et al, 1984;Arthers et al, 1983) of this has been reported, the ED data was only available for CsReO4 (Petrov et al, 1980) and T1ReO 4, (Roddatis et al, 1973) and that for KReO4 (Spridonov et al, 1965) was very poor. The IR and ED data both indicate that the structure of these molecular species have C2v symmetry with bidentate coordination of the Rb.…”

“…The only other significant features in the IR spectra were from the ubiquitous matrix isolated H20 , CO 2 and CO that are always present in such experiments. On the basis of previous 180 enrichment studies (Arthers, 1983;Bencivenni, 1984) the bands are assigned as: 970.0 cm l ( vA, terminal), 941.1 cm -1 ( vs~ terminal), 914.6 cm "1 (vA, bridging), 893.6 cm -z (vs, bridging). The other very low intensity bands are probably due to small traces of dimeric species also trapped in the matrix, thus indicating the usefulness of combined in-situ FTIR monitoring in identifying the species under investigation.…”

Ion‐ and Liquid‐Assisted Grinding: Improved Mechanochemical Synthesis of Metal–Organic Frameworks Reveals Salt Inclusion and Anion Templating

“…This band does not appear in 1 a or 1 b prepared using other salts, and is consistent with one of four ReO 4 À vibrational modes expected between 840 and 980 cm À1 . [21] In pure salts this band is broadened by coupling to lattice vibrations and we interpret its sharpening as anion inclusion in 1 b. Inclusion of NaReO 4 , NaCl, and Na 2 S 2 O 3 in MOFs is also inferred from the 23 Na MAS NMR spectra of ILAG products, which differ from those of pure salts (Figure 3 c).…”