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Chapter 7 173
7.3 Experimental data on chapter 4
Ruthenium SBU precursor [Ru2(OOCCH3)4Cl]n [202] as well as the parent single-linker Ru-
MOF [82, 198] were prepared following procedures previously described in the literature and
in Chapter 7.2. All other reagents were available commercially and used without further
purification. Before further manipulations, all activated samples were stored in a glovebox
under inert Ar atmosphere.
7.3.1 Synthesis of Ru-DEMOF samples (1a-1d, 2a-2d, 3a-3d, 4a-4c)
[Ru3(BTC)2-x(5-X-ip)xXy]n (X = counter ion; 0.1 ≤ x ≤ 1; 0 ≤ y ≤ 1.5). The samples were
synthesized according to the reported method [138] applying the so-called controlled SBU
approach. The mixtures of parent linker (1,3,5-benzenetricarboxylic acid, i.e. H3BTC) and
defective linker (5-X-isophthalic acid, i.e. 5-X-ip, X = OH (1), H (2), NH2 (3) and Br (4),
respectively) combined with 1.5 molar equivalents of [Ru2(OOCCH3)4Cl]n (0.36 mmol,170
mg) were placed in the 20 ml Teflon vessels. Subsequently, 4 ml of HPLC grade water and
0.7 ml of glacial acetic acid were added. The molar ratios and amounts of the linkers used
in the starting materials are listed in the Table 7.3. The Teflon reaction vessels were then
placed in the Teflon-lined stainless steel autoclaves. The autoclaves were further sealed
and placed into the pre-heated oven at 433 K for 72 h. Afterwards the autoclaves were
taken out and cooled down at room temperature. The resulting powder products were
collected by centrifugation. Afterwards, they were soaked into HPLC grade water (ca. 20
ml) and the solvent was refreshed by the same water amount every 24 hours for 3 times.
Finally, the solvent was removed and collected powders were dried under air at room
temperature. The activation of the solids was performed by heating at 423 K for 24 h
under dynamic vacuum (ca. 10 -3 mbar).