IOR Chemco (Norway)

MIL-101(Cr), one of the most important prototypical MOFs, is well investigated and widely used in many scientific fields. With regard to MOF synthesis in general, the addition of a modifier is commonly used to improve the properties of the products. The effect of inorganic (mineral) and organic acid modifiers was thoroughly investigated in the synthesis of MIL-101(Cr) and HNO3 could increase the yield to over 80% of a product with average SBET > 3200 m(2) g(-1) in repeated experiments (from an average of 50% in most published syntheses) in small-scale laboratory synthesis. The large-scale synthesis could use the finding of HNO3 addition and produce MIL-101(Cr) in >100 g quantities with yields near 70% and BET-surface areas near 4000 m(2) g(-1). The addition of acetic acid (CH3COOH) together with seeding could decrease the reaction temperature, the lowest being 160 °C (from typically 220 °C in published procedures), with still relatively good yield and BET surface area of the product. The use of other strong inorganic or weak carboxylic acids as modulators typically caused a decrease in yield and porosity.

Part III is divided into two chapters—Chaps. 4 and 5. These chapters are the most important for those who want to become proficient in the routine application of CASE analysis for solving structural problems which appear in analytical laboratories. Here CASE-based solutions to 66 real-world structural problems are fully explained. Spectroscopic data for the problems were adopted mainly from Organic Letters and Journal of Natural Products, the corresponding articles being published in recent years (2011–2013). For computer-based structure elucidation, the problems we selected were primarily related to molecules possessing unique or unprecedented skeletons. Spectroscopic data for these problems are also (as described in Chap. 3) available in the form of electronic tables coded in the formats needed by Structure Elucidator. The student therefore has the possibility to repeat the solutions described in Part III and perform additional computational experiments to follow how the results change depending on the composition of the initial axiom set. This chapter describes 33 real-world problems which are solved using strict structure generation. This program mode assumes that all HMBC and COSY correlations are of “standard” lengths corresponding to the coupling constants 2−3 J CH and 2−3 J HH correspondingly.