TY - JOUR
T1 - Solution and solid-state preparation of 18-crown[6] complexes with M[HSO4]n Salts (M = NH4+, K +, Sr2+ and n = 1, 2) and an investigation of solvation/desolvation processes and crystal polymorphism
AU - Braga, Dario
AU - Gandolfi, Massimo
AU - Lusi, Matteo
AU - Paolucci, Demis
AU - Polito, Marco
AU - Rubini, Katia
AU - Grepioni, Fabrizia
PY - 2007
Y1 - 2007
N2 - 18-Crown[6] ether has been used to prepare a new class of organic-inorganic complexes of general formula 18-crown[6]·M[HSO4]n (where M = NH4+, K+, Sr2+ and n = 1, 2) by reacting directly in solution or in the solid state the crown ether 18-crown[6] with inorganic salts such as [NH4][HSO4], K[HSO4], and Sr[HSO4]2. The structures of 18-crown[6]·[NH4][HSO4]·2H2O (1·2 H2O), 18-crown[6]·[NH4][HSO 4] (1), 18-crown[6]·K[HSO4]·2H2O (2·2 H2O), 18-crown[6]·K[HSO4] (2), and 18-crown[6]·Sr[HSO4]2 (3) have been characterized by single-crystal X-ray diffraction. The reversible water loss in compounds 1·2 H2O and 2·2 H2O leads to formation of the corresponding anhydrous phases 18-crown[6]·[NH4]-[HSO 4] (1), and 18-crown[6]·K[HSO4] (2), which undergo, on further heating, enantiotropic solid-solid transitions very likely associated with the on-set of a solid state dynamical process. Similar high-temperature behavior is shown by 18-crown[6]·Sr[HSO 4]2 (3). The dehydration and phase-transition processes have been investigated by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and variable temperature X-ray powder diffraction.
AB - 18-Crown[6] ether has been used to prepare a new class of organic-inorganic complexes of general formula 18-crown[6]·M[HSO4]n (where M = NH4+, K+, Sr2+ and n = 1, 2) by reacting directly in solution or in the solid state the crown ether 18-crown[6] with inorganic salts such as [NH4][HSO4], K[HSO4], and Sr[HSO4]2. The structures of 18-crown[6]·[NH4][HSO4]·2H2O (1·2 H2O), 18-crown[6]·[NH4][HSO 4] (1), 18-crown[6]·K[HSO4]·2H2O (2·2 H2O), 18-crown[6]·K[HSO4] (2), and 18-crown[6]·Sr[HSO4]2 (3) have been characterized by single-crystal X-ray diffraction. The reversible water loss in compounds 1·2 H2O and 2·2 H2O leads to formation of the corresponding anhydrous phases 18-crown[6]·[NH4]-[HSO 4] (1), and 18-crown[6]·K[HSO4] (2), which undergo, on further heating, enantiotropic solid-solid transitions very likely associated with the on-set of a solid state dynamical process. Similar high-temperature behavior is shown by 18-crown[6]·Sr[HSO 4]2 (3). The dehydration and phase-transition processes have been investigated by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and variable temperature X-ray powder diffraction.
KW - Crown compounds
KW - Crystal polymorphism
KW - Desolvation
KW - Phase transitions
KW - X-ray diffraction
UR - http://www.scopus.com/inward/record.url?scp=34250890758&partnerID=8YFLogxK
U2 - 10.1002/chem.200601850
DO - 10.1002/chem.200601850
M3 - Article
AN - SCOPUS:34250890758
SN - 0947-6539
VL - 13
SP - 5249
EP - 5255
JO - Chemistry - A European Journal
JF - Chemistry - A European Journal
IS - 18
ER -