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

被引:33
作者
Braga, Dario [1 ]
Gandolfi, Massimo [1 ]
Lusi, Matteo [1 ]
Paolucci, Demis [1 ]
Polito, Marco [1 ]
Rubini, Katia [1 ]
Grepioni, Fabrizia [1 ]
机构
[1] Univ Bologna, Dipartimento Chim G Ciamician, I-40126 Bologna, Italy
关键词
crown compounds; crystal polymorphism; desolvation; phase transitions; X-ray diffraction;
D O I
10.1002/chem.200601850
中图分类号
O6 [化学];
学科分类号
0703 ;
摘要
18-Crown[6] ether has been used to prepare a new class of organic-inorganic complexes of general formula 18-crown[6]center dot 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]center dot[NH4][HSO4]center dot 2H(2)O (1 center dot 2H(2)O), 18-crown[6]center dot[NH4][HSO4] (1), 18-crown[6]center dot K[HSO4]center dot 2 H2O (2 center dot 2H(2)O), 18-crown [6]center dot K[HSO4] (2), and 18-crown [6]center dot Sr[HSO4](2) (3) have been characterized by single-crystal X-ray diffraction. The reversible water loss in compounds 1 center dot 2H(2)O and 2 center dot 2H(2)O leads to formation of the corresponding anhydrous phases 1.8-crown[6]center dot[NH4][HSO4] (1), and 18-crown[6]center dot 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]center dot Sr[HSO4](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.
引用
收藏
页码:5249 / 5255
页数:7
相关论文
共 41 条
[1]   Laying traps for elusive prey: Recent advances in the non-covalent binding of anions [J].
Atwood, JL ;
Holman, KT ;
Steed, JW .
CHEMICAL COMMUNICATIONS, 1996, (12) :1401-1407
[2]  
Bernstein J., 2002, Polymorphism of molecular crystals
[3]   Inorganic crystal engineering using self-assembly of tailored building-blocks [J].
Blake, AJ ;
Champness, NR ;
Hubberstey, P ;
Li, WS ;
Withersby, MA ;
Schröder, M .
COORDINATION CHEMISTRY REVIEWS, 1999, 183 :117-138
[4]   Mechanochemical preparation of molecular and supramolecular organometallic materials and coordination networks [J].
Braga, D ;
Giaffreda, SL ;
Grepioni, F ;
Pettersen, A ;
Maini, L ;
Curzi, M ;
Polito, M .
DALTON TRANSACTIONS, 2006, 6 (10) :1249-1263
[5]   Unprecedented mechanochemical preparation of 18Crown[6] and 15Crown[5] adducts of ammonium hydrogen sulfate by grinding or kneading [J].
Braga, D ;
Curzi, M ;
Lusi, M ;
Grepioni, F .
CRYSTENGCOMM, 2005, 7 :276-278
[6]   Crystal engineering, where from? Where to? [J].
Braga, D .
CHEMICAL COMMUNICATIONS, 2003, (22) :2751-2754
[7]   Reactions between or within molecular crystals [J].
Braga, D ;
Grepioni, F .
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION, 2004, 43 (31) :4002-4011
[8]   Hydrogen bonding interactions between ions: A powerful tool in molecular crystal engineering [J].
Braga, D ;
Maini, L ;
Polito, M ;
Grepioni, F .
SUPRAMOLECULAR ASSEMBLY VIA HYDROGEN BONDS II, 2004, 111 :1-+
[9]   New trends in crystal engineering [J].
Braga, D ;
Brammer, L ;
Champness, NR .
CRYSTENGCOMM, 2005, 7 :1-19
[10]   Crystal engineering and organometallic architecture [J].
Braga, D ;
Grepioni, F ;
Desiraju, GR .
CHEMICAL REVIEWS, 1998, 98 (04) :1375-1405