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Structural Study of Alkaline‐Earth Metal Heterocycles Supported by Triazole‐based Sulfur Ligands
Author(s) -
BalantaDíaz Jhon A.,
MoyaCabrera Mónica,
Jancik Vojtech,
Toscano Rubén A.,
MoralesJuárez T. Jesús,
CeaOlivares Raymundo
Publication year - 2011
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.201100122
Subject(s) - chemistry , salt metathesis reaction , bimetallic strip , metathesis , metal , ligand (biochemistry) , alkaline earth metal , molar ratio , magnesium , salt (chemistry) , alkaline hydrolysis , medicinal chemistry , hydrolysis , inorganic chemistry , sulfur , hydroxide , potassium , organic chemistry , polymerization , catalysis , biochemistry , receptor , polymer
The alkaline earth metal complex [Mg{4,5‐(P(S)Ph 2 ) 2 } 2 tz} 2 (thf) 4 ] ( 2 ) and the bimetallic complexes, [ M {4,5‐(P(S)Ph 2 ) 2 } 2 tz} 2 (thf)] 2 [ M = Ca ( 3 ), Sr ( 4 ), Ba ( 5 )], [SrI{4,5‐(P(S)Ph 2 ) 2 tz} 2 (thf) 3 ] 2 ( 6 ), and [{BaI(4,5‐(P(S)Ph 2 ) 2 tz)} 2 (thf) 7 ] ( 7 ) were prepared in good yields from the metathesis reactions of the potassium salt of 4,5‐bis(diphenylthiophosphoranyl)‐1,2,3‐triazole [H{4,5‐(P(S)Ph 2 ) 2 tz}] ( 1 ) and M I 2 ( M = Ca, Sr, Ba), whereas the tetrametallic magnesium hydroxide [Mg 2 (μ‐OH){4,5‐(P(S)Ph 2 ) 2 } 2 tz} 3 ] 2 ( 8 ) was obtained as the hydrolysis product from the starting material (Mg n BuCl) and 1 . The NMR study of 2 – 8 in solution suggests the formation of solvated species in CD 3 OD‐ d 4, whereas for 4 , 5 , and 6 a fluxional behavior is observed in CD 2 Cl 2 . The structural analyses of 3 – 5 , 6 , and 7 in solid state reveal in all cases a central core defined by M 2 N 4 heterocycle bearing M –S bonding. The degree of aggregation observed for these compounds depends significantly on the size of the metal atom as well as on the metal‐ligand molar ratio employed for each reaction.