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High‐Yield Synthesis and Crystal Structure Determination of Sodium Triphenylphosphane Monosulfonate (TPPMS Na )
Author(s) -
Karschin Arndt,
Kläui Wolfgang,
Peters Wilfried,
Spingler Bernhard
Publication year - 2010
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/ejic.200901002
Subject(s) - chemistry , yield (engineering) , anhydrous , thermogravimetric analysis , sodium , thermal decomposition , salt (chemistry) , sulfonate , crystal structure , sodium salt , nuclear chemistry , inorganic chemistry , organic chemistry , materials science , metallurgy
A simple, high‐yield synthesis is described that leads tothe sodium salt of monosulfonated triphenylphosphane (TPPMS Na ) as a pure product in large quantities without complicated workup techniques. The single‐crystal X‐ray structure of TPPMS Na · 2.5H 2 O is reported. The structure is built up by alternating layers of aquated sodium sulfonate units and hydrophobic triphenyl units. Thermogravimetric analyses show the loss of one molecule of water at 70 and one at 105 °C. Thermal decomposition occurs at temperatures above 400 °C. The anhydrous ligand is hygroscopic. The preparation of the free acid TPPMS H starting from the sodium salt is also reported. TPPMS H is an extremely hygroscopic solid that could not be isolated in the crystalline form.