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Ammonothermal Synthesis of Alkali N , N′ ‐Bis(aminocarbonyl)phosphorodiamidates M[PO 2 (NHCONH 2 ) 2 ] (M = Na, K, Rb)
Author(s) -
Wirnhier Eva,
Boller Ruth Deborah,
Schnick Wolfgang
Publication year - 2012
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.201200209
Subject(s) - chemistry , alkali metal , thermogravimetric analysis , thermal decomposition , context (archaeology) , differential thermal analysis , autoclave , crystallography , ion , x ray crystallography , inorganic chemistry , crystal structure , decomposition , powder diffraction , diffraction , nuclear chemistry , organic chemistry , paleontology , physics , optics , biology
Compounds M[PO 2 (NHCONH 2 ) 2 ] with M = Na, K, and Rb, which are the salts of N , N′ ‐bis(aminocarbonyl)phosphorodiamidic acid, were synthesized by ammonolysis of the corresponding alkali biuretooxophosphates M[PO 2 (NH) 3 (CO) 2 ] (M = Na, K, Rb) at 350 °C and 120–150 bar in an autoclave. The structures were solved by single‐crystal X‐ray diffraction and exhibit 3D frameworks in which N , N′ ‐bis(aminocarbonyl)phosphorodiamidate ions connect the corresponding alkali ions. The thermal behavior was investigated by combined thermogravimetric (TG) and differential thermal analysis (DTA) as well as temperature‐dependent powder X‐ray diffraction to evaluate applicability of the alkali N , N′ ‐bis(aminocarbonyl)phosphorodiamidates as precursors for the synthesis of CNP(O) networks. In this context, the concept of Le Chatelier's principle for the hindrance of premature decomposition by applying elevated pressure was examined.