Ammonothermal Synthesis of Alkali N,N '-Bis(aminocarbonyl)phosphorodiamidates M[PO2(NHCONH2)2] (M = Na, K, Rb)

作者：Wirnhier Eva; Boller Ruth Deborah; Schnick Wolfgang^*

来源：European Journal of Inorganic Chemistry, 2012, (20): 3296-3301.

DOI：10.1002/ejic.201200209

• Ammonothermal synthesis
• Alkali metals
• High-pressure chemistry
• X-ray diffraction
• Thermal behavior

Compounds M[PO2(NHCONH2)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[PO2(NH)3(CO)2] (M = Na, K, Rb) at 350 degrees C and 120150 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.

• 出版日期2012-7