The literature known, but not fully characterized, silver dinitramide transfer reagents AgN(NO 2 ) 2 (1), [Ag(NCCH 3 )]-[N(NO 2 ) 2 ] (2), and [Ag(py) 2 ][N(NO 2 ) 2 ] (3) have been investigated by 109 Ag, 14 N NMR and vibrational spectroscopy (IR, Raman). In addition, the poorly understood [Cu(NH 3 ) 4 ][N(NO 2 ) 2 )] 2 (4) and [Pd(NH 3 ) 4 ][N(NO 2 ) 2 ] 2 , (5) have also been prepared and characterized by 14 N NMR and vibrational spectroscopy (IR, Raman).
Synthese, Charakterisierung und Kristallstrukturen von Cu-, Ag-und Pd-DinitramidsalzenInhaltsübersicht. Die aus der Literatur bekannten, aber nicht völlig charakterisierten Silberdinitramid-Transferreagenzien AgN(wurden mittels 109 Ag-, 14 N-NMR und IR-sowie Raman-Spektroskopie 1) present address: Glasgow, untersucht. Ferner wurden die wenig verstandenen Verbindungen [Cu(NH 3 ) 4 ][N(NO 2 ) 2 )] 2 (4) und [Pd(NH 3 ) 4 ][N(NO 2 ) 2 ] 2 (5) dargestellt und charakterisiert ( 14 N-NMR, IR, Raman). Die Strukturen von 2 Ϫ 5 wurden röntgenographisch bestimmt. dinitramide transfer reagents [5]. AgN(NO 2 ) 2 (1), [Ag(NCCH 3 )][N(NO 2 ) 2 ] (2) and [Ag(py) 2 ][N(NO 2 ) 2 ] (3) were first prepared by Lykanov [1], however, these compounds were only characterized by elemental analysis and melting point. Therefore, we have undertaken the first extensive study of 1Ϫ3, in order to fully characterize these salts and furthermore to investigate their ability to act as dinitramide transfer reagents. Characterization included 109 Ag, 14 N NMR, vibrational spectroscopy (IR, Raman) and X-ray diffraction studies (of 2 and 3 only). The only heavy metal dinitramide salts which have been studied using X-ray diffraction techniques so far are fac-[Re(bpy)-(CO) 3 N 3 O 4 ] [6], hexaaquomanganese and hexaaquozinc dihydrate dinitramide [7]. Therefore, due to the surprisingly interesting structure of 2, [Cu(NH 3 ) 4 ][N(NO 2 ) 2 )] 2 (4) [1] and [Pd(NH 3 ) 4 ][N(NO 2 ) 2 ] 2 , (5) have also been prepared and characterized by 14 N NMR, vibrational spectroscopy (IR, Raman) and X-ray diffraction studies .
Results and Discussion
Preparation and spectroscopic characterizationAll compounds, with the exception of [Cu(NH 3 ) 4 ]-[N(NO 2 ) 2 ] 2 (4), were prepared by a metathesis reaction using KN(NO 2 ) 2 . 4 was prepared by the reaction of