Untitled

Abstract

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

Synthesis and Characterization of Various Photosensitive Copper(II) Complexes with 5‐(1‐Methylhydrazinyl)‐1H‐tetrazole as Ligand and Perchlorate, Nitrate, Dinitramide, and Chloride as Anions

“…A broad absorption band at 2934 cm À1 can be assigned to the C À H valence vibrations of the methyl group. [18] The HMHT vibrations of complex 8 are similar to those discussed above. [21] The according vibrations of the HMHT ligand are shifted upon complexation to higher wavenumbers for the neutral form and to lower wavenumbers for the deprotonated MHT ligand (Figure 9).…”

“…with literature values. [18] The crystal water forms a large set of hydrogen bonds ( Figure S4 in the Supporting Information) to the dinitramide anion and the MHT ligand. The complex dimers are further interconnected through hydrogen bonds between the MHT and HMHT ligands to form a 3D network ( Figure S4 in the Supporting Information).…”

“…[18] The crystal water forms a large set of hydrogen bonds ( Figure S4 in the Supporting Information) to the dinitramide anion and the MHT ligand. [18] The crystal water forms a large set of hydrogen bonds ( Figure S4 in the Supporting Information) to the dinitramide anion and the MHT ligand.…”

Synthesis and Application of Trimethylsilyl Dinitramide Me3SiN(NO2)2 as Dinitramide Transfer Reagent; Preparation of Covalent Organotellurium(IV) Dinitramides

“…Starting from the corresponding dichlorides R 2 TeCl 2 , the reaction with silver dinitramide or its pyridine or acetonitrile solvates [19,21] resulted in the formation of the corresponding organotellurium(IV) dinitramides (4) (1)…”

“…Silver dinitramide reagents [19,21] and organotellurium(IV) dihalogenides R 2 TeX 2 (R = Me, Ph, Mes; X = F, Cl) [26] were prepared according to literature procedures. Evaporation of all volatile materials resulted in the formation of nitrous gases and a remaining brownish solid, which could not be identified.…”