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
Urotropinium nitrate, N-methylurotropinium azide, dinitramide and azotetrazolate salts have been prepared and fully characterized by analytical and spectoscopic ( 1 H, 13 C, 14 N NMR, IR, Raman) methods. The structures of all four compounds have been determined using X-ray diffraction techniques and represent Synthese, Charakterisierung und Kristallstrukturen von verschiedenen energiereichen Urotropinsalzen mit Azid-, Nitrat-, Dinitramid-und Azotetrazolat-GegenionenInhaltsübersicht. Urotropinnitrat, N-methylurotropinazid, -Dinitramid-und -Azotetrazolat-Salze wurden dargestellt und analytisch und spektroskopisch ( 1 H-, 13 C-, 14 N-NMR, IR, Raman) charakte-
The use of a strategy combining ligand design and changes of reaction conditions has been investigated with the goal of directing the assembly of mononuclear, dinuclear, tetranuclear, and polymeric copper(II) complexes. As a result, closely related copper monomers, alkoxo dimers, and hydroxo cubanes, along with a carbonate-bridged polymeric species, have been synthesized using the rigid, aliphatic amino ligands cis-3,5-diamino-trans-hydroxycyclohexane (DAHC), cis-3,5-diamino-trans-methoxycyclohexane (DAMC), and the glutaryl-linked derivative glutaric acid bis-(cis-3,5-diaminocyclohexyl) ester (GADACE). The composition of the monomeric complex has been determined by X-ray crystallography as [Cu(DAHC)2](ClO4)2 (1), the two dimers as [{Cu(DAHC)(OMe)}2](ClO4)2.MeOH (2) and [{Cu(DAMC)(OMe)(ClO4)}2] (3), the three Cu4O4 cubanes as [{Cu(DAHC)(OH)}4](ClO4)(4).2.5MeOH (4), [{Cu(DAMC)(OH)}4](ClO4)4.H2O (5), and [{Cu2(OH)2(GADACE)}2]Cl4.2MeOH.6H2O (6), and an infinite-chain structure as [{Cu(DAHC)(CO3)}n] (7). Furthermore, the cubane structures 4 and 5 have been investigated magnetically. Our studies indicate that formation of the monomeric, dimeric, and tetranuclear DAHC and DAMC complexes can be controlled by small changes in reaction conditions and that further preorganization of the ligand moiety by linking the DAHC cores (GADACE) allows more effective direction of the self-assembly of the Cu4O4 cubane core.
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