Tetraamminecopper(2 ) bis(permanganate) ([Cu(NH 3 ) 4 ](MnO 4 ) 2 ; 1) was prepared, and its properties were studied in both aqueous solution and the solid phase. The presence of H-bond interactions between the ammonia ligand of the complex cation and an O-atom of the permanganate ion was detected by IR and Raman methods. The solid-phase thermal deammoniation of 1 led to an unusual intramolecular redox reaction between the MnÀO ¥¥¥ HÀN linkage with formation of NH 4 NO 3 and CuMn 2 O 4 -type mixed oxides instead of stepwise deammoniation, even below 1008. The thermal deammoniation of 1 in aqueous solution led, instead of to hydrated copper(2 ) bis(permanganate), to the formation of NH 4 MnO 4 (2). Since the temperature of the thermal deammoniation of 1 is lower than the decomposition temperature of the permanganate ion, the regulated solid-phase decomposition of 1 allowed preparation of CuMn 2 O 4 -type oxides with mixing of copper and manganese at the atomic level.
A widely used oxidizing agent in organic chemistry with an assumed structure of '[Ag(py)2]MnO4' and its perchlorate and perrhenate analogues are studied. Their synthesis in pure form is challenging. In order to clarify the chemical nature of known compounds and find routes to new derivatives, a systematic study is presented for the synthesis of [Ag(py)n]XO4 (X= Mn, Cl, Re, n=2-4) complexes. Ten complexes including four new derivatives, namely [Ag(py)4]MnO4, [Ag(py)4]MnO4•4[Ag(py)2]MnO4, [Ag(py)2]ClO4•0.5py, and [Ag(py)2]ReO4 are synthesized and characterized. The chemical identity of 'Ag(py)2MnO4' is also clarified. A novel route to prepare [Ag(py)2]MnO4 is developed. The reaction of AgXO4 salts with neat pyridine followed by various crystallization techniques is used to prepare [Ag(py)2]XO4, [Ag(py)4]XO4, [Ag(py)4]XO4•4[Ag(py)2]XO4 and [Ag(py)2]XO4•0.5py (X=Cl, Mn), complexes. The solid phase structure of [Ag(py)2]MnO4•0.5py is determined (a=19.410 Å, b=7.788 Å, c=21.177 Å, =104.20°, C2/c (15), Z=4(8)). [Ag(py)2] + cations in the crystal form dimeric units where silver ions are connected by oxygen atoms of two MnO4anions. The Ag…Ag distance is indicative of argentophilic interaction. The pyridine ring … interactions contribute to the stability of the crystal lattice.
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