113859-76-0Relevant articles and documents
Use of tetra-n-butylammonium permanganate for inorganic syntheses in nonaqueous solvents. Preparation and structure of a manganese(III) dimer containing bridging phenoxo oxygen atoms
Vincent, John B.,Folting, Kirsten,Huffman, John C.,Christou, George
, p. 996 - 999 (2008/10/08)
The use of N-n-Bu4MnO4 for the synthesis of inorganic complexes in nonaqueous solvents is explored. A reaction system leading to the preparation of known Mn(pic)3·H2O (1) (picH = picolinic acid) is described. 1 can be synthesized in high yields (40-70%) by using EtOH, MeCN, DMF, and Me2CO as solvents. With salicylic acid (salH2) in pyridine (pyr) the product, after recrystallization from EtOH/petroleum spirits, is the new compound [Mn(EtOH)4] [Mn2(sal)4(pyr)2] (2). Complex 2 crystallizes in the monoclinic space group P21/n with a = 13.142 (3) A?, b = 16.742 (5) A?, c = 10.842 (2) A?, β= 97.15 (1)°, and Z = 2 at T = -160°C. The anion consists of two Mn(III) atoms bridged by two μ-phenoxo oxygen atoms from salicylate groups whose carboxylates are also bound to the metal. Each Mn(III) additionally contains another salicylate and a pyridine; the dimer has Ci symmetry with each metal octahedrally coordinated. The cation is a Mn(II) atom possessing four EtOH and two trans oxygen ligands, the latter belonging to salicylate carboxyl groups in the anion. The Mn(II) is thus octahedrally coordinated and serves to link the anionic dimers to yield an infinite network in the crystal. 2 is the first example of a structurally characterized Mn(III) dimer containing phenoxide bridges. Magnetic moment measurements in Me2SO yield values of 3.14 μB/Mn(III), indicating that the dimer remains intact in solution and that the two d4 Mn(III) atoms are antiferromagnetically coupled.