Pyridine and imidazole are connected by an azo group (
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N
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N
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) to synthesize 2-[(3′-pyridyl)azo]imidazole (3′-PyaiH) and this has been confirmed by X-ray structure determination. The N(1)-alkylation gi
ves 1-alkyl-2-[(3′-pyridyl)azo]imidazole (3′-PyaiR′) (R′ = Me (
2a), Et (
2b), Bz (
2c)). The reaction between Mn(ClO
4)
2 · 6H
2O and 3′-PyaiR′ in methanol has synthesized [Mn(3′-PyaiR′)
4](ClO
4)
2 (
3). The structure has been confirmed by single crystal X-ray diffraction study in one case, in addition to other spectral characterization. The structure re
veals a tetrahedral orientation of four ligands coordinating through imidazole-N only. Cyclic
voltammetry exhibits a Mn(III)/Mn(II) couple at >1.1 V along with azo reductions. Howe
ver, the reaction of MnCl
2 · 4H
2O + 3′-PyaiR′ in the presence of NaN
3 or NH
4CNS (1:2:2 mole proportion) has synthesized Mn(3′-PyaiR′)
2(X)
2 (X = N
3 (
4), NCS (
5)).