Diaminoguanidinium and triaminoguanidinium Schiff bases of 1,3-bis(3,5-di-tert-butyl-2-hydroxyphenylmethylideneamino) guanidine hydrochloride (H 5 saldag tBu2 ⋅ HCl) and tris(3,5-di-tertbutyl-2-hydroxybenzylidene)-triaminoguanidinium chloride (H 5 saltag tBu2 ⋅ HCl) are synthesized. Treatment of H 5 saldag tBu2 ⋅ HCl with Na 2 MoO 4 ⋅ 2H 2 O or (NH 4) 6 Mo 7 O 24 ⋅ 4H 2 O under different molar ratios afforded mono-and di-nuclear molybdenum(VI) complexes of [(MoO 2)(MeOH)(H 3 saldag tBu2)] (1), [(MoO 2) 2 (MeOH) 2 (Hsaldag tBu2)] ⋅ 2DMF (2 ⋅ 2DMF), and [(MoO 2) 2 (Hsaldag tBu2)] ⋅-[(MoO 2) 2 (H 2 O) 2 (Hsaldag tBu2)] (3). Interactions of H 5 saltag tBu2 ⋅ HCl with Na 2 MoO 4 ⋅ 2H 2 O or (NH 4) 6 Mo 7 O 24 ⋅ 4H 2 O under different reaction conditions resulted mono-, di-, and tetra-nuclear molybdenum(VI) complexes of [(MoO 2)(MeOH)(H 3 saltag tBu2)] (4), [(MoO 2)(H 2 O)(H 3 saltag tBu2)] (5), [(MoO 2) 2 (H 2 O)(DMF)(Hsaltag tBu2)] ⋅ 3DMF (6) (Ref [31]), and [(MoO 2) 4 (DMF) 2 (Hsaltag tBu2) 2 ] ⋅ 2H 2 O (7 ⋅ 2H 2 O). Complexes 1-7 were characterized by IR, 1 H NMR and UV/vis spectroscopies. Molecular structures of H 5 saltag tBu2 ⋅ MeOH, 1, 2 ⋅ 2DMF, 3-5 and 7 ⋅ 2H 2 O are confirmed by single crystal X-ray diffraction ananlysis, which shows that the diaminoguanidinium and triaminoguanidinium Schiff bases are coordinated to the cis-{MoO 2 } 2 + moieties via ONN atoms to form five-and sixmembered rings, sharing one MoÀ N bond. The catalytic properties of these cis-dioxo-molybdenum(VI) complexes for epoxidation of cyclohexene were also investigated.
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