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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Interactions of C‐iso‐butyl‐calix[4]resorcinarene (1) with sodium sulfite and formaldehyde solution gave a new water‐soluble sulfonatomethylated calix[4]resorcinarene (C4RS) 2 in a quantitative yield. Treatment of 2 with NaOH in a mixture of water, acetonitrile, and methanol afforded complex [Na4(C4RS‐4H)(CH3CN)(H2O)6]2⋅CH3OH (3). Reaction of 2 with NaOH aqueous solution, followed by addition of cesium chloride, led to isolation of complex Cs4Na[(C4RS)2‐5H)](H2O)2 (4). Cation exchange of aluminum nitrate hydrate with complex 3 afforded complex {Al3(H2O)5[(C4RS)2‐9H)]}2⋅(C2H5OH)2⋅(H2O)4 (5). The three new coordination complexes 3–5 were characterized by single crystal X‐ray diffraction analysis. Complexes 3 and 4 display a two‐dimensional bilayer structure through bridging of the sulfonate groups by sodium/cesium cations. The aluminum sulfonatomethylated calix[4]resorcinarene sheets in complex 5 are associated in a one‐dimensional bilayer arrangement and further connected by hydrogen bonds to form a two‐dimensional network.

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Treatment of cis-[Ru(acac) 2 (CH 3 CN) 2 ] (acac À = acetylacetonate) with 1.5 equiv. of corresponding bidentate nitrogen and sulfur ligands in ethanol gave a series of bis(acetylacetonato) ruthenium(II/III) complexes [(acac 4) and [(acac) 2 Ru(S 2 CNMe 2 )] (5), respectively.Complexes 1-5 were characterized by FT-IR, NMR and UV-Vis spectroscopies along with their electrochemical properties. The structures of complexes 1-5 have been unambiguously established by single crystal X-ray crystallography. The photocatalytic properties for hydrogen production by water splitting of complexes 1-5 under visible light (λ > 420 nm) were also investigated in the paper.