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The syntheses of Na(TttMe) (1), K(TttMe) (2), K(BttMe) (3), and Na(BttPh) (4) are reported, where (TttMe)− and (BttR)− (R = Me, Ph) are tri- and di-substituted boron-centered soft ligands; they were produced by the reaction of NaBH4 and KBH4 with the corresponding tetrazole heterocycles: 1-methyl-5-thiotetrazole (L1H) and 1-phenyl-5-thiotetrazole (L2H). The syntheses of Na(TttMe) (1) and K(TttMe) (2) were carried out following Trofimenko's protocol. The anion (TttMe)− is a typical Janus scorpionate ligand. Na(TttMe) (1) and Na(BttPh) (4) were reacted with Bi(CH3COO)3 to observe the coordination pattern of these ligands towards bismuth ions. These reactions afforded the complexes [Bi(TttMe)2(CH3COO)] (5), [Bi(L2)2]2 (6a, 6b) and [Bi(L2)3] (7). The products were characterized by NMR spectroscopy, elemental analyses and mass spectrometry. Solid state structures were determined by X-ray diffraction of single crystals of 1, 2, 3, 4, 5, 6a, 6b and 7. M(TttMe) (M = Na (1), K (2)) and K(BttMe) (3) exhibit sheet-like structures. The alkali metal complexes 1–4 dissociate in solution as observed in 1H, 13C NMR and 1H diffusion NMR experiments. Negative mode ESI-MS data also indicate the presence of monomers. Both the sodium salts of (TttMe)− and (BttPh)− as well as the Bi complexes 5 and 7 were investigated by absorption and emission spectroscopy.
