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The iodido bismuthates [Bi(18-crown-6)I 2 ][BiI 4 ] ( 1 ) and [Bi(18-crown-6)I 2 ][Bi 3 I 10 ] ( 2 ), the neutral complex [Bi(C 6 H 14 O 4 )I 3 ](18-crown-6) ( 3 ) as well as the polyiodides [Bi(18-crown-6)I 2 ][I 5 ](18-crown-6) ( 4 ), [Bi(18-crown-6)I 2 ] 2 [I 14 ] ( 5 ) and [Bi(18-crown-6)I 2 ] 2 [I 19 ] ( 6 ) were prepared by reaction of BiI 3 , 18-crown-6, and I 2  at  T  = 60–120 °C. The compounds  1–5  were prepared in [ n -Bu 3 MeN][N(Tf) 2 ] as an ionic liquid ([ n -Bu 3 MeN]: tributylmethylammonium, [N(Tf) 2 ]: bis(trifluoromethylsulfonyl)imide), whereas  6  was obtained only by direct reaction of the starting materials. The title compounds exhibit two different constitutions of the [Bi(18-crown-6)I 2 ] +  cation as well as a non-charged, molecular [Bi(C 6 H 14 O 4 )I 3 ] unit with a triethylene glycol ligand generated  in situ  by cleavage of the crown ether. Infinite chain-like[BiI2   /   1I4   /   2]−∞   1${}_{\infty }{}^{1}\left[{{\text{BiI}}_{2/1}{\text{I}}_{4/2}\right]}^{-}$and[Bi   6I18   /   1I4   /   2∞   1]−${{}_{\infty }{}^{1}\left[{\text{Bi}}_{6}{\text{I}}_{18/1}{\text{I}}_{4/2}\right]}^{-}$anions occur in  1  and  2 , whereas various polyiodide anions (e.g. [I 3 ] − , [I 5 ] − , [I 7 ] − , [I 9 ] − ) with partly complex interaction are observed in  4 ,  5 , and  6 . The title compounds were characterized by single-crystal X-ray diffraction analysis and infrared spectroscopy. In the case of  1  and  2 , the optical band gap was determined to be  Eg    = 1.91 and 1.62 eV, respectively. Especially, the ionic-liquid-based synthesis affords the different metastable compounds with variable composition and structure in a narrow temperature range.

On iodido bismuthates, bismuth complexes and polyiodides with bismuth in the system BiI 3 /18-crown-6/I 2