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The synthesis of [Bi(C 18 H 14 P(O)SO 3 ) 2 (DMSO) 3 ](NO 3 )∙DMSO∙2H 2 O starting from [Bi 6 O 4 (OH) 4 ](NO 3 ) 6 ∙H 2 O and 2-(diphenylphosphino)benzenesulfonic acid is presented.  31 P{ 1 H}-NMR experiments confirm the  in situ  oxidation of 2-(diphenylphosphino)benzenesulfonic acid to give 2-(diphenylphosphine oxide)benzenesulfonic acid by heating in dimethyl sulfoxide (DMSO). In the presence of [Bi 6 O 4 (OH) 4 ](NO 3 ) 6 ∙H 2 O, subsequent formation of single crystals of the title compound is observed. The crystal structure determination reveals that the bismuth atom shows a [5+4] coordination with short Bi–O distances in the range of 2.278(11) to 2.398(11) Å to the oxygen atoms of DMSO and phosphine oxide groups and with longer Bi–O bonds of 2.74(2) and 2.88(2) Å to the chelating sulfonate groups.

Synthesis and molecular structure of the novel bismuth(III) sulfonate complex [Bi(C 18 H 14 P(O)SO 3 ) 2 (DMSO) 3 ](NO 3 )∙DMSO∙2H 2 O