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The compounds  Pn (pyS) 3  ( Pn  = P, As, Sb, Bi) were synthesized from the respective chloride ( Pn  = P, As, Sb) or nitrate (Bi), pyridine-2-thiol (pySH) and triethylamine (NEt 3 ) as a supporting base in THF (P, Sb), CHCl 3  (As) or methanol (Bi). Sb(pyS) 3  was also obtained from the reaction of SbCl 3  with LipyS (prepared  in situ ) in methanol. The compounds Sb(pyS) 2 Ph and Sb(pyS)Ph 2  were prepared in a one-pot reaction starting from SbCl 3  and SbPh 3  (1:1 ratio). Upon Cl/pyS substitution, the resulting reaction mixture allows for a facile separation of the products in hot hexane. P(pyS) 3  and As(pyS) 3  crystallize isostructurally to the reported structure of Sb(pyS) 3  with  κ -S-bound pyS ligands. These crystal structures feature close  Pn ··· Pn  contacts which are most pronounced for the arsenic derivative. Bi(pyS) 3  adopts a different molecular structure in the solid state, which features two chelating ( κ  2 -S,N-pyS) ligands and a  κ -S-bound ligand. The presence of N→Bi interactions between the nitrogen atom of the  κ -S-pyS ligand and the Bi atom of another molecule renders this structure a polymer chain along the crystallographic  b  axis with Bi⋅⋅⋅Bi van-der-Waals contacts. The structures of this set of  Pn (pyS) 3  compounds were also studied in solution using  1 H NMR spectroscopy, revealing equivalent pyS ligands in discrete  Pn (pyS) 3  molecules. The molecular structure of Sb(pyS)Ph 2  was optimized by quantum chemical methods, and a comparison with the structures reported for the other Sb/pyS/Ph combinations reveals Sb(pyS) 2 Ph to feature the strongest Sb···N interactions with the  κ -S-pyS ligand. The results of  1 H NMR spectroscopic investigations of the compounds Sb(pyS)  x  Ph 3– x   ( x  = 3–0) suggest the Ph protons in  ortho  position to be incorporated into intramolecular C–H···S contacts for  x  = 2 and 1. Natural localized molecular orbital (NLMO) calculations were employed in order to gain insights into the electronic situations of the  Pn  atoms and  Pn –R bonds (R = S, C), especially for the effects caused by formal substitution of  Pn  in the compounds  Pn (pyS) 3  and the ligand patterns in the compounds Sb(pyS)  x  Ph 3– x   ( x  = 3–0). For the latter series of compounds, the electronic situation of the Sb atom was further studied by  121 Sb Mössbauer spectroscopy, providing a correlation between the calculated electron density at Sb [ ρ (0)] and the experimentally observed isomer shift  δ . The missing link between group 15 and group 13 metal compounds of the type  M (pyS) 3 , compound Al(pyS) 3 , was synthesized in this work. In the solid state (confirmed crystallographically), the  mer  isomer of this  tris -chelate complex with distorted octahedral Al coordination sphere was found. This coordination mode was confirmed for the solution state (CDCl 3 ) by  1 H and  13 C NMR spectroscopy at  T  = −40 °C.

zeitschrift für naturforschung b

Compounds of the types  Pn (pyS) 3  ( Pn  = P, As, Bi; pyS: pyridine-2-thiolate) and Sb(pyS)  x  Ph 3– x   ( x  = 3–1); molecular structures and electronic situations of the  Pn  atoms