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The reaction of a phosphorus trihalide PX 3 (X = Cl, Br, or I) with a thiophosphorus halide P(S)Y 3 (Y = Cl or Br) in the presence of zinc powder as a halogen acceptor has led to the formation of several new mixed-valence phosphorus species in solution. These include examples with two or three phosphorus atoms present, such as Y 2 P(S)PX 2 and Y 2 P(S)P(X)P(S)Y 2 , or halogen exchange derivatives thereof. Structural assignments for these species have been made on the basis of

Variation in the position of CF3 groups in several aromatic Group‐14 compounds was studied by 19F‐NMR spectroscopy. In these compounds RnECl4−n (n=1 or 2; E=Si, Ge, or Sn; R=2,4,6‐(CF3)3C6H2 (=Ar), 2,6‐(CF3)2C6H3 (=Ar′), or 2,4‐(CF3)2C6H3 (=Ar″)), Ar, Ar′, and Ar″ are all bulky, strongly electron‐withdrawing ligands. The 19F‐NMR studies of the variation in position of the CF3 substituents in these compounds as revealed by chemical shifts could be correlated with the electronegativities of the central elements E, and with intramolecular E–F interactions derived from single‐crystal X‐ray diffraction data. These interactions are considered to play an important role in the stabilization of these compounds.