The synthesis of the new ligand bis(6‐diphenylphosphinoacenaphth‐5‐yl)sulfoxide, [6‐(Ph2P)‐5‐Ace‐6]2‐SO (1), is presented along with six transition metal complexes thereof, namely, 1·MCl (M = Rh, Cu, Ag, Au) and 1·MCl2 (M = Ni, Pd). Within these novel complexes, close metal‐sulfur distances are observed and the nature of the M–S coordination, as well as the response of the +S–O– bond, are investigated in detail with a set of spectroscopic, crystallographic and real‐space bonding indicators.
The 2,6‐difluorophenyltrialkylstannanes 2,6‐F2C6H3SnR3 (1, R=Me; 2, R=Bu) were prepared from commercial products. With Ph2PLi, 1 and 2 underwent nucleophilic substitution to give the 2,6‐bis(diphenylphosphino)phenyltrialkylstannanes 2,6‐(Ph2P)2C6H3SnR3 (3, R=Me; 4, R=Bu). The reaction of 3 with n‐BuLi and BrCH2CH2Br afforded 2,6‐bis(diphenylphosphino)bromobenzene (2,6‐(Ph2P)2C6H3Br, 5), the oxidation of which gave the related bis(phosphine oxide) 2,6‐[Ph2P(O)]2C6H3Br (6). The reaction of 5 with n‐BuLi gave rise to the formation of 2,6‐bis(diphenylphosphino)phenyl lithium, 2,6‐(Ph2P)2C6H3Li (7). Attempts to prepare the related bis(phosphine oxide) 2,6‐[Ph2P(O)]2C6H3Li (8) from 6 in a similar way at low temperatures was hampered by decomposition. Compounds 3, 5 and 7 hold potential for a new anionic tridentate PCP−coordinating ligand, namely, the bis(2,6‐diphenyl)phosphinophenyl ion [2,6‐(Ph2P)2C6H3]−.
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