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Intermediates and Side-Reactions in the Synthesis of Molecular Diphenolatonickel Compounds Containing Trimethylphosphane Ligands

✍ Scribed by Hans-Friedrich Klein; Attila Dal; Thomas Jung; Ulrich Flörke; Hans-Jürgen Haupt

Publisher
John Wiley and Sons
Year
1998
Tongue
English
Weight
164 KB
Volume
1998
Category
Article
ISSN
1434-1948

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✦ Synopsis

Admission of molecular oxygen to a solution containing hydroxyphenylnickel compounds Ni(ArЈ) X(PMe 3 ) 3 [ArЈ = 2-OH-C 6 H 4 ; X = Br (6), I (7)], trans-Ni(ArЈ)Cl(PMe 3 ) 2 [ArЈ = 2-Ni(PMe 3 ) 4 and substituted phenols (ArOH) affords bisphenolatonickel compounds trans-Ni(OAr) 2 (PMe 3 ) 2 OH-3,5-Cl 2 -C 6 H 2 (8)] and trans-Ni(OAr)Cl(PMe 3 ) 2 [Ar = 2,4,6-Cl 3 -C 6 H 2 (9)] is observed. An X-ray crystal structure [ArOH = 2-chlorophenol (1), 2-bromophenol (2), 2,4,6trichlorophenol (3)]. In the absence of dioxygen the phenols determination of 1 shows a trans square planar arrangement of donor atoms, that of 6 shows a distorted square pyramid, reversibly protonate the nickel complex to form ionic compounds [NiH(PMe 3 ) 4 ] + Y -containing hydrogen-bonded while 4 contains tetrahedral nickel cations with a delocalized hydrogen atom and triphenolate anions H 2 (ArO) 3 -. anions Y = [H 2 (2-Cl-C 6 H 4 O) 3 ] (4), [H(2-OH-C 6 H 4 COO) 2 ] (5). As a side-reaction, formal insertion of nickel to give 2-

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The reaction of one equivalent of In with a molten flux of (Ph 4 P) 2 Se 5 and P 2 Se 5 (1 : 2), at 250 °C gave the (Ph 4 P)[In(P 2 Se 6 )] (I). Stoichiometric elemental synthesis at 750 °C produced the Cs 5 In(P 2 Se 6 ) 2 (II). The thin, yellow crystals of (I), and the irregular, dark orange cryst