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• W2078984207 abstract "The structural coordination chemistry of the sterically hindered 3,3‘-bis(triphenylsilyl)-1,1‘-bi-2-phenoxide ligand ([TPSLO2]2-), an isosteric homologue of a chiral binaphthoxide ligand used in asymmetric induction, has been investigated on Fe(II), Fe(III), and Cr(II). The ligand diol (TPSL(OH)2, 2) can be prepared on a multigram scale from 2,2‘-dimethoxybiphenyl via a convenient, two-step ortho-metalation/silylation/deprotection sequence; the sodium salt of the ligand dianion (Na2[TPSLO2], 3) can be obtained by NaH deprotonation and was crystallographically characterized with two THF ligands bound to each cation. Protonolysis of Fe[N(SiMe3)2]2 or Cr[N(SiMe3)2]2(THF)2 with biphenol 2 in arene solvent gives [Fe(μ-TPSLO2)]2 (4) or (TPSLO2)Cr(THF)2 (9), respectively, while anion metathesis of FeCl2 or FeCl3/bipy with biphenoxide salt 3 in THF yields (TPSLO2)Fe(THF)2 (8) or ferric monomer (TPSLO2)FeCl(bipy) (10), respectively. Dimer 4 reacts with exogenous ligands to form monomeric ligand adducts of Fe(II): with py, (TPSLO2)Fe(py)2 (5); with bipy, (TPSLO2)Fe(bipy) (6); with XyNC (Xy = 2,6-xylyl), (TPSLO2)Fe(CNXy)4 (7); and with THF, 8. Complexes were characterized in solution by 1H NMR and in the solid state by single-crystal X-ray diffraction. The 4-coordinate complexes (5, 6, 8, 9) adopt skew-distorted tetrahedral (for Fe(II)) or square planar (for Cr(II)) geometries; the 5- and 6-coordinate complexes (10 and 7) assume more typical distorted square pyramidal/trigonal bipyramidal and cis-octahedral stereochemistries. Dimer 4 possesses an unusual structure where each Fe(II) center is pseudo-4-coordinate and each biphenoxide ligand provides one terminal phenoxide donor, one bridging phenoxide, and a weak aromatic π-interaction from one of the phenyl groups of a SiPh3 substituent. The steric influence of the hindered biphenoxide ligand within the coordination sphere is revealed structurally through distortion of coordination polyhedra in the 4-coordinate species and through conformational and deformational changes within the biphenoxide ligand itself." @default.
• W2078984207 created "2016-06-24" @default.
• W2078984207 creator A5011824851 @default.
• W2078984207 creator A5034112949 @default.
• W2078984207 date "2002-01-01" @default.
• W2078984207 modified "2023-10-11" @default.
• W2078984207 title "3,3‘-Bis(triphenylsilyl)biphenoxide as a Sterically Hindered Ligand on Fe(II), Fe(III), and Cr(II)" @default.
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• W2078984207 doi "https://doi.org/10.1021/ic010909y" @default.
• W2078984207 hasPubMedId "https://pubmed.ncbi.nlm.nih.gov/11800621" @default.
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