Synthesis and solid-state characterization of platinum complexes with hexadentate amino- and iminophosphine ligands

Authors: Thibault, Marie-Hélène; Lucier, Bryan; Schurko, Robert W.; Fontaine, Frédéric-Georges
Abstract: Hexadentate ligands cis,cis-C6H9(N[double bond, length as m-dash]CHC6H4(PPh2))3 (1) and cis,cis-C6H9(NHCH2C6H4(PPh2))3 (2) were synthesized starting from cis,cis-1,3,5-triaminocyclohexane, and characterized using NMR spectroscopy and single-crystal X-ray diffraction. These ligands can bind both Pt(0) and Pt(II) metal centers using either or both of the soft phosphine moieties and the hard amine/imine moieties. In many cases the resulting complexes are negligibly soluble; hence, 31P and 195Pt solid-state NMR (SSNMR) spectroscopy was applied to analyse the bonding modes of the hexadentate ligands. The 195Pt SSNMR spectroscopy of these complexes is particularly challenging, since 1H–195Pt cross polarization is extremely inefficient, the 195Pt longitudinal relaxation times are extremely long and the 195Pt powder patterns are expected to be quite broad due to platinum chemical shift anisotropy. It is demonstrated that the ultra-wideline 195Pt SSNMR spectra can be efficiently acquired with a combination of frequency-stepped piecewise acquisitions and cross-polarization/Carr–Purcell Meiboom–Gill (CP/CPMG) NMR experiments. The 195Pt and 31P SSNMR data are correlated to important structural features in both Pt(0) and Pt(II) species
Document Type: Article de recherche
Issue Date: 29 July 2009
Open Access Date: 20 April 2018
Document version: AM
This document was published in: Dalton Transactions, No 37, 7701–7716 (2009)
Royal Society of Chemistry
Alternative version: 10.1039/b907737e
Collection:Articles publiés dans des revues avec comité de lecture

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