A simple molecule with a complex crystal structure: interplay of P-31 solid-state NMR spectroscopy and single-crystal x-ray diffraction in the structure determination of a ruthenium diphosphine diamine complext

摘要

A comprehensive P-31 solid-state NMR study of Ru(eta(1)-Ph2PCH2CH2OCH3)(2)(eta(2)-en)Cl-2 (en = ethylenediamine) (1), by 1D (contact time variation, inversion-recovery, SPARTAN) and 2D techniques (homonuclear J-resolved, SECSY) indicated that the crystal structure of 1 should be complex. The single-crystal x-ray structure determination confirmed the presence of eight independent molecules in the asymmetric unit, with P-31 isotropic chemical shifts in the range 27.3-40.1 ppm, while the spans of the phosphorus chemical shift tensors are of the order of 170 ppm. Based on unique structural features and NMR data, one molecule has been tentatively assigned. Copyright (C) 2004 John Wiley Sons, Ltd.